Microindentation Hardness of Materials: Standard Test Method For

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E384 − 17
Standard Test Method for

Microindentation Hardness of Materials1
This standard is issued under the fixed designation E384; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* 2. Referenced Documents

1.1 This test method covers determination of the microin- 2.1 ASTM Standards:2
dentation hardness of materials. C1326 Test Method for Knoop Indentation Hardness of
1.2 This test method covers microindentation tests made Advanced Ceramics
with Knoop and Vickers indenters under test forces in the range C1327 Test Method for Vickers Indentation Hardness of
from 9.8 × 10-3 to 9.8 N (1 to 1000 gf). Advanced Ceramics
E3 Guide for Preparation of Metallographic Specimens
1.3 This test method includes an analysis of the possible E7 Terminology Relating to Metallography
sources of errors that can occur during microindentation testing E92 Test Method For Vickers Hardness of Metallic Materials
and how these factors affect the precision, bias, repeatability, E140 Hardness Conversion Tables for Metals Relationship
and reproducibility of test results. Among Brinell Hardness, Vickers Hardness, Rockwell
1.4 Information pertaining to the requirements for direct Hardness, Superficial Hardness, Knoop Hardness, Sclero-
verification and calibration of the testing machine and the scope Hardness, and Leeb Hardness
requirements for the manufacture and calibration of Vickers E175 Terminology of Microscopy
and Knoop reference hardness test blocks are in Test Method E177 Practice for Use of the Terms Precision and Bias in
E92. ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to
NOTE 1—While Committee E04 is primarily concerned with metals, the
test procedures described are applicable to other materials.
Determine the Precision of a Test Method
E766 Practice for Calibrating the Magnification of a Scan-
1.5 Units—The values stated in SI units are to be regarded ning Electron Microscope
as standard. No other units of measurement are included in this E1268 Practice for Assessing the Degree of Banding or
standard. Orientation of Microstructures
1.6 This standard does not purport to address all of the E2554 Practice for Estimating and Monitoring the Uncer-
safety concerns, if any, associated with its use. It is the tainty of Test Results of a Test Method Using Control
responsibility of the user of this standard to establish appro- Chart Techniques
priate safety and health practices and determine the applica- E2587 Practice for Use of Control Charts in Statistical
bility of regulatory limitations prior to use. Process Control
1.7 This international standard was developed in accor- 2.2 ISO Standard:3
dance with internationally recognized principles on standard- ISO/IEC 17025 General Requirements for the Competence
ization established in the Decision on Principles for the of Testing and Calibration Laboratories
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 3. Terminology
Barriers to Trade (TBT) Committee. 3.1 Definitions—For definitions of terms used in this test
method, see Terminology E7.
3.2 Definitions of Terms Specific to This Standard:
1
This test method is under the jurisdiction of ASTM Committee E04 on
Metallography and is the direct responsibility of Subcommittee E04.05 on Micro-
2
indentation Hardness Testing. With this revision the test method was expanded to For referenced ASTM standards, visit the ASTM website, www.astm.org, or
include the requirements previously defined in E28.92, Standard Test Method for contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Vickers Hardness Testing of Metallic Material that was under the jurisdiction of Standards volume information, refer to the standard’s Document Summary page on
E28.06 the ASTM website.
3
Current edition approved June 1, 2017. Published August 2017. Originally Available from International Organization for Standardization (ISO), 1, ch. de
approved in 1969. Last previous edition approved in 2016 as E384 – 16. DOI: la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://
10.1520/E0384-17 www.iso.org.
*A Summary of Changes section appears at the end of this standard

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E384 − 17
3.2.1 calibrating, v—determining the values of the signifi- geometrical variations between diamond indenters, and human
cant parameters by comparison with values indicated by a errors in measuring indentation lengths will affect the precision
reference instrument or by a set of reference standards. of the calculated material hardness. The magnitude of the error
3.2.2 Knoop hardness number, HK, n—an expression of that variations of each of these parameters have on the
hardness obtained by dividing the force applied to the Knoop calculated value of a microindentation measurement is dis-
indenter by the projected area of the permanent impression cussed in Section 10.
made by the indenter. 3.3.1 For Knoop hardness tests, in practice, test loads are in
3.2.3 Knoop indenter, n—a rhombic-based pyramidal- grams-force and indentation diagonals are in micrometers. The
shaped diamond indenter with edge angles of / A = 172° 30' Knoop hardness number is calculated using the following:
and / B = 130° 0' (see Fig. 1). HK 5 1.000 3 103 3 ~ P/A p ! 5 1.000 3 103 3 P/ ~ c p 3 d 2 ! (1)
3.2.4 microindentation hardness test, n—a hardness test or
using a calibrated machine to force a diamond indenter of
HK 5 14229 3 P/d 2 (2)
specific geometry into the surface of the material being
evaluated, in which the test forces range from 1 to 1000 gf (9.8 /B
tan
× 10-3 to 9.8 N), and the indentation diagonal, or diagonals, are 2
cp 5 (3)
measured with a light microscope after load removal; for any /A
2tan
microindentation hardness test, it is assumed that the indenta- 2
tion does not undergo elastic recovery after force removal. where:
NOTE 2—Use of the term microhardness should be avoided because it P = force, gf,
implies that the hardness, rather than the force or the indentation size, is d = length of long diagonal, µm,
very low.
Ap = projected area of indentation, µm 2
3.2.5 verifying, v—checking or testing the instrument to /A = included longitudinal edge angle, 172° 30’
assure conformance with the specification. /B = included transverse edge angle, 130° 0’ (see Fig. 1
3.2.6 Vickers hardness number, HV, n—an expression of and,
hardness obtained by dividing the force applied to a Vickers cp = indenter constant relating projected area of the inden-
indenter by the surface area of the permanent impression made tation to the square of the length of the long diagonal,
by the indenter. ideally 0.07028.
3.2.7 Vickers indenter, n—a square-based pyramidal-shaped 3.3.2 The Knoop hardness, kgf/mm2 is determined as fol-
diamond indenter with face angles of 136° (see Fig. 2). lows:
3.3 Formulae—The formulae presented in 3.3.1 – 3.3.4 for HK 5 14.229 3 P 1 /d 1 2 (4)
calculating microindentation hardness are based upon an ideal
where:
tester and conditions. The measured value of the microinden-
tation hardness of a material is subjected to several sources of P1 = force, kgf, and
errors. Based on Eq 1-9, variations in the applied force, d1 = length of long diagonal, mm.
FIG. 1 Knoop Indenter
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FIG. 2 Vickers Indenter
3.3.3 The Knoop hardness reported with units of GPa is 3.4 Equations for calculating % Error and Repeatability for
determined as follows: periodic verification is determined as follows:
where:
HK 5 0.014229 3 P 2 /d 2 2 (5)
E 5 100 S d̄ 2 d ref
d ref
D (10)
P2 = force, N, and where:

d2 = length of the long diagonal of the indentation, mm. E = % error in performance of the periodic verification,
3.3.4 For the Vickers hardness test, in practice, test loads are d̄ = the measured mean diagonal length in µm, and
in grams-force and indentation diagonals are in micrometers. dref = the reported certified mean diagonal length, µm.
The Vickers hardness number is calculated as follows:
HV 5 1.000 3 103 3 P/A s 5 2.000 3 103 3 Psin~ α/2 ! /d 2 (6)
R 5 100 S d max 2 d min
d̄
D (11)
or where:
HV 5 1854.4 3 P/d 2 (7) R = repeatability in performance of the periodic
where: verification,
dmax = the longest diagonal length measurement on the
P = force, gf, standardized test block, µm,
As = surface area of the indentation, µm2, dmin = the shortest diagonal length measurement on the
d = mean diagonal length of the indentation, µm, and
standardized test block, µm, and
α = face angle of the indenter, 136° 0’ (see Fig. 2).
d̄ = the measured mean diagonal length in µm.
3.3.5 The Vickers hardness, kgf/mm2 is determined as
follows: 4. Summary of Test Method
HV 5 1.8544 3 P 1 /d 1 2 (8) 4.1 In this test method, a hardness number is determined
where: based on the formation of a very small indentation by appli-
P1 = force, kgf, and cation of a relatively low force, in comparison to traditional
d1 = mean diagonal length of the indentations, mm. bulk indentation hardness tests.
3.3.6 The Vickers hardness reported with units of GPa is 4.2 A Knoop or Vickers indenter, made from diamond of
determined as follows: specific geometry, is pressed into the test specimen surface
under an applied force in the range of 1 to 1000 gf using a test
HV 5 0.0018544 3 P 2 /d 2 2 (9)
machine specifically designed for such work.
where:
4.3 The size of the indentation is measured using a light
P2 = force, N, and microscope equipped with a filar type eyepiece, or other type
d2 = mean diagonal length of the indentations, mm. of measuring device (see Terminology E175).
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4.4 The Knoop hardness number is based upon the force Knoop hardness is not normally used to define bulk hardness,
divided by the projected area of the indentation. The Vickers except at 500 gf where E140 gives conversions to other test
hardness number is based upon the force divided by the surface scales, and Knoop tests should not be performed at test forces
area of the indentation. above 1000 gf. The majority of Knoop tests of case hardness
4.5 It is assumed that elastic recovery does not occur when variations are conducted at forces from 100 to 500 gf. If the test
the indenter is removed after the loading cycle, that is, it is is being conducted to meet a specified bulk hardness value,
assumed that the indentation retains the shape of the indenter such as HRC, then most such tests will be conducted with
after the force is removed, but this is not always true. In Knoop Knoop at a 500 gf load. Because of the large difference
testing, it is assumed that the ratio of the long diagonal to the between the long and short Knoop diagonals, the Knoop
short diagonal of the impression is the same as for the indenter, indenter is often better suited for determining variations of
7.114, but this is not always true due to elastic recovery. hardness over very small distances compared to the Vickers
indenter. Vickers and Knoop tests at forces ≤25 gf are
5. Significance and Use susceptible to imprecision due to the difficulty in measuring
extremely small indents (<20 µm) by light microscopy with
5.1 Hardness tests have been found to be very useful for high precision and reproducibility. Tests made at forces ≤25 gf
materials evaluation, quality control of manufacturing pro- should be considered to be qualitative in nature. Likewise, test
cesses and research and development efforts. Hardness, al- forces that create indents <20 µm in length should be avoided
though empirical in nature, can be correlated to tensile strength whenever possible and should be considered to be qualitative
for many metals and alloys, and is also an indicator of in nature. The success of the specimen preparation procedure in
machinability, wear resistance, toughness and ductility. removing preparation-induced damage can, and will, influence
5.2 Microindentation tests are utilized to evaluate and quan- test results; this problem becomes more critical as the test force
tify hardness variations that occur over a small distance. These decreases.
variations may be intentional, such as produced by localized
surface hardening, for example, from shot blasting, cold 6. Apparatus
drawing, flame hardening, induction hardening, etc., or from 6.1 Test Machine—The test machine must support the test
processes such as carburization, nitriding, carbonitriding, etc.; specimen and control the movement of the indenter into the
or, they may be unintentional variations due to problems, such specimen under a preselected test force, and should have a light
as decarburization, localized softening in service, or from optical microscope to select the desired test locations and to
compositional/microstructural segregation problems. Low test measure the size of the indentations produced by the test. The
forces also extend hardness testing to materials too thin or too plane of the surface of the test specimen must be perpendicular
small for macroindentation tests. Microindentation tests permit to the axis of the indenter and the direction of the force
hardness testing of specific phases or constituents and regions application. The plane of the test specimen surface must be flat,
or gradients too small for evaluation by macroindentation tests. and free of surface relief, in order to obtain valid, usable test
5.3 Because microindentation hardness tests will reveal data. The hardness test machine must meet the verification
hardness variations that commonly exist within most materials, requirements defined in Test Method E92.
a single test value may not be representative of the bulk 6.1.1 Force Application—The test machine shall be capable
hardness. Vickers tests at 1000 gf can be utilized for determi- of applying the test forces according to the following:
nation of the bulk hardness, but, as for any hardness test, it is 6.1.1.1 The time from the initial application of the force
recommended that a number of indents are made and the until the full test force is reached shall not exceed 10 s.
average and standard deviation are calculated, as needed or as 6.1.1.2 The indenter shall contact the specimen at a velocity
required. between 15 and 70 µm/s. Indenter velocity is not usually
5.4 Microindentation hardness testing is generally per- adjustable by the user.
formed to quantify variations in hardness that occur over small 6.1.1.3 The full test force shall be applied for 10 to 15 s
distances. To determine these differences requires a very small unless otherwise specified.
physical indentation. Testers that create indents at very low test 6.1.1.4 For some applications it may be necessary to apply
forces must be carefully constructed to accurately apply the test the test force for longer times. In these instances the tolerance
forces exactly at the desired location and must have a high- for the time of the applied force is 6 2 s.
quality optical system to precisely measure the diagonal (or 6.1.2 Vibration Control—During the entire test cycle, the
diagonals) of the small indents. Test forces in the upper range test machine should be protected from shock or vibration. To
of the force range defined in 1.2 may be used to evaluate bulk minimize vibrations, the operator should avoid contacting the
hardness. In general, the Vickers indenter is better suited for machine, or the support table, in any manner during the entire
determining bulk (average) properties as Vickers hardness is test cycle.
not altered by the choice of the test force, from 25 to 1000 gf, 6.2 Vickers Indenter—The Vickers indenter normally pro-
because the indent geometry is constant as a function of indent duces geometrically-similar indentation shapes at all test
depth. The Knoop indentation, however, is not geometrically forces. Except for tests at very low forces that produce
identical as a function of depth and there will be variations in indentations with diagonals smaller than about 20 µm, the
Knoop hardness, particularly at test forces <200 gf, over the Vickers hardness number will be the same, within statistical
force range defined in 1.2 (and above this range); consequently, precision limits, as produced using test forces that produce
4
E384 − 17
diagonal lengths ≥20 µm, using either a microindentation test 6.4 Measuring Equipment—The test machine’s measuring
machine up to 1000 gf or a macroindentation test machine with device should report the diagonal lengths in 0.1 µm increments
test forces ≥ 1 kgf, as long as the material being tested is for indentations with diagonals from 1 to 200 µm.
reasonably homogeneous and the magnification and image NOTE 3—This is the reported length and not the resolution of the system
quality are optimal (see Appendix X4). For isotropic materials, used for performing the measurements. As an example, if a length of 200
the two diagonals of a Vickers indentation are equal in size. µm corresponds to 300 filar units or pixels, the corresponding calibration
Metals/alloys with preferred crystallographic textures may constant would be 200/300 = 0.66666667. This value would be used to
produce distorted indents and invalid or questionable test compute diagonal lengths, but the reported length would only be reported
to the nearest 0.1 µm.
results. The Vickers indenter must meet the verification re-
quirements defined in Test Method E92. 6.4.1 The optical portion of the measuring device should
6.2.1 The ideal Vickers indenter is a highly polished, utilize Köhler illumination. Consult the manufacturer’s instruc-
tion manual for the adjustments that can be made on your
pointed, square-based pyramidal diamond with face angles of
tester.
136° 0'. The effect that geometrical variations of these angles
6.4.2 To obtain maximum resolution, the measuring micro-
have on the measured values of Vickers hardness is discussed
scope should have high quality objectives with adequate
in Section 10.
numerical apertures, a suitable eyepiece, adjustable illumina-
6.2.2 The four faces of the Vickers indenter shall be equally tion intensity, adjustable alignment and aperture and field
inclined to the axis of the indenter (within 6 30') and shall diaphragms. These are adjusted in the same manner as on a
meet at a sharp point. The line of junction between opposite reflected light microscope or metallograph. Some systems are
faces (offset) shall be not more than 0.5 µm in length as shown now designed using computer monitors and indent length
in Fig. 2. detection by image analysis and may not utilize a traditional
6.3 Knoop Indenter—The Knoop indenter does not produce eyepiece, but have a projection lens connected to a CCD
geometrically-similar indentation shapes as a function of test camera. While a traditional eyepiece has a circular field of
force and indent depth. Consequently, the Knoop hardness will view, the computer monitor is rectangular and its height-to-
vary with test force (see Appendix X4). Due to its rhombic width ratio can vary.
shape, the indentation depth is shallower for a Knoop inden- 6.4.3 Magnifications should be provided so that the diago-
tation compared to a Vickers indentation under identical test nal can be enlarged to greater than 25 % but less than 75 % of
conditions. But, for the same test force, the Knoop long the field width. If the computer screen has a 4 to 3 ratio of
diagonal will be substantially longer than the mean of the two width to height, or a greater difference between the screen
Vickers diagonals. The two diagonals of a Knoop indentation width and height, the maximum field height must be <75% of
are markedly different. Ideally, the long diagonal is 7.114 times the width to measure both Vickers diagonals. A 40× or 50×
longer than the short diagonal, but this ratio is influenced by objective may not be adequate for precise measurement of
elastic recovery. Because of its shape, the Knoop indenter is indents <30 µm in length. Measurements of diagonal lengths
very useful for evaluating hardness gradients or thin coatings. <20 µm in length with the light microscope may be imprecise,
The Knoop test is not recommended for use above a 1 kgf test regardless of the objective magnification used, with the prob-
load. The Knoop indenter must meet the verification require- lem becoming more acute as the diagonal length decreases
ments defined in Test Method E92. below 20 µm.
6.3.1 The Knoop indenter is a highly polished, pointed, 7. Test Specimen
rhombic-based, pyramidal diamond (1).4 The ideal included
7.1 For optimum accuracy of measurement, the test should
longitudinal edge angles are 172° 30' and 130° 0'. The ideal
be performed on a flat specimen with a polished surface free of
indenter constant, cp, is 0.07028. The effect that geometrical
preparation-induced damage. The surface must be free of any
variations of these angles have on the measured values of
problems that could affect the indentation or the subsequent
Knoop hardness is discussed in Section 10.
measurement of the diagonals. Conducting tests on non-planar
6.3.2 The four faces of the Knoop indenter shall be equally surfaces is not recommended. Results will be affected even in
inclined to the axis of the indenter (within 6 30') and shall the case of the Knoop test where the radius of curvature is in
meet at a sharp point. The line of junction between opposite the direction of the short diagonal.
faces (offset) shall be not more than 1.0 µm in length for 7.1.1 In all tests, the indentation perimeter, and the inden-
indentations greater than 20 µm in length, as shown in Fig. 1. tation tips in particular, must be clearly defined in the micro-
For shorter indentations, the offset should be proportionately scope field of view.
less. 7.1.2 For best results, the specimen surface should not be
6.3.3 Indenters should be examined periodically and re- etched before making an indentation (2), although etching is
placed if they become worn, dulled, chipped, cracked or often necessary to aid indent location. Deeply etched surfaces
separated from the mounting material. Never touch the in- will obscure the edge of the indentation, making an accurate
denter tip with your finger. measurement of the size of the indentation difficult or impos-
sible. When determining the microindentation hardness of an
isolated phase or constituent, or when evaluating segregated
4
The boldface numbers in parentheses refer to the list of references at the end of compared to non-segregated areas, and other similar situations,
this standard. a light etch is required to delineate the object or area of interest
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so that the indentations can be placed in the desired locations. 8.8 Activate the tester so that the indenter is automatically
The necessary quality of the required surface preparation does lowered and makes contact with the specimen for the normally
vary with the forces and magnifications used in microindenta- required time period. Then, remove the force either manually
tion hardness testing. The lighter the force and the smaller the or automatically.
indentation size, the more critical is the surface preparation. 8.9 After the force is removed, switch to the measuring
Some materials are more sensitive to preparation-induced mode, and select the proper objective lens. Focus the image,
damage than others. In general, face-centered cubic metals (for adjust the light intensity if necessary, and adjust the apertures
example, austenitic stainless steels, copper and its alloys, for maximum resolution and contrast.
nickel and its alloys, gold and silver) exhibit a larger deforma-
tion field around the indent than an indent of the same test force 8.10 Examine the indentation for its position relative to the
made in a body-centered cubic metal (for example, ferritic and desired location and for its symmetry.
martensitic steels). 8.10.1 If the indentation did not occur at the desired spot,
7.1.3 Due to the small size of the indentations, special the tester is out of alignment. Consult the manufacturer’s
precautions must be taken during specimen preparation. It is instruction manual for the proper procedure to produce align-
well known that improper preparation can alter test results. ment. Make another indentation and recheck the indentation
Specimen preparation must remove any damage introduced location. Readjust and repeat as necessary.
during these steps, either due to excessive heating or cold 8.10.2 For a Knoop indentation, if one half of the long
work, for example. diagonal is more than 10 % longer than the other diagonal half,
7.1.4 Specimen preparation should be performed in accor- or if both ends of the indentation are not in sharp focus, the test
dance with Guide E3. specimen surface may not be perpendicular to the indenter
axis. Such an indent may yield incorrect data and the calculated
7.2 In many instances, it is necessary to mount the specimen HK based upon it should be reported outside these limits.
for convenience in preparation and for best edge retention. Check the specimen alignment and make another test to be sure
When mounting is required, the specimen must be adequately that the test data is correct.
supported by the mounting medium so that the specimen does 8.10.3 For a Vickers indentation, if one half of either
not move during force application, such as might happen in an diagonal is more than 5 % longer than the other half of that
improperly cured polymer mount. diagonal, or if the four corners of the indentation are not in
sharp focus, the test surface may not be perpendicular to the
8. Procedure indenter axis. Such an indent may yield incorrect data and the
8.1 Turn on the illumination system and power for the tester. calculated HV based upon it should be reported outside these
limits. Check the specimen alignment and make another test to
8.2 Select the desired indenter. If it is necessary to physi- be sure that the test data is correct.
cally change indenters, refer to the manufacturer’s instructions. 8.10.4 If the diagonal legs are unequal as described in 8.10.2
With some machines, both indenters can be mounted on the or 8.10.3, rotate the specimen 90° and make another indenta-
turret and changed by a simple switch or computer command. tion in an untested region. If the nonsymmetrical aspect of the
Occasionally clean the indenter with a cotton swab and indentations has rotated 90°, then the specimen surface is not
alcohol. Avoid creating static charges during cleaning. Never perpendicular to the indenter axis. If the nonsymmetrical
touch the indenter tip with your fingers as this will alter the nature of the indentation remains in the same orientation, check
measurements. the indenter for misalignment or damage.
8.3 Place the specimen on the stage or in the stage clamps, 8.10.5 Some materials may have nonsymmetrical indenta-
so that the specimen surface is perpendicular to the indenter tions even if the indenter and the specimen surface are
axis. A top-referenced clamping system for mounts is an perfectly aligned. Tests on single crystals or on textured
excellent device for aligning the test plane perpendicular to the materials may produce such results. When this occurs, check
indenter, particularly if the back face of the mount is not the alignment using a test specimen, such as a standard, known
parallel to the polished front surface. If clay is used on a slide, to produce uniformly shaped indentations.
use very stiff clay and use high pressure when seating the 8.10.6 Brittle materials, such as ceramics, may crack as a
specimen against the clay. result of being indented. Specific details for testing ceramics
are contained in Test Methods C1326 and C1327.
8.4 Focus the measuring microscope with a low power
objective so that the specimen surface can be observed. 8.11 Measure the long diagonal of a Knoop indentation, or
both diagonals of a Vickers indentation, in accordance with the
8.5 Adjust the light intensity and adjust the apertures for
manufacturer’s instruction manual.
optimum resolution and contrast. Zero the measuring device
8.11.1 Determine the length of the long diagonal of a Knoop
according to the manufacturer’s recommended method.
indentation or both diagonals of a Vickers indentation to within
8.6 Select the area desired for hardness determination. 0.1 µm (see 6.3). For the Vickers indentations, average the two
Before applying the force, make a final focus using the diagonal length measurements.
measuring objective.
8.12 Compute the Knoop or Vickers hardness number using
8.7 Adjust the tester so that the indenter is in the proper the appropriate equation in Section 3 or using tables supplied
place for force application. Select the desired force. with the tester, respectively. Modern testers usually give an
6
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automatic readout of the hardness after the diagonal or diago- in GPa, and the rather narrow range of GPa values for metals,
nals have been measured. a “soft” SI system approach is recommended.
8.13 Spacing of Indentations—Generally, more than one 9.1.2 Test force, and
indentation is made on a test specimen. It is necessary to ensure 9.1.3 Any unusual conditions encountered during the test.
that the spacing between indentations is large enough so that 9.2 The symbols HK for Knoop hardness and HV for
adjacent tests do not interfere with each other. Because Vickers hardness shall be used with the reported numerical
face-centered cubic (FCC) metals (for example, austenitic values.
stainless steels, copper, nickel, silver and gold) work harden 9.2.1 For this standard, the microindentation hardness test
more dramatically than body-centered cubic (BCC) metals results can be reported in several different ways. For example,
(ferritic steels, for example), the indent spacing distance is if the Knoop hardness was found to be 400, and the test force
more critical for FCC metals as the deformation zone around was 100 gf, the test results may be reported as follows:
the indent is larger than for a BCC metal, as mentioned in
9.2.1.1 For microindentation hardness tests, where the test
7.1.2.
force is generally in gram force units, with test forces ≤1000 gf,
8.13.1 For most testing purposes, the minimum recom-
this result can be reported as 400 HK 0.1, for example, when
mended spacing between separate tests and the minimum
a test at 100 gf yields a Knoop hardness of 400. The same
distance between an indentation and the surface of the
approach is used to report the Vickers hardness.
specimen, are illustrated in Fig. 3.
9.2.1.2 In the SI system the hardness would be reported as
8.13.2 For some applications, closer spacing of indentations
3.92 GPa, but this practice is not preferred for the reasons
than those shown in Fig. 3 may be necessary. If a closer
stated in 9.1.1.
indentation spacing is used, it shall be the responsibility of the
testing laboratory to verify the accuracy of the testing proce- 9.2.1.3 For nonstandard dwell times, other than 10 to 15 s,
dure. Parallel, staggered bands of indents from the surface the hardness would be reported as 400 HK 0.1/22 s. In this
inward can be utilized to obtain closer overall spacing of case, 22 s would be the actual time of the full load dwell time.
indents with respect to the distance from the surface than can 9.2.1.4 For macro-Vickers tests with forces >1 kgf, see Test
be safely done with a single line of indents from the surface Method E92 for the recommended notation.
inward, or within the interior of the specimen. 9.3 Examples of the calculation of measurement uncertainty
are given in Test Method E92.
9. Report
9.1 Report the following information: 10. Precision and Bias
9.1.1 The number of tests and, where appropriate or
10.1 The precision and bias of microindentation hardness
required, the mean, standard deviation and 95% confidence
measurements depend on strict adherence to the stated test
interval for the tests. Due to the long history of hardness
procedure and are influenced by instrumental and material
calculations, and because the traditional kg/mm2 unit is not
factors and indentation measurement errors.
part of the SI system, the calculated numbers will be reported
without mention of the units. Also, due to the general unfamil- 10.2 The consistency of agreement for repeated tests on the
iarity of the metallurgical community with hardness numbers same material is dependent on the homogeneity of the material,
FIG. 3 Minimum Recommended Spacing for Knoop and Vickers Indentations
7
E384 − 17
reproducibility of the hardness tester, and consistent, careful bigger effect on the precision of the HV value than a larger
measurement of the indents by a competent operator. error in the test force or the face geometry. For the Knoop test,
10.3 Instrumental factors that can affect test results include: an error in measuring the long diagonal has a bigger influence
accuracy of loading; inertia effects; speed of loading; vibra- on the precision of the HK value than a larger error in the test
tions; the angle of indentation; lateral movement of the force. But, errors in the two face angles, Fig. 1, have a very
indenter or specimen; and, indentation and indenter shape significant effect on the precision of the HK value.
deviations. 10.8 Three separate interlaboratory studies have been con-
10.3.1 Vibrations during indenting will produce larger in- ducted in accordance with Practice E691 to determine the
dentations with the potential influence of vibrations becoming precision, repeatability, and reproducibility of this test method.
greater as the force decreases (2, 3). The three studies are defined as follows: (a) Knoop and Vickers
10.3.2 The angle between the indenter and specimen surface tests, six test forces in the micro range, twelve laboratories,
should be within 2° of perpendicular. Greater amounts of tilting manual measurements, and seven different hardness level
may produce non-uniform indentations and incorrect test specimens (see 10.8.1 and Appendix X1). Results were pub-
results. lished in 1989 (7, 8) and in ASTM Research Report RR:E04-
10.4 Material factors that can affect test results include: 1004.5(b) Knoop and Vickers tests, two test forces in the micro
specimen homogeneity, orientation or texture effects; improper range, seven laboratories, image analysis and manual
specimen preparation; low specimen surface reflectivity; and, measurements, four different hardness level specimens (see
transparency of the specimen. 10.8.2, Appendix X2 and ASTM Research Report RR:E04-
10.4.1 Residual deformation from mechanical polishing 1006).6(c) Knoop and Vickers tests, six test forces in the micro
must be removed, particularly for low-force (≤200 gf) testing. range, twenty-five laboratories, manual measurements, six
10.4.2 Distortion of the indentation shape, due to either different hardness level specimens (see 10.8.3, Appendix X3
crystallographic or microstructural texture, influences diagonal and ASTM Research Report RR:E04-1007).7
lengths and the validity of the calculated hardness. 10.8.1 An interlaboratory test program was conducted in
10.4.3 Plastic deformation during indentation can produce accordance with Practice E691 to develop information regard-
ridging around the indentation periphery that will affect diago- ing the precision, repeatability, and reproducibility of the
nal measurement accuracy. measurement of Knoop and Vickers indentations (supporting
10.4.4 Testing of etched surfaces, depending on the extent data have been filed at ASTM Headquarters; request RR:E04-
of etching, may produce results that are different from those 1004).5 The test forces were 25, 50, 100, 200, 500, and 1000 gf
obtained on unetched surfaces (2). on three ferrous and four nonferrous specimens (7, 8). Twelve
laboratories measured the indentations, five of each type at
10.5 Measurement errors that can affect test results include: each force on each sample. Additional details of this study are
inaccurate calibration of the measuring device; inadequate given in Appendix X1.
resolving power of the objective; insufficient magnification; 10.8.1.1 Tests of the three ferrous specimens revealed that
operator bias in sizing the indentations; poor image contrast; nine laboratories produced similar measurements while two
non-uniform illumination; and, improper zeroing of the mea- laboratories consistently undersized the indentations and one
suring device. laboratory consistently oversized the indentations; that is,
10.5.1 The accuracy of microindentation hardness testing is biased results were produced. These latter results were most
strongly influenced by the accuracy to which the indentations pronounced as the force decreased and specimen hardness
can be measured. increased (that is, as the diagonal size decreased) and were
10.5.2 The error in measuring the diagonals increases as the observed for both Vickers and Knoop indentations. Results for
numerical aperture of the measuring objective decreases (4, 5). the lower hardness nonferrous indentations produced better
In general, indents <30 µm in length should be measured with agreement. However, none of the laboratories that obtained
objectives having greater magnification than 40 or 50×. Image higher or lower results on the ferrous specimens measured the
contrast between the indent and the specimen is critical for nonferrous indentations.
precise measurement of diagonal length. 10.8.1.2 Repeatability Interval—The difference due to test
10.5.3 Bias is introduced if the operator consistently under- error between two test results in the same laboratory on the
sizes or over-sizes the indentations. same material increases with increasing specimen hardness and
10.6 Some of the factors that affect test results produce with decreasing test force (see X1.4.4).
systematic errors that influence all test results while others 10.8.1.3 Reproducibility Interval—The difference in test
primarily influence low-force (≤25 gf) test results (6). Some of results on the same material tested in different laboratories
these problems occur continually, others may occur in an
undefined, sporadic manner. Low-force hardness tests are 5
Supporting data have been filed at ASTM International Headquarters and may
influenced by these factors to a greater extent than higher force be obtained by requesting Research Report RR:E04-1004. Contact ASTM Customer
Service at [email protected].
tests. 6
10.7 For both the Vickers and Knoop hardness tests, the be obtained by requesting Research Report RR:E04-1006. Contact ASTM Customer
Service at [email protected].
calculated microindentation hardness is a function of three 7
variables: force, indenter geometry and diagonal measurement. be obtained by requesting Research Report RR:E04-1007. Contact ASTM Customer
For the Vickers test, the error in measuring the diagonals has a Service at [email protected].
8
E384 − 17
increased with increasing specimen hardness and with decreas- made by two different test methods. Hence, it is not possible to
ing test force (see X1.4.5). statistically and accurately compare the hardness measure-
10.8.1.4 The within-laboratory and between-laboratory pre- ments made by the manual and automated procedures.
cision values improved as specimen hardness decreased and However, this information is graphically represented for com-
test force increased. The repeatability interval and reproduc- parative purposes, X2.6.
ibility interval were generally larger than the precision 10.8.3 Tests of six ferrous alloys with hardness values of
estimate, particularly at low test forces and high specimen <20 HRC, 30, 40, 50, 60 and 67 HRC were tested using Knoop
hardness. and Vickers tests at a variety of test forces, usually 25, 50, 100,
10.8.2 An interlaboratory test program was conducted in 300, 500 and 1000 gf (except that the lowest test forces for
accordance with Practice E691 to develop information regard- Vickers tests of the 60 and 67 HRC specimens were not
ing the repeatability and reproducibility of Knoop and Vickers performed). Twenty-five different laboratories tested the steels
measurements made with automated image analysis systems using the Vickers test while thirteen different laboratories
compared to measurements by manual procedures. Four fer- tested the steels using the Knoop test. Additional details of this
rous specimens were used in the round robin. The tests were study are given in Appendix X3.
conducted at 100 gf and 300 gf. The participants in the test
program measured the same indentations on the four speci- 10.8.3.1 Repeatability and reproducibility statistics were
mens. Seven labs measured the specimens using both proce- determined for the Knoop and Vickers diagonal measurements.
dures. The Knoop indentations on specimen C1 were too long Results are tabulated in Table X3.1 and Table X3.2 and are
for accurate measurements to be made by one lab; hence, only shown graphically in Fig. X3.1 and Fig. X3.2.
six sets of measurements were made on this specimen. Near the 10.8.3.2 Repeatability and reproducibility statistics were
end of the test program, specimen B1 was lost in shipping; thus determined for the Knoop and Vickers hardness values. Results
only six sets of measurements were made on this specimen. are tabulated in Table X3.3 and Table X3.4 and are shown
Additional details of the study are contained in Appendix X2. graphically in Fig. X3.3 and Fig. X3.4.
10.8.2.1 Repeatability concerns the variability between in-
dividual test results obtained within a single laboratory by a 11. Conversion to Other Hardness Scales or Tensile
single operator with a specific set of test apparatus. For both Strength Values
the manual and automated measurements, the repeatability
11.1 There is no generally accepted method for precise
interval increased with specimen hardness and decreasing test
conversion of Knoop or Vickers microindentation hardness
force, Appendix X2. For equivalent testing conditions, the
numbers to other hardness scales or tensile strength values.
repeatability interval for automated measurements was slightly
Such conversions are empirical and are limited in precision and
larger than for manual measurements.
should be used with caution, except for special cases where a
10.8.2.2 Reproducibility deals with the variability between
reliable basis for the conversion has been obtained by com-
single test results obtained by different laboratories applying
parison tests. For loads ≥ 25 gf microindentation Vickers
the same test methods to the same or similar test specimens.
hardness numbers are in statistical agreement with macro-
For both the manual and automated measurements, the repro-
ducibility interval increased with specimen hardness and de- Vickers hardness numbers. Refer to Standard Hardness Con-
creasing test force, Appendix X2. For equivalent testing version Tables in E140.
conditions, the reproducibility interval for automated measure-
ments was slightly larger than for manual measurements. 12. Keywords
10.8.2.3 Neither Practice E691, nor any other ASTM 12.1 hardness; indentation; Knoop; microindentation; Vick-
standard, deals with comparing test results of a single property ers
ANNEXES
(Mandatory Information)
A1. VERIFICATION OF KNOOP AND VICKERS HARDNESS TESTING MACHINES AND INDENTERS
A1.1 Scope ing the consistency of microindentation measurements based

A1.1.1 Annex A1 specifies three types of procedures for on the periodic verification tests and detecting measurement
verifying microindentation (Knoop and Vickers) hardness test- deviations is described in Practices E2554 and E2587.
ing machines: direct verification, indirect verification, and A1.1.2 Direct verification is a process normally performed
periodic verification. This annex also contains geometric speci- by the manufacture for verifying that critical components of the
fications for the indenter. A control chart method for monitor- hardness testing machine are within allowable tolerances by
9
E384 − 17
direct measurement of the applied test forces, the indentation formed in accordance with the schedule given in Table A1.1 for
measuring system, and the testing cycle. For additional infor- each microindentation hardness indenter that will be used.
mation about direct verification see Test Method E92. A1.3.2 It is recommended that the periodic verification
A1.1.3 Indirect verification is a process performed by the procedures be performed whenever the indenter is changed,
user of the machine, or by an outside certification agency, to that is, if one indenter is physically removed from the port and
periodically verify the performance of the testing machine by another is inserted into its place. This is not required with
means of standardized test blocks. For additional information machines that have both types of indenter mounted on the same
about the indirect verification procedure, see Test Method E92. turret. It is also recommended to perform a periodic verifica-
A1.1.4 The periodic (formerly called “weekly”) verification tion when loads are changed (to verify that the load is not
is a process for monitoring the performance of the testing “hanging up”).
machine between indirect verifications by means of standard- A1.3.3 Periodic Verification Procedures—The procedure to
ized test blocks and is performed by the user. use when performing a periodic verification is as follows.
A1.3.3.1 At least one standardized test block that meets the
A1.2 General Requirements requirements of Annex A2 shall be used for each microinden-
A1.2.1 The testing machine shall be verified at specific tation hardness indenter to be used. When test blocks are
instances and at periodic intervals as specified in Table A1.1, commercially available, the hardness level of the test blocks
and when circumstances occur that may affect the performance shall be chosen at approximately the same hardness value as
of the testing machine. See Annex A1 in Test Method E92 for the material to be measured. If various hardness ranges are to
interval details for direct and indirect verifications. be made, it is recommended to take a test block from each
A1.2.2 All instruments used to make measurements re- range of hardness as described in Table A1.2.
quired by this Annex shall be calibrated traceable to national A1.3.3.2 The indenter to be used for the periodic verifica-
standards when a system of traceability exists, except as noted tion shall be the indenter that is normally used for testing.
otherwise. A1.3.3.3 Before performing the periodic verification tests,
ensure that the testing machine is working freely, the stage and
A1.2.3 Periodic verification and the indirect verification of test block are clean, and the measuring device is properly
the testing machine shall be performed at the location where adjusted and zeroed.
the tester is used. A1.3.3.4 Make at least three hardness measurements on
A1.2.4 Direct verification of newly manufactured or rebuilt each of the verification test blocks. The tests shall be distrib-
testing machines may be performed at the place of uted uniformly over the surface of the test blocks.
manufacture, rebuild or the location of use. Details of this A1.3.3.5 Let d̄ be the average of the measurements. Deter-
procedure can be found in Test Method E92. mine the error E and the repeatability R in the performance of
NOTE A1.1—It is recommended that the calibration agency that is used the testing machine using Eq 10 and Eq 11 from 3.4 for each
to conduct the verifications of microindentation hardness testing machines standardized test block that is measured.
be accredited to the requirements of ISO 17025 (or an equivalent) by a (1) If the error E and the repeatability R calculated for each
recognized accrediting body that operates to the requirements of ISO
Guide 58. test block is within the tolerances given in Table A1.3, the
testing machine with the indenter may be regarded as perform-
A1.2.5 Verification of Indenter—The geometry of the in-
ing satisfactorily.
denter is verified at the time of manufacturing and it is
(2) If the error E and the repeatability R calculated for any
mandatory for new machines. Subsequent verifications of the
of the test blocks is outside the tolerances, the periodic
indenter are performed by visual inspection of the resulting
verification may be repeated with a different indenter. If the
indentation; it is usually sufficient for the user to verify the
average of the hardness measurements again falls outside of
absence of defects from the shape of indentations performed on
tolerances for any of the test blocks, an indirect verification
test blocks. Details of this process are given in Test Meth-
shall be performed.
odE92.
A1.3.3.6 If a testing machine fails a periodic verification,
A1.3 Periodic Verification the hardness tests made since the last valid periodic verification
may be suspect.
A1.3.1 The periodic (formerly known as the “weekly”)
verification is intended as a tool for the user to monitor the NOTE A1.2—It is highly recommended that the results obtained from
performance of the testing machine between indirect verifica- the periodic verification testing be recorded using accepted Statistical
Process Control techniques, such as, but not limited to, X-bar (measure-
tions. At a minimum, the periodic verification shall be per- ment averages) and R-charts (measurement ranges), and histograms (see
Practices E2554 and E2587).
TABLE A1.1 Verification Schedule for a Microindentation
Hardness Testing Machine
TABLE A1.2 Hardness Ranges Used for Periodic Verification
Verification
Schedule
Procedure Range Knoop Vickers
Periodic Verification Required each week that the machine is used. Low < 250 < 240
Recommended whenever the indenter is physically Mid 250–650 240–600
removed and replaced by another indenter. High > 650 > 600
10
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TABLE A1.3 Repeatability and Error of Test Machines— Periodic Verification by Standardized Test Blocks Based on Measured
Diagonal LengthsA
R E
Hardness Range of Force, Maximum Maximum
Standardized Test Blocks gf Repeatability Error
(%) (%)
Knoop Vickers
HK > 0 HV > 0 1 # F <100 13 3

HK < 100 HV < 100 100 # F # 1000 13 3
100 # HK # 250 100 # HV # 240 100 # F < 500 13 2

250 < HK # 650 240 < HV # 600 5 2
HK > 650 HV > 600 4 2
100 # HK # 250 100 # HV # 240 500 # F # 1000 8 2

250 < HK # 650 240 < HV # 600 4 2
HK > 650 HV > 600 3 2
A
In all cases, the repeatability is the greater of the percentage given or 1 µm; the maximum error is the greater of the value obtained or 0.5 µm.
A1.4 Verification Report (2) Means of verification (test blocks, elastic proving
A1.4.1 A verification report is required for direct and devices, etc.) with statements defining traceability to a national
indirect verifications. A verification report is not required for a standard.
periodic verification. Additional details concerning creation of (3) The microindentation hardness scale(s) verified.
the verification report can be found in Test Method E92. (4) The individual or calculated results used to determine
whether the testing machine meets the requirements of the
A1.4.2 The verification report shall be produced by the
verification performed. Measurements made to determine the
person performing the verification and include the following
information when available as a result of the verification as-found condition of the testing machine shall be included
performed. whenever they are made.
A1.4.2.1 Full details of the verification report can be found (5) Description of adjustments or maintenance done to the
in Test Method E92. testing machine.
A1.4.2.2 The basic components of the verification report, as (6) Date of verification and reference to the verifying
defined in detail in Test Method E92, are summarized below. agency or department.
(1) Identification of the hardness testing machine and the (7) Signature of the person performing the verification.
indenters used.
A2. CALIBRATION OF STANDARDIZED HARDNESS TEST BLOCKS FOR MICROINDENTATION HARDNESS

TEST MACHINES
A2.1 Scope A2.2 Certification of Standardized Test Block

A2.1.1 The calibration of standardized hardness test blocks A2.2.1 The certificate accompanying each standardized
used to verify microindentation hardness test machines is hardness test block shall include the following information: the
described in Test Method E92. The standardizing machine shall arithmetic mean of each group of five impression diagonals;
meet the direct verification method described in Test Method the arithmetic mean and standard deviation of all impression
E92.
diagonals, the corresponding hardness value, the test force,
A2.1.2 Re-polishing of the test block will invalidate the serial number of the test block, name of the manufacturer and
standardization and is not recommended. Cleaning of the certifying organization, magnification used, and the date.
polished test block surface is often required in normal usage
but must not alter the hardness or quality of the polished test
surface.
11
E384 − 17
APPENDIXES
(Nonmandatory Information)
X1. RESULTS OF INTERLABORATORY TEST OF THE MEASUREMENT OF MICROINDENTATIONS
X1.1 Introduction hardness. For specimens below about 300 HV, there was
X1.1.1 This interlaboratory test program (7, 8) was con- relatively little difference in HV over the test force range.
ducted to develop precision and bias estimates for the mea- X1.4.3 For the Knoop test data, most of the laboratories
surement of both Knoop and Vickers indentations using forces agreed that the hardness decreased continually with increasing
of 25 to 1000 gf for ferrous and nonferrous specimens covering test force and then became reasonably constant. However, the
a wide range of hardness (see Research Report RR:E04- two laboratories that exhibited outlier data for the ferrous
1004).5 specimens did show the opposite trend; this is highly unusual.
X1.2 Scope The difference in HK values between low forces and high
forces increased with increasing specimen hardness. For speci-
X1.2.1 This interlaboratory test program provides informa- mens with hardness below about 300 HK, the difference in
tion on the measurement of the same indentations by different hardness was quite small over the test force range.
laboratories according to the procedures of Practice E691.
X1.4.4 Repeatability Interval—The difference due to test
X1.3 Procedure error between two test results in the laboratory on the same
X1.3.1 Five indentations were made under controlled con- material was calculated using the (Sr)j values, the pooled
ditions at each force (25, 50, 100, 200, 500, and 1000 gf), with within-laboratory standard deviation. (Sr)j increased with di-
both Knoop and Vickers indenters using three ferrous and four agonal size and the relationship varied for each material and
nonferrous specimens. test type. Table X1.1 lists regression equations that show the
relationship between (Sr)j and the diagonal length, µm. The
X1.3.2 Twelve laboratories measured the indentations on
the ferrous specimens and the nonferrous specimens. Two repeatability interval (Ir)j, was calculated based on the rela-
laboratories measured the hardness of both groups. tionships in Table X1.1. Because the repeatability intervals are
also a function of diagonal length, regression equations were
X1.3.3 Each laboratory used the same stage micrometer to also calculated, Table X1.2. The repeatability intervals, in
calibrate their measuring device. terms of Knoop and Vickers values for ferrous and nonferrous
X1.3.4 Results were tabulated and analyzed in accordance specimens, are shown in Figs. X1.1-X1.4.
with Practice E691.
X1.4.5 Reproducibility Interval—The difference in test re-
X1.4 Results sults on the same material in different laboratories was calcu-
lated using the (SR)j values, the between-laboratory estimate of
X1.4.1 For the three ferrous specimens, results from nine
precision. (SR)j increased with diagonal size and the relation-
laboratories showed general agreement as to the diagonal sizes.
ship varied for each material and test type. Table X1.3 lists the
Two other laboratories consistently undersized the indentations
regression equations that show the relationship between (SR)j
(higher hardness) and one laboratory consistently oversized the
and the diagonal length, µm. The reproducibility intervals (IR)j,
indentations (lower hardness). This bias was observed with
both Vickers and Knoop indentations sized by these laborato- were calculated based on the relationships shown in Table
ries with the degree of bias increasing as the indentation size X1.3. Because the reproducibility intervals are also a function
decreased and the specimen hardness increased. Test on the of diagonal length, regression equations were also calculated,
four nonferrous specimens produced general agreement, but Table X1.4. The reproducibility intervals, in terms of Knoop
none of the three laboratories that produced biased results for and Vickers values for the ferrous and nonferrous specimens,
the ferrous specimens measured the nonferrous specimens. are shown in Figs. X1.1-X1.4.
X1.4.2 For the Vickers test data, the calculated hardness X1.4.6 The within-laboratory and between-laboratory pre-
increased with increasing force and then became reasonably cision values were calculated from (Vr(%))j and (VL(%))j
constant. This trend was apparent in the data from the nine which are the coefficients of variation for within-laboratory and
consistent laboratories (ferrous specimens) and for the labora- between-laboratory tests. Both are a function of the length of
tory that oversized the indentations. The two laboratories that the diagonal. The within-laboratory and between-laboratory
consistently undersized the Vickers indentations exhibited precision values were relatively similar for both Vickers and
substantial data scatter for the tests with forces of less than 100 Knoop test data, either ferrous or nonferrous. In general, the
gf. However for higher forces, their indentation measurements repeatability intervals and reproducibility intervals were larger
were relatively constant. The force at which the hardness than the precision estimates, particularly at low test forces and
became relatively constant increased with increasing specimen high specimen hardness.
12
E384 − 17
TABLE X1.1 Relationship Between Diagonal Length and (Sr)j, the
Pooled Within-Laboratory Standard Deviation
Correlation
Material Test Regression Equation
Coefficient
Ferrous Vickers (Sr)j = 0.231 + 0.00284 d̄1 0.535
Ferrous Knoop (Sr)j = 0.216 + 0.006 d̄1 0.823
Nonferrous Vickers (Sr)j = 0.373 + 0.008 d̄1 0.862
Nonferrous Knoop (Sr)j = 0.057 + 0.0177 d̄1 0.8196
TABLE X1.2 Relationship Between the Diagonal Length and (Ir)j,

the Repeatability Interval
Ferrous Vickers (Ir)j = 0.653 + 0.008 d̄1
Ferrous Knoop (Ir)j = 0.614 + 0.017 d̄1
Nonferrous Vickers (Ir)j = 1.0556 + 0.0226 d̄1
Nonferrous Knoop (Ir)j = 0.161 + 0.05 d̄1
FIG. X1.1 Repeatability and Reproducibility Intervals in Terms of Vickers Hardness (6) for the Ferrous Sample as a Function of Test
Load and Specimen Hardness
FIG. X1.2 Repeatability and Reproducibility Intervals in Terms of Knoop Hardness (6) for the Ferrous Samples as a Function of Test
13
E384 − 17
FIG. X1.3 Repeatability and Reproducibility Intervals in Terms of Vickers Hardness (6) for the Nonferrous Samples as a Function of
Test Load and Specimen Hardness
FIG. X1.4 Repeatability and Reproducibility Intervals in Terms of Knoop Hardness (6) for the Nonferrous Samples as a Function of Test
14
E384 − 17
TABLE X1.3 Relationship Between Diagonal Length and (SR)j, the
Between-Laboratory Estimate of Precision
Correlation
Coefficient
Ferrous Vickers (SR)j = 0.31 + 0.004 d̄1 0.747
Ferrous Knoop (SR)j = 0.333 + 0.007 d̄1 0.899
Nonferrous Vickers (SR)j = 0.357 + 0.0156 d̄1 0.8906
Nonferrous Knoop (SR)j = 0.378 + 0.0177 d̄1 0.8616
TABLE X1.4 Relationship Between the Diagonal Length and (IR)j,

the Repeatability Interval
Ferrous Vickers (IR)j = 0.877 + 0.0113 d̄1
Ferrous Knoop (IR)j = 0.946 + 0.0198 d̄1
Nonferrous Vickers (IR)j = 1.0103 + 0.0441 d̄1
Nonferrous Knoop (IR)j = 1.07 + 0.05 d̄1
X2. RESULTS OF AN INTERLABORATORY TEST COMPARING MICROINDENTATION HARDNESS TESTING USING

MANUAL AND AUTOMATED MEASURING SYSTEMS
X2.1 Introduction X2.4 Repeatability

X2.1.1 An interlaboratory test program was conducted to X2.4.1 Repeatability concerns the variability between indi-
develop information comparing Knoop and Vickers microin- vidual test results obtained within a single laboratory by a
dentation hardness tests made with measurements using auto- single operator with a specific set of test apparatus. For both
the manual and automated measurements, the repeatability
mated image analysis systems and by the standard manual
interval increased with specimen hardness and decreasing test
procedure. Four ferrous specimens were used in the test
force, Tables X2.1-X2.4, and Figs. X2.1-X2.4. For equivalent
program (see Research Report RR:E04-1006).6 testing conditions, the repeatability interval for automated
measurements was slightly larger than for manual measure-
X2.2 Scope ments.
X2.2.1 This interlaboratory test program provides informa- X2.5 Reproducibility
tion on measurements of the same indentations made by
X2.5.1 Reproducibility deals with the variability between
different laboratories using two different measuring methods
single test results obtained by different laboratories applying
according to the procedures of Practice E691. the same test methods to the same or similar test specimens.
For both the manual and automated measurements, the repro-
X2.3 Procedure ducibility interval increased with specimen hardness and de-
X2.3.1 The test was conducted under controlled conditions creasing test force, Tables X2.1-X2.4, and Figs. X2.1-X2.4.
using loads of 100 gf and 300 gf. Ten Knoop and ten Vickers For equivalent testing conditions, the reproducibility interval
indentations were made for each load, a total of 40 indenta- for automated measurements was slightly larger than for
tions. The participants in the test program measured the same manual measurements.
indentations on the four specimens. Seven laboratories mea- X2.6 Comparisons
sured the specimens using both procedures. The results of these X2.6.1 Neither Practice E691, nor any other ASTM
seven sets of measurements were used for the analysis. The standard, deals with comparing test results of a single property
Knoop indentations on specimen C1 were too long for accurate made by two different test methods. Hence, it is not possible to
measurements to be made by one lab; hence, only six sets of statistically and accurately compare the hardness measure-
measurements were made on this specimen. Near the end of the ments made by the manual and automated procedures.
test program, specimen B1 was lost in shipping; thus only six However, this information is graphically represented for com-
sets of measurements were made on this specimen. parative purposes, Figs. X2.5-X2.8.
15
E384 − 17
TABLE X2.1 Precision Statistics for Manual and Automated Knoop Tests at 100 gf Load
Manual
Spec. Labs Mean Sx Sr SR r R
C1 7 228.62 6.88 9.30 11.18 26.03 31.32
D1 7 344.80 10.54 9.80 14.06 27.44 39.36
A2 7 491.48 28.67 14.87 31.95 41.63 89.45
B1 6 901.67 62.40 21.17 65.55 59.28 183.55
Automated
C1 7 232.07 7.29 9.54 11.62 26.72 32.55
D1 7 348.97 10.74 9.54 14.04 26.70 39.32
A2 7 510.13 30.35 19.53 35.56 54.69 99.56
B1 6 914.72 57.82 29.22 64.13 81.83 179.56
TABLE X2.2 Precision Statistics for Manual and Automated Knoop Tests at 300 gf Load
Manual
C1 6 215.81 5.49 7.66 9.10 21.44 25.49
D1 7 330.64 6.99 7.49 9.97 20.98 27.92
A2 7 466.95 17.99 11.45 21.02 32.06 58.85
B1 6 827.47 20.41 16.13 25.51 45.16 71.43
Automated
C1 6 217.82 5.73 6.87 8.68 19.24 24.31
D1 7 335.76 12.23 8.22 14.50 23.03 40.61
A2 7 476.97 23.46 10.56 25.51 29.58 71.44
B1 6 821.00 24.62 10.89 26.70 30.50 74.76
TABLE X2.3 Precision Statistics for Manual and Automated Vickers Tests at 100 gf Load
Manual
C1 7 205.31 6.36 6.82 9.07 19.10 25.40
D1 7 299.52 6.07 7.65 9.46 21.43 26.50
A2 7 482.76 21.58 12.29 24.53 34.42 68.69
B1 6 821.56 46.01 24.02 51.35 67.25 143.77
Automated
C1 7 203.30 6.94 6.47 9.27 18.12 25.95
D1 7 299.78 14.36 5.23 15.19 14.63 42.54
A2 7 482.86 32.07 16.50 35.69 46.19 99.93
B1 6 808.17 47.72 21.30 51.82 59.63 145.09
TABLE X2.4 Precision Statistics for Manual and Automated Vickers Tests at 300 gf Load
Manual
C1 7 197.07 3.40 5.32 6.09 14.91 17.06
D1 7 298.91 5.47 7.38 8.89 20.68 24.89
A2 7 474.58 18.00 12.45 21.53 34.86 60.28
B1 6 810.60 29.67 16.50 33.55 46.21 93.94
Automated
C1 7 196.37 6.44 5.57 8.33 15.60 23.32
D1 7 297.88 10.42 6.69 12.20 18.72 34.15
A2 7 483.72 18.96 12.30 22.26 34.44 62.34
B1 6 809.55 20.55 11.60 23.31 32.49 65.27
16
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FIG. X2.1 Reproducibility of the Knoop 100 gf Manual and Automated Microindentation Hardness Tests
FIG. X2.2 Reproducibility of the Knoop 300 gf Manual and Automated Microindentation Hardness Tests
17
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FIG. X2.3 Reproducibility of the Vickers 100 gf Manual and Automated Microindentation Hardness Tests
FIG. X2.4 Reproducibility of the Vickers 300 gf Manual and Automated Microindentation Hardness Tests
18
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FIG. X2.5 Comparison between Knoop 100 gf Manual and Automated Microindentation Hardness Tests
FIG. X2.6 Comparison between Knoop 300 gf Manual and Automated Microindentation Hardness Tests
19
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FIG. X2.7 Comparison between Vickers 100 gf Manual and Automated Microindentation Hardness Tests
FIG. X2.8 Comparison between Vickers 300 gf Manual and Automated Microindentation Hardness Tests
X3. RESULTS OF INTERLABORATORY TEST OF THE MEASUREMENT OF MICROINDENTATIONS
X3.1 Introduction X3.2.2 The precision statement was determined through

statistical examination of results from twenty-five laboratories,
X3.1.1 The interlaboratory program was conducted on
on six ferrous materials. These six ferrous materials were
steels to develop precision statistics for Knoop and Vickers
described as:
tests (see Research Report RR:E04-1007).7
Specimen A: H13, mill annealed, hardness less than 20 HRC
Specimen B: H13, austenitized, quenched, and tempered to ~ 50 HRC
X3.2 Scope Specimen C: H13, austenitized, quenched, and tempered to ~ 40 HRC
Specimen D: H13, austenitized, quenched, and tempered to ~ 30 HRC
X3.2.1 Twenty five laboratories tested six steel specimens Specimen E: O1, austenitized, quenched and tempered O1 steel to ~ 60 HRC
for Vickers hardness and thirteen laboratories tested the six Specimen T: T15, P/M, austenitized, quenched and tempered to ~ 67 HRC
steel specimens for Knoop hardness, all as a function of test NOTE X3.1—To judge the equivalency of two test results, it is
forces ranging from 25 to 1000 gf, except for the hardest recommended to choose the material closest in characteristics to the test
specimens. material.
20
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X3.3 Results for that material; “R” is the interval representing the critical
X3.3.1 Details of this study can be obtained from ASTM; difference between two test results for the same material,
request Research Report RR:E04-1006.6 obtained by different operators using different equipment in
different laboratories.
X3.3.2 Repeatability limit (r)—Two test results obtained
within one laboratory were judged not equivalent if they X3.3.5 Reproducibility limits in diagonal lengths (µm) are
differed by more than the “r” value for that material; “r” is the listed in Table X3.1 and Table X3.2 and Fig. X3.1 and Fig.
interval representing the critical difference between two test X3.2 and in hardness units (HK, HV) in Table X3.3 and Table
results for the same material, obtained by the same operator X3.4 and Fig. X3.3 and Fig. X3.4.
using the same equipment on the same day in the same X3.3.6 The above terms (repeatability limit and reproduc-
laboratory. ibility limit) are used as specified in Practice E177.
X3.3.3 Repeatability limits in diagonal lengths (µm) are X3.3.7 Any judgment in accordance with statements X3.3.2
listed Table X3.1 and Table X3.2 and in hardness units (HK, and X3.3.4 would have an approximate 95% probability of
HV) in Table X3.3 and Table X3.4. being correct.
X3.3.4 Reproducibility limit (R)—Two test results shall be X3.3.8 The data are listed in Tables 1-4. and are shown
judged not equivalent if they differ by more than the “R” value graphically in Figs. 1- 4.
TABLE X3.1 Precision Statistics for an Interlaboratory Study of the Knoop Microindentation Hardness Test for Ferrous Specimens in
Diagonal Units (µm)
Specimen Test Force Average Standard Repeatability Reproducibility Repeatability Reproducibility
(gf) Diagonal Deviation Standard Standard Limit (µm) Limit (µm)
(µm) (µm) Deviation Deviation
(µm) (µm)
d̄ Sx Sr SR r R
A 25 35.61 1.40 0.72 1.54 2.00 4.31
50 51.77 1.33 1.11 1.66 3.12 4.66
100 74.84 1.65 1.77 2.28 4.95 6.40
300 132.28 2.63 2.57 3.50 7.20 9.79
500 171.51 2.07 2.46 3.02 6.89 8.45
1000 243.11 1.72 2.96 3.16 8.29 8.84
B 25 23.66 0.95 0.48 1.04 1.34 2.91
50 34.33 0.94 0.56 1.07 1.57 2.99
100 49.61 1.12 0.65 1.26 1.82 3.54
300 88.64 1.39 0.88 1.59 2.45 4.46
500 115.48 1.68 1.11 1.95 3.11 5.46
1000 164.38 1.65 1.52 2.14 4.25 5.98
C 25 27.62 1.33 0.49 1.41 1.38 3.93
50 39.47 1.14 0.50 1.22 1.39 3.43
100 56.66 1.05 0.64 1.20 1.79 3.35
300 100.14 1.25 0.81 1.44 2.26 4.03
500 130.19 1.50 0.83 1.68 2.33 4.69
1000 184.84 1.79 1.19 2.08 3.33 5.82
D 25 31.04 1.04 0.46 1.11 1.28 3.12
50 44.64 0.85 0.46 0.95 1.30 2.65
100 64.22 1.08 0.67 1.24 1.89 3.47
300 113.94 0.94 0.82 1.19 2.29 3.33
500 148.16 1.16 0.74 1.33 2.06 3.73
1000 210.10 2.03 1.64 2.50 4.58 7.00
E 25 20.02 0.72 0.48 0.84 1.36 2.34
50 29.03 1.00 0.48 1.09 1.34 3.05
100 42.21 1.15 0.52 1.24 1.46 3.46
300 76.03 1.00 0.53 1.11 1.48 3.10
500 99.25 1.06 0.49 1.15 1.37 3.21
1000 141.67 1.27 0.85 1.48 2.39 4.15
T 25 17.14 0.88 0.48 0.98 1.35 2.76
50 25.59 1.03 0.47 1.12 1.32 3.12
100 37.20 1.45 0.52 1.52 1.46 4.26
300 67.43 1.39 0.65 1.51 1.82 4.22
500 88.27 1.11 0.66 1.26 1.85 3.53
1000 126.96 1.47 0.75 1.61 2.09 4.52
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TABLE X3.2 Precision statistics for an Interlaboratory Study of the Vickers Microindentation Hardness Test for Ferrous Specimens in
Diagonal Units (µm)
(gf) Diagonal Deviation Standard Standard Limit (µm) Limit (µm)
(µm) (µm) Deviation Deviation
(µm) (µm)
d̄ Sx Sr SR r R
A 25 13.89 0.75 0.30 0.80 0.85 2.24
50 19.81 0.61 0.34 0.68 0.95 1.91
100 28.10 0.57 0.45 0.70 1.26 1.96
300 49.19 0.75 0.72 0.99 2.02 2.77
500 63.65 0.81 0.88 3.16 2.47 1.13
1000 90.48 0.98 1.31 1.53 3.66 4.28
B 25 9.35 0.40 0.25 0.46 0.69 1.28
50 13.06 0.37 0.23 0.42 0.63 1.18
100 18.51 0.39 0.39 0.52 1.09 1.47
300 32.11 0.43 0.30 0.50 0.84 1.41
500 41.68 0.51 0.36 0.60 1.00 1.69
1000 59.21 0.55 0.52 0.72 1.46 2.03
C 25 10.81 0.53 0.19 0.56 0.54 1.56
50 15.13 0.42 0.20 0.46 0.57 1.29
100 21.34 0.40 0.22 0.45 0.62 1.25
300 36.85 0.38 0.21 0.43 0.59 1.20
500 47.68 0.55 0.24 0.59 0.67 1.64
1000 67.60 0.58 0.33 0.65 0.93 1.83
D 100 24.50 0.43 0.29 0.50 0.82 1.40
300 42.52 0.41 0.28 0.48 0.80 1.35
500 55.02 0.50 0.25 0.55 0.70 1.54
1000 78.14 0.70 0.34 0.77 0.97 2.15
E 100 15.61 0.40 0.18 0.43 0.52 1.20
300 27.25 0.41 0.25 0.46 0.70 1.30
500 35.26 0.43 0.20 0.46 0.55 1.30
1000 50.06 0.41 0.24 0.46 0.67 1.29
T 300 23.94 0.47 0.17 0.49 0.49 1.38
500 31.00 0.51 0.21 0.55 0.59 1.53
1000 44.12 0.50 0.25 0.55 0.69 1.53
22
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TABLE X3.3 Precision statistics for an Interlaboratory Study of the Knoop Microindentation Hardness Test for Ferrous Specimens in
Hardness units (HK)
Diagonal Deviation Standard Standard Limit (HK) Limit (HK)
(µm) (HK) Deviation Deviation
(HK) (HK)
(gf) d Sx Sr SR r R
A 25 35.61 22.07 11.35 24.29 31.56 68.41
50 51.77 13.64 11.39 17.03 32.05 47.98
100 74.84 11.20 12.02 15.49 33.68 43.61
300 132.28 9.70 9.48 12.91 26.60 36.21
500 171.51 5.84 6.94 8.52 19.45 23.86
1000 243.11 3.41 5.86 6.26 16.43 17.52
B 25 23.66 51.07 25.79 55.92 72.09 157.50
50 34.33 33.07 19.70 37.65 55.27 105.55
100 49.61 26.11 15.15 29.38 42.45 82.72
300 88.64 17.04 10.79 19.49 30.04 54.74
500 115.48 15.52 10.26 18.02 28.75 50.50
1000 164.38 10.57 9.74 13.71 27.24 38.34
C 25 27.62 44.96 16.55 47.67 46.65 134.05
50 39.47 26.39 11.57 28.24 32.19 79.67
100 56.66 16.43 10.01 18.78 28.02 52.50
300 100.14 10.63 6.89 12.24 19.22 34.29
500 130.19 9.67 5.35 10.83 15.03 30.26
1000 184.84 8.07 5.36 9.37 15.01 26.24
D 25 31.04 24.75 10.94 26.42 30.48 74.60
50 44.64 13.60 7.36 15.20 20.80 42.46
100 64.22 11.61 7.20 13.33 20.32 37.34
300 113.94 5.43 4.73 6.87 13.22 19.23
500 148.16 5.08 3.24 5.82 9.01 16.32
1000 210.10 6.23 5.03 7.67 14.06 21.49
E 25 20.02 63.88 42.57 74.54 120.86 208.90
50 29.03 58.20 27.92 63.44 78.02 178.37
100 42.21 43.53 19.68 46.94 55.28 131.37
300 76.03 19.43 10.30 21.56 28.76 60.27
500 99.25 15.43 7.13 16.74 19.94 46.74
1000 141.67 12.71 8.51 14.81 23.92 41.55
T 25 17.14 124.50 67.85 138.69 191.33 395.07
50 25.59 87.53 39.91 95.19 112.23 266.90
100 37.20 80.22 28.75 84.10 80.77 237.05
300 67.43 38.71 18.10 42.06 50.70 117.74
500 88.27 22.97 13.65 26.07 38.28 73.09
1000 126.96 20.44 10.43 22.39 29.07 62.90
23
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TABLE X3.4 Precision statistics for an Interlaboratory Study of the Vickers Microindentation Hardness Test for Ferrous Specimens in
Hardness units (HV)
Diagonal Deviation Standard Standard Limit (HV) Limit (HV)
(µm) (HV) Deviation Deviation
(HV) (HV)
(gf) d Sx Sr SR r R
A 25 13.89 25.99 10.38 27.73 29.46 78.52
50 19.81 14.56 8.11 16.23 22.69 45.77
100 28.10 9.53 7.52 11.70 21.08 32.84
300 49.19 7.01 6.73 9.26 18.90 25.94
500 63.65 5.83 6.33 22.75 17.78 8.13
1000 90.48 4.91 6.56 7.66 18.34 21.45
B 25 9.35 45.41 28.37 52.24 78.48 146.56
50 13.06 30.81 19.15 34.98 52.51 98.63
100 18.51 22.81 22.81 30.42 63.85 86.24
300 32.11 14.45 10.08 16.81 28.24 47.43
500 41.68 13.06 9.22 15.37 25.62 43.32
1000 59.21 9.83 9.29 12.87 26.09 36.29
C 25 10.81 38.95 13.95 41.16 39.69 115.71
50 15.13 22.50 10.71 24.64 30.54 69.32
100 21.34 15.27 8.40 17.18 23.67 47.79
300 36.85 8.45 4.67 9.56 13.12 26.70
500 47.68 9.41 4.11 10.09 11.46 28.07
1000 67.60 6.96 3.96 7.80 11.17 21.98
D 100 24.50 10.85 7.31 12.61 20.69 35.36
300 42.52 5.93 4.05 6.95 11.58 19.55
500 55.02 5.57 2.78 6.12 7.79 17.15
1000 78.14 5.44 2.64 5.99 7.54 16.72
E 100 15.61 39.01 17.55 41.94 50.73 117.35
300 27.25 22.55 13.75 25.30 38.50 71.56
500 35.26 18.19 8.46 19.46 23.27 55.03
1000 50.06 12.12 7.10 13.60 19.81 38.15
T 300 23.94 38.12 13.79 39.74 39.74 112.09
500 31.00 31.75 13.07 34.24 36.73 95.35
1000 44.12 21.59 10.80 23.75 29.80 66.11
FIG. X3.1 The Relationship between Reproducibility (R) and Diagonal length (d) from Table X3.1 in µm units, for the Knoop Hardness
Tests for Specimens B, C, D, E and T
24
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FIG. X3.2 The Relationship between Reproducibility and Diagonal length (d) from Table X3.2 in µm units, for the Vickers Hardness Tests
for Specimens B, C, D, E and T
FIG. X3.3 The Relationship between Reproducibility (R) and Diagonal length (d) from Table X3.3 in HK units, for the Knoop Hardness
25
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FIG. X3.4 The Relationship between Reproducibility (R) and Diagonal length (d) from Table X3.4 in HV units, for the Vickers Hardness
X4. RECOMMENDATIONS FOR LIGHT FORCE MICROINDENTATION HARDNESS TESTING
X4.1 Introduction X4.2 Scope

X4.1.1 Microindentation hardness of materials can be de- X4.2.1 These recommendations provide guidance and sug-
termined using a variety of loads to force the indenter into the gest additional precautions for microindentation hardness test-
test piece. Testing is considered to be using a light force when ing when the measured indentation diagonals are less than 20
the force in use produces indentations with a diagonal length of µm in length.
less than 20 µm. Both Knoop and Vickers hardness numbers
increase in proportion to the inverse of the square of the X4.3 Environment
indentation diagonal length, Eq 2 and Eq 7. Thus, hardness X4.3.1 Vibration:
numbers obtained from indentations with diagonals measuring X4.3.1.1 Vibration of the microindentation hardness tester
less than 20 µm are much more sensitive to variations of a few during a light force test can cause a large percentage increase
tenths of a micrometer in the actual or measured length of the in the measured diagonals. Reasonable accuracy and precision
diagonals than hardness numbers obtained by measuring larger can only be achieved when the test instrument is isolated from
indentations. Creation of valid indentations, and the accurate vibration as much as possible during testing. Use of an
measurement of their diagonals, becomes even more impera- isolation table or isolation platform is mandatory. Airborne
tive as the indentations become smaller. For example, consider vibrations in the vicinity of the test instrument, such as air
a material with a Vickers hardness of 500. For a force of 100 currents and loud noises, are to be avoided.
gf, the diagonal length would be 19.258 µm. To maintain an X4.3.1.2 It is recommended that test instruments not be
error of 6 1 %, the accuracy of the diagonal measurement must located above the ground floor of the building due to the
be ≤ 0.096 µm. Similarly, for a material with a Knoop hardness increase in vibration usually experienced by the upper floors.
of 500, when tested with a 20 gf force, the diagonal length Test instruments should be located in areas away from machin-
would be 23.86 µm. To maintain an error of 6 1 %, the ery that may cause low (<20 Hz) frequency vibrations, since
accuracy of the diagonal measurement has to be ≤ 0.12 µm. low frequencies are more easily transmitted through isolation
Measurements to this level of accuracy are impossible to tables and platforms.
achieve by light optical microscopy. Because of the inherent
difficulties involved in obtaining and measuring indentations X4.3.2 Level—Microindentation hardness testers must be
with diagonals less than 20 µm, and the increasing effect of level in order to obtain usable information. Errors due to minor
possible indentation or measurement errors, light force micro- un-leveling become more important as the forces become
indentation hardness testing requires precautions in addition to lighter.
those normally necessary. Small indentations may be due to X4.3.3 Temperature—Control of the temperature of the
high test piece hardness or the use of light forces, or both. In specimen, testing instrumentation, and surrounding area should
either case, some of the concerns involved with obtaining be considered. It is recommended that these temperatures be
accurate hardness results are addressed in this appendix. maintained at 23 6 3°C. As the length of the measured
26
E384 − 17
diagonal becomes smaller, it may be necessary to increase X4.5.3 Diagonal Measuring Device—The measurement
control of temperature to reduce variability. technique and the devices used to perform the measurements
should be capable of discerning differences in length of 0.1 µm
X4.4 Specimens or less. In some cases, it may be preferable to obtain a
photomicrograph of the indentation first, and measure the
X4.4.1 Specimen Preparation:
length of the diagonal as seen in the photomicrograph. In all
X4.4.1.1 Usually, test pieces require mounting. Care must
cases, calibration of magnifications and measuring devices is
be taken to ensure that the specimens are well supported in the
necessary.
mounting material, and that the surface to be tested can be
placed into the test instrument such that it will be normal to X4.5.4 Accuracy of Forces—Often, small indentation diago-
both the loading and optical axes. nal lengths are the result of the use of very light forces, in many
X4.4.1.2 The surface properties of the test specimen must cases 10 gf or less. Force accuracy of 6 1.5 % is required. For
not be altered due to specimen preparation. Metallographic light forces, this requires that no oils, dust, or other minor
specimen preparation should be performed using accepted contaminants be present. For example, when using a force of
techniques known to eliminate all preparation-induced defor- 2.0 g, contaminants with a total mass of more than 0.02 g
mation on the test surface of the specimen. Light etching render the results of the test invalid.
followed by light re-polishing may be used to further decrease X4.5.5 Loading Rates—When using light forces, the impact
the thickness of any deformed layer. Electropolishing may of the indenter on the surface of the test piece can cause
provide surfaces essentially free of deformation due to prepa- significant inaccuracies to occur. Use of the slowest loading
ration when properly performed. Areas to be tested must rate available for each instrument is recommended.
appear flat in the field of focus of the microscope used to
X4.5.6 Indenters—Greater repeatability, accuracy, and pre-
measure the diagonals of the indentations.
cision may be obtained by the careful selection of indenters.
X4.4.1.3 The surfaces to be tested should be as clean as
Verification of the included angles of the faces, the degree of
possible. Care must be taken to avoid surface contaminants that
mismatch at the vertex, and the sharpness of the edges are
may be absorbed into the surfaces of some materials such as
appropriate criteria for the selection of indenters. Using the
polymers or ceramics.
manufacturer’s certification, the exact indenter constant should
X4.4.2 Microstructure of Specimen—If the microstructure be calculated and used to minimize errors.
of the test piece is on the same size scale as the indentation
diagonal length, an increase in the variability of the hardness X4.6 Measurement of Indentations
data should be expected. Indentations placed within a single X4.6.1 Indentations that do not appear symmetrical should
grain will experience resistance to deformation somewhat not be considered valid for diagonal measurement. A difference
dependent on the orientation of that grain to the test surface. in symmetry greater than 10 % should be addressed with
Since these orientations are normally random, variability of concern. If consistently asymmetrical indentations are
results is increased. Indentation diagonal lengths can vary obtained, the alignment of the specimen to the indenter should
depending upon the number of grain boundaries traversed by be adjusted. If the problem persists, the microindentation
the indentation. Multiphase material systems will provide hardness instrument should be serviced by a qualified techni-
indentation diagonal lengths that may be proportional to the cian.
volume percentage of each phase included within the volume
of deformation caused by the indentation. In the above cases, X4.7 Scanning Electron Microscope
an increase in the number of measurements taken will be
necessary to provide meaningful results. X4.7.1 Measurement of indentation diagonals using a scan-
ning electron microscope is possible. However, careful cali-
bration of the SEM photographic image at the exact magnifi-
X4.5 Instruments
cation to be used is essential. For these measurements, the
X4.5.1 Magnification of Microscope—Classic microinden- specimen must be perpendicular to the beam, that is, the tilt
tation hardness testers make use of optics that usually provide angle should be 0°. The accelerating voltage and other param-
magnifications from 400 to 600×. Higher magnifications are eters should remain as they were for calibration. (The SEM
required when performing light force testing. Specimens may should be calibrated in both the X and the Y directions; refer to
be removed from the test instrument following the indentation Practice E766. Indentations to be measured should not extend
operation, and the diagonals of the indentations measured to the periphery of the SEM field of view, as the video signal
using a separate high quality light (or SEM measurements, see can be distorted at the edges of the video monitor.
X4.7.1) microscope capable of providing higher magnifica-
tions. X4.8 Video and Automatic Measuring Systems
X4.5.2 Optical Quality of Microscope—Use of highly cor- X4.8.1 Typical video or computerized measuring systems
rected objectives with numerical apertures of 0.9 or greater is lack the necessary resolution for obtaining acceptable results
recommended. Use of dark field illumination or differential when indentation diagonal lengths are less than 20 µm. Loss of
interference contrast may improve the contrast of the image resolution within the digitized image can cause a substantial
and also enhance the user’s ability to detect the ends of the decrease in the accuracy of the measurement. Extremely high
indentations. resolution video cameras and monitors, when appropriately
27
E384 − 17
assembled into a measuring system, may be capable of
resolution sufficient to provide accurate results.
X5. A PRIMER ON CHOOSING THE INDENTER AND TEST FORCE
X5.1 Introduction Knoop indents while Fig. X5.2 shows this relationship for
X5.1.1 Users of E384 often ponder over which indenter they Vickers indents. As the test load decreases, and the hardness
should use for a given problem and also which test force is best rises, the slope of the curves for diagonal versus hardness
for a given evaluation task. Although it has been claimed that becomes nearly vertical. Hence, in this region, small variations
etching of a specimen can lead to bad hardness data, is that in diagonal measurements will result in large calculated hard-
only true for a deeply etched specimen, or for all etched ness variations.
specimens? The constancy of Vickers hardness over a wide test
X5.2.2 If we assume that the repeatability of the diagonal
load range has been claimed to be poor for forces ≤100 gf.
measurement by the average user is about 6 0.5 µm, and we
Knoop hardness does vary with test load, but by how much?
add and subtract this value from the long diagonal length or the
Can anything be done to determine HK500 equivalent data at
lower applied forces? This appendix offers examples for users mean diagonal length, we will calculate two hardness values.
to study and pick up advice to help them find solutions as The difference between these values is ∆HK and ∆HV, shown
effectively as possible. in Fig. X5.3 and Fig. X5.4. From these two figures, we can see
how the steepness of the slopes shown in Fig. X5.1 and Fig.
X5.2 Influence of the Equations Defining HV and HK on X5.2 will affect the possible range of obtainable hardness
Precision values as a function of the diagonal length and test force for a
X5.2.1 The basic definitions of HK and HV, where the relatively small measurement imprecision, 6 0.5 µm. These
applied force is multiplied by a geometric constant (Eq 2 and figures show that the problem is greater for the Vickers
Eq 7, respectively) and then divided by the long diagonal indenter than for the Knoop indenter for the same diagonal
squared or the mean diagonal squared, respectively, cause an length and test force. For the same specimen and the same test
inherent problem in measuring small indents, that is diagonals force, the long diagonal of the Knoop indent is 2.7 times
≤20 µm in length. Fig. X5.1 shows the calculated relationship greater than the mean of the Vickers’ diagonals, as shown in
between the diagonal and load and the resulting hardness for Fig. X5.5.
FIG. X5.1 Relationship between the long diagonal length and the Knoop hardness as a function of the test force. Note how the slope
of the lines becomes more vertical as the test force decreases.
28
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FIG. X5.2 Relationship between the mean diagonal length and the Vickers hardness as a function of the test force. Note how the slope
of the lines becomes more vertical as the test force decreases.
FIG. X5.3 Plot showing the possible range of Knoop hardness due to a 6 0.5 µm measurement imprecision as a function of the diago-
nal length and the applied test force. The results are plotted for materials with a maximum HK of 1100-1200. Note that the problem for
specimens with diagonals #20 µm is greatest for 10 and 25 gf test loads
29
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FIG. X5.4 Plot showing the possible range of Vickers hardness due to a 6 0.5 µm measurement imprecision as a function of the diago-
nal length and the applied test force. The results are plotted for materials with a maximum HV of 1100-1200. Note that the problem for
specimens with diagonals #20 µm is greatest for 10 to 100 gf test loads.
FIG. X5.5 Relationship between the Knoop long diagonal and the mean Vickers diagonal for equivalent hardness (per E 140) at a 500
gf test load. The Knoop diagonal is 2.7 times longer than the Vickers diagonal.
X5.3 Consistency in HV for Specimens as a Function of materials than for soft materials. On the other hand, the Vickers
Test Force and the “Load-Hardness” Problem indenter does produce geometrically identically-shaped indent
X5.3.1 Numerous studies of Knoop and Vickers tests made cavities as a function of depth, so the Vickers hardness should
on metals over a range of hardness and test forces have shown be constant with test force. However, many studies conducted
an inconsistency in the hardness values, the so-called “load- using test forces ≤1000 gf have shown deviations from
hardness” problem. For the Knoop indenter, because the indent constancy at test loads ≤100 gf. In almost all cases, this
cavity is not geometrically identical as a function of indent problem has been attributed to interactions between disloca-
depth, the hardness should vary somewhat with test force. tions and the indenter at these low loads. A review of more than
Because of the difficulty in measuring small indents, and the 60 publications (9) about such studies has revealed four
influence of small variations in measurement, this inconsis- different published load-HV trends. They are (from most
tency would be expected to be greater for high hardness common to least common): (1) at test loads ≤100 gf, the HV
30
E384 − 17
decreases; (2) at test forces ≤100-200 gf, the HV rises slightly <12.5 µm in length; and, all indents made with a 50 gf load
and then decreases; (3) at test loads ≤100 gf, the HV increases; were <17.5 µm in length. Despite these very small sizes due to
and, 4) at test forces from 1000 gf to either 10 or 25 gf, the HV the light loads, measurements using a 100X objective (0.95
was constant. Trend number 1 was by far the most commonly NA) gave reasonably good data. The overall results are much
observed trend. An example of such a study (9) is shown in Fig. better than the results in Fig. X5.6 and Fig. X5.7, as well those
X5.6. In this experiment, five indents made at each test force, reported in (7, 8), the first interlaboratory study (Research
from 5 to 500 gf, were measured at 500X magnification using Report RR:E04-1004).8
five HRC test blocks covering a wide hardness range. Note that
trends 1 and 2 are observed in this data. In the interlaboratory X5.4 Variability in HK as a Function of Applied Force
study (see Appendix X1 and (7, 8), all four trends were X5.4.1 Unlike the Vickers square-based indenter, the
observed for the same indents measured by different laborato- rhombohedral-shaped Knoop indenter does not produce geo-
ries. The literature claimed that macro-Vickers testers were metrically identical indent cavities as a function of depth and
immune from this problem, however, no published examples of the hardness should vary with the applied force. In general, this
work like that shown in Fig. X5.6 could be found in the variation is small over the range from 200 to 1000 gf. As the
literature for macro-Vickers testers using test loads from 1 to force decreases below 200 gf, the increase in HK becomes
120 kgf, or from 1 to 50 kgf. Consequently, the same HRC test greater. Unlike the Vickers indents, the Knoop indents are more
blocks were evaluated as a function of applied test force from likely to be undersized than oversized when they are smaller in
1 to 50 kgf revealing results (9), shown in Fig. X5.7, that size. This error also increases the HK value and adds to the
exhibit trends 1 and 2. These indents were measured using usual upward trend observed as the test force decreases. The
100X magnification, typically used with macro-Vickers sys- literature contains many examples of this trend. However, in
tems. These results clearly suggest that the inconsistency in the first interlaboratory test (7, 8) (see Appendix X1 and
HV at low test loads is a visual perception problem due to Research Report RR: RR:E04-1004) a few laboratories actu-
inadequate resolution and perhaps inadequate image contrast. ally showed the opposite trend, decreasing HK with decreasing
X5.3.2 If higher magnification optics with high numerical test force below 200 gf, never published previously. The four
aperture ratings are utilized, can the “load-hardness” problem test blocks evaluated for Vickers hardness, Fig. X5.8, were also
be overcome? To test this, Vickers indents (six at each test evaluated for Knoop hardness, using six indents at each test
load) were made over a range of test forces varying from 10 gf force and a range from 10 to 1000 gf. The results are shown in
to 10 kgf and the indents were measured with objectives Fig. X5.9. All of the indents made with a 10 gf load were <20
varying from 10X to 100X using four HRC test blocks with a µm in length; all of the indents made with a 25 gf load were
range of hardness (10). Fig. X5.8 shows that the results were
much better than those shown in Fig. X5.6 (5 to 500 gf) and 8
Fig. X5.7 (1 to 50 kgf). All indents made with a 10 gf load were be obtained by requesting Research Report RR:E04-1004. Contact ASTM Customer
<8 µm in length; all of the indents made with a 25 gf load were Service at [email protected].
FIG. X5.6 Vickers hardness as a function of test load from 5 to 500 gf for five HRC test blocks revealing trends 1 and 2. Measurements
were made at 500X.
31
E384 − 17
FIG. X5.7 Vickers hardness as a function of test load from 1 to 50 kgf for five HRC test blocks revealing trends 1 and 2. Measurements
were made at 100X.
FIG. X5.8 Vickers indents made on four HRC test blocks at test forces from 10 gf to 10 kgf and measured using 10X to 100X objectives.
The indents made with test forces of 10, 25, 50 and 100 gf averaged ~4.7 to 7.7 µm, ~7.5 to 12.2 µm, ~10.8 to 17.2 µ and ~15.0 to
24.3µm for the four blocks – all but the 100 gf tests for the 44.7 and the 32.5 HRC test blocks were in the range #20 µm where mea-
surements are very difficult.
<31 µm in length; all of the indents made with a 50 gf load mining HK values, versus HV values, at low loads. However,
were <45 µm in length; and, all of the indents made with a 100 the variation in HK with test force is a constraint to using the
gf load were <65 µm in length. For the same specimen and test Knoop test at varying test loads and then trying to compare that
load, the Knoop long diagonal is ~2.7 times longer than the data to results from other hardness scales. Being able to correct
Vickers mean diagonal which improves the precision in deter- for this deviation would be advantageous.
32
E384 − 17
FIG. X5.9 Knoop hardness indents were made on four HRC test blocks at test forces from 10 to 1000 gf and were measured using 10X
to 100X objectives. The indents made with test forces of 10, 25, 50 and 100 gf averaged ~13.2 to 19.9µm, ~20 to 30.7 µm, ~28.7 to 44.5
µm and ~41.4 to 64.4µm for the four blocks – only the 10 gf values had long diagonal lengths <20 µm.
X5.5 Examples of the Use of HK and HV at Various metallographically and by microindentation hardness testing. A
Loads to Evaluate Specimens few examples will be presented as an aid to the user.
X5.5.1 The metallographer is often required to use micro- X5.5.2 Induction hardening is widely performed but control
indentation testing as an aid to solving various characterization of the process can be challenging because the heat is applied
tasks both for research purposes and in production work for for only a few seconds and there will be a substantial
process control and specification conformance. There are many temperature gradient from the surface inward. Fig. X5.10
such processes that are evaluated both metallographically and shows evaluation of the induction hardened case of 1053
by microindentation hardness testing; for example, case hard- carbon steel using Knoop and Vickers indents. The Knoop
ening by flame or induction heating, surface compositional hardness for indents made at 50 gf applied force are consis-
modifications followed by heat treatment, as in carburizing or tently greater than the 200 gf Knoop values, a classic problem
carbonitriding, or preceded by heat treatment, as in nitriding. with the Knoop test. The Vickers data at 100 and 200 gf is in
Banding and other forms of segregation are evaluated both better agreement, but there are numerous locations where the
FIG. X5.10 Knoop testing at 50 and 200 gf (left) is compared to Vickers testing at 100 and 200 gf (right) revealing relatively similar
hardness trends and illustration of the change from the hardened case to the unhardened core at the same location. Note the charac-
teristic increase in hardness from the surface to the end of the case. The Knoop indents reveal more of the minor hardness variability
but the 50 gf data are higher for the case than the 200 gf data, which is to be expected for the Knoop test. If the depth to an equivalent
HRC value must be determined, the increase in HK as the load decreases below 500 gf must be corrected in some way. The Vickers
data at 100 and 200 gf are in good agreement, although some of the 100 gf data points are higher.
33
E384 − 17
100 gf HVs are significantly higher than the 200 gf HVs. For applied loads from 100 to 500 gf. For the HV data, the
both tests, it is clear that the surface hardness is lower than at maximum case hardness was obtained with the first indent at
the end of the case due to the temperature gradient and its affect 0.0127 mm for the 100 gf data, while the higher applied forces
on grain size and retained austenite content. The transition revealed decreased hardness at the extreme surface with the
from the case to core is defined well by both tests. The core maximum case hardness at: 0.050, 0.051 and 0.050 mm for
hardness defined by both tests at all test loads are in good applied loads of 200, 300 and 500 gf. The average case
agreement, mainly due to the larger size of the lower hardness hardness, Fig. X5.13, except for the 100 gf data, was higher for
core indents. the HV data than for the HK data. The conversion tables in
X5.5.3 Carburized specimens are commonly evaluated E140 list that the HV equivalent hardness is higher than the
metallographically and by microindentation hardness tests. equivalent HK equivalents for 67 and 68 HRC, while for 66
Fig. X5.11 shows evaluation of the carburized case after a HRC and below, the equivalent HK value is greater than the
subsequent hardening treatment for an 1141 carbon steel using equivalent HV value. The tests shown in Fig. X5.12 agree with
Knoop tests at 100, 200, 300 and 500 gf and Vickers tests at that unexpected trend. Fig. X5.13 shows the average case
200, 300 and 500 gf. For the Vickers tests, a test force of 100 hardness and the hardness at the end of the case (the end of the
gf gave indent diagonals <20 µm. Consequently 100 gf HV was dark-etching surface layer at 0.14 mm)
not used. The Knoop data at the four test loads does show a X5.5.5 Segregation of various types is often evaluated by
continuous increasing hardness trend with decreasing test metallographic methods and by microindentation hardness
force, as expected, while the Vickers data at the three test loads testing (see, for example, Practice E1268). While Practice
also shows some variation in HV, but less than the HK data. E1268 utilizes microindentations, it is limited to determining
Both sets of data show a drop in hardness near the extreme the mean HK of the alternating bands (long axis parallel to the
surface, but this is defined better with the Knoop data, except bands). This procedure can be expanded as shown in the
for the 200 gf data. As these tests were performed at different following example for an offshore plate steel (Fe – 0.13% C –
locations along the surface, the 200 gf result at the surface 1.40% Mn – 0.33% Si – 0.026% Nb) with bands of ferrite
could be due to a composition/microstructural difference at that alternating with bands of variable martensite, bainite and
location. The Knoop surface hardness data for the 300 and 500 pearlite content. Several parallel bands of HV and HK indents
gf indents are identical. were made over the same segregation bands at each test load
X5.5.4 Nitrided parts are also frequently evaluated both from 25, 50, 100, 200, 300 and 500 gf (only HV at 500 gf –
metallographically and with microindentation hardness tests to results not plotted here; HK indents at 500 gf were too long to
define the effective case depth. There are a number of nitriding measure) as shown in Fig. X5.14.
processes and some, like ion-nitriding and ferritic nitro- X5.5.5.1 The test results can also be examined by plotting
carburizing, do exhibit very thin cases where the Knoop indent the mean and standard deviations of the measurements with
is required. Those with thicker cases, such as the nitrided H13 each indenter at each test force, as shown in Fig. X5.15, and by
mold (no compound layer) shown in Fig. X5.12, can be plotting the maximum and the minimum HK and HV value at
evaluated using either the Knoop or the Vickers indenter. As each test force, as shown in Fig. X5.16. Note how the
expected, the HK values using test forces from 100 to 500 gf minimum values do not change much, regardless of the test
show a wider spread in HK at all locations compared to the HV load or indenter type. These identical trends have been ob-
data. For the HK data, the maximum case hardness was served in all such banded specimens evaluated by this tech-
obtained at a depth of 0.021, 0.030, 0.045 and 0.050 mm for nique.
FIG. X5.11 Evaluation of the carburized surface of 1141 carbon steel after heat treatment using four test forces for the Knoop indents
(left) and three for the Vickers indents (right). Note that three of the test forces using the Knoop indenter revealed a decrease in hard-
ness at the extreme surface but this was not detected as well using the three test forces and the Vickers indenter. Retained austenite
was present in the case to a depth of ~0.32 mm while grain boundary ferrite began to be observed at a depth of ~1.25 mm.
34
E384 − 17
FIG. X5.12 Evaluation of a nitrided H13 die using 100, 200, 300 and 500 gf test forces with both the Knoop and Vickers indenters. Note
that, as before, the range of HK at each location using these four test loads is broader than the HV range. The HV range is tight, ex-
cept at the near surface area. All four HK traces show a drop in hardness at the surface while the 200-500 gf HV indents show a
similar, but lesser, trend. The dark-etching case ended at ~0.14 mm.
FIG. X5.13 Plots of the average case hardness (left) and the hardness at the end of the dark-etching case at ~0.14 mm (right) for the
nitrided H13 mold. For HV values of 900 and greater, the conversion chart (Table 1 of E140) shows lower HK numbers; while the re-
verse is shown for HV values <900.
X5.6 Correlating Knoop Data made at <500 gf to the X5.7 Influence of Etching upon Microindentation Hard-
Equivalent HK500 Value ness Results
X5.6.1 The above tests results point out some excellent X5.7.1 In general, if the structure is deeply etched, the
characteristics of the Knoop test, but also one very significant metallographer will be unable to see the indent tips. For
problem – the increase in HK with decreasing test force. It is example, when the nitrided H13 specimen in X5.6 above was
possible to develop correction factors, although these factors etched with nital, the nitrided case was a dark black and the
have some inherent imprecision and will probably vary from indents tips could not be detected optically. In general, if the
operator to operator. An individual’s own variation in HK etching results are not excessively dark, there was no signifi-
between 500 gf and lower test forces can be easily checked and cant difference observed for the microindentation values in the
compared to the data shown below by performing a number of etched vs. un-etched condition. Two examples are shown in
indents, for example, 5, at various test loads from 500 gf and Fig. X5.19. The first is a thick carburized case on 8620 alloy
below on a certified test block, such as an HRC test block. An steel which was subsequently heat treated with an isothermal
example of such tests made on a number of steel tensile bars hold to form lower bainite in the case while the core was
covering a wide range of HK is given in Fig. X5.17. Fig. X5.18 tempered low-carbon martensite. The first observance of mar-
shows the approximate shift in HK as the applied force tensite was at a depth of ~0.5 mm and the structure was fully
decreases and as the HK500 value increases. Table X5.1 lists martensitic after a depth of ~0.69 mm. Overall, the difference
these approximate correction values as a function of the in hardness between the as-polished specimen and the etched
applied load and the HK500 value. specimen was not significant, except for the slightly higher HK
35
E384 − 17
FIG. X5.14 Evaluation of banding heterogeneity of an offshore plate steel using test forces from 25 to 300 gf reveals that the Knoop
indenter, due to its long narrow shape better reveals the variability in hardness, best seen at the lowest test load. Some of the bands
contained varying amounts of martensite, bainite and pearlite and these patches are small; hence, the Knoop 25 gf indenter was better
able to detect the extreme hardness variations. At each test force, the Knoop indenter gave more detail of the hardness variations than
the Vickers indenter.
36
E384 − 17
FIG. X5.14 (continued)
FIG. X5.15 Examination of the test data shown in Fig. X5.14 (plus the 500 gf HV data not shown) reveals that the mean Knoop hard-
ness was greater than the mean Vickers hardness at all loads (left), with this difference increasing with decreasing applied load, as
would be expected. But, the rise in mean HV at 25 and 50 gf reflects the better ability of the smaller Vickers and Knoop indents to
sense the hardness variations within the bands. In line with this, the standard deviations for the 25 and 50 gf Vickers indents are nota-
bly greater than the nearly constant standard deviation from 100 to 500 gf (right). The much higher standard deviations for the Knoop
indents made #200 gf are in agreement with the data plots in Fig. X5.14.
in the core from a depth of ~1.5 to 2.25 mm. The second than in the as-polished condition. In both cases, the second run
example shows the measurement of decarburization depth in was performed near the first run. If there is concern, and the
quenched and tempered 41S50 alloy steel. Overall, the differ- structure must be etched to locate the indents, etch as lightly as
ences are insignificant, although the two tests at depths of possible
~0.05 and 0.09 mm are slightly lower in the etched condition
37
E384 − 17
FIG. X5.16 Further evaluation of the data for the banded offshore plate steel microindentation hardness data reveals that the minimum
HK is slightly greater than the minimum HV data at each test force (in agreement with the correlation between HV and HK in E140), and
that the minimum HK and HV varied very little over the test load range. The maximum hardness at each test force, however, increased
at forces <300 gf, with substantially greater HK values at each test force. This is mainly due to the greater ability of the elongated
Knoop indenter to sense hardness increases within the narrow bands containing martensite, bainite and pearlite.
FIG. X5.17 Linear regression analysis was performed on HK data made at test forces of 25, 50, 100, 200, 300 and 500 gf.
38
E384 − 17
FIG. X5.18 Graph based upon the data shown in X5.17 showing the increase in HK compared to the HK500 value for test forces 25, 50,
100, 200 and 300 gf. These values would be subtracted from the HK value at test loads from 25 to 300 gf to approximate the HK500
value.
TABLE X5.1 Approximate Correction Values for Reducing Knoop Values at Test Forces from 25 to 300 gf to an Equivalent HK500 Value
HK500 25 gf 50 gf 100 gf 200 gf 300 gf
150 1.88 1.96 0 0 0
200 15.4 12.4 6.5 0 0
250 28.9 22.8 13.7 4.1 0.7
300 42.44 33.2 20.8 8.3 2.4
350 55.96 43.6 27.9 12.4 4.1
400 69.48 54 35 16.5 5.8
450 83 64.5 42.1 20.7 7.5
500 96.5 74.9 49.3 24.8 9.3
550 110 85.3 56.4 28.9 11
600 123.6 95.7 63.5 33.1 12.7
650 137.1 106.1 70.6 37.2 14.4
700 150.6 116.5 77.7 41.3 16.1
FIG. X5.19 Two examples of extensive microindentation hardness test runs on adjacent locations before and after etching.
39
E384 − 17
REFERENCES
(1) Knoop, F., et al.,“A Sensitive Pyramidal-Diamond Tool for Indenta- (7) Vander Voort, G.P.,“Results of an ASTM E04 Round Robin on the
tion Measurements,” Journal of Research National Bureau of Precision and Bias of Measurements of Microindentation Hardness,”
Standards, Vol. 23, July 1939, pp. 39-61. Factors that Affect the Precision of Mechanical Tests, ASTM STP
(2) Campbell, R.F., et al., “A New Design of Microhardness Tester and 1025, ASTM, Philadelphia, 1989, pp. 3-39.
Some Factors Affecting the Diamond Pyramid Hardness Number at (8) Vander Voort, G.F.,“Operator Errors In the Measurement of Microin-
Light Loads,” Trans. ASM, Vol 40, 1948 , pp. 954-982. dentation Hardness,” Accreditation Practices for Inspections, Tests,
(3) Kennedy, R.G., and Marrotte, N.W., “The Effect of Vibration on and Laboratories, ASTM STP 1057, ASTM, Philadelphia, 1989, pp.
Microhardness Testing,” Materials Research and Standards, Vol 9, 47-77.
November 1969, pp. 18-23. (9) Vander Voort, G. F., Metallography: Principles and Practice,
(4) Brown, A.R.G., and Ineson, E., “Experimental Survey of Low-Load
McGraw-Hill Book Co., NY, 1984; ASM International, Materials
Hardness Testing Instruments,” Journal of the Iron and Steel Inst., Vol
Park, OH, 1999, pp. 356, 357, 380 and 381.
169, 1951, pp. 376-388.
(10) Vander Voort, G. F. and Fowler, R., “Low-Load Vickers Microin-
(5) Thibault, N.W., and Nyquist, H.L., “The Measured Knoop Hardness
of Hard Substances and Factors Affecting Its Determination,” Trans. dentation Hardness Testing”, Advanced Materials & Processes, Vol.
ASM, Vol 38, 1947, pp. 271-330. 170, April 2012, pp, 28-33.
(6) Tarasov, L.P., and Thibault, N.W., “Determination of Knoop Hardness
Numbers Independent of Load,” Trans. ASM, Vol 38, 1947, pp.
331-353.
SUMMARY OF CHANGES
Committee E04 has identified the location of selected changes to this standard since the last issue (E384 – 16)
that may impact the use of this standard. (Approved June 1, 2017.)
(1) Appendix X5 was added.
Committee E04 has identified the location of selected changes to this standard since the last issue
(E384 – 11ε1) that may impact the use of this standard. (Approved February 1, 2016.)
(1) This test method was heavily revised. Changes were made
throughout the text.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
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40

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

Standard Test Method for

1. Scope* 2. Referenced Documents

*A Summary of Changes section appears at the end of this standard

FIG. 1 Knoop Indenter

FIG. 2 Vickers Indenter

P2 = force, N, and where:

FIG. 3 Minimum Recommended Spacing for Knoop and Vickers Indentations

A1.1 Scope ing the consistency of microindentation measurements based

HK > 0 HV > 0 1 # F <100 13 3

100 # HK # 250 100 # HV # 240 100 # F < 500 13 2

100 # HK # 250 100 # HV # 240 500 # F # 1000 8 2

A2. CALIBRATION OF STANDARDIZED HARDNESS TEST BLOCKS FOR MICROINDENTATION HARDNESS

A2.1 Scope A2.2 Certification of Standardized Test Block

X1. RESULTS OF INTERLABORATORY TEST OF THE MEASUREMENT OF MICROINDENTATIONS

TABLE X1.2 Relationship Between the Diagonal Length and (Ir)j,

TABLE X1.4 Relationship Between the Diagonal Length and (IR)j,

X2. RESULTS OF AN INTERLABORATORY TEST COMPARING MICROINDENTATION HARDNESS TESTING USING

X2.1 Introduction X2.4 Repeatability

X3. RESULTS OF INTERLABORATORY TEST OF THE MEASUREMENT OF MICROINDENTATIONS

X3.1 Introduction X3.2.2 The precision statement was determined through

X4. RECOMMENDATIONS FOR LIGHT FORCE MICROINDENTATION HARDNESS TESTING

X4.1 Introduction X4.2 Scope

X5. A PRIMER ON CHOOSING THE INDENTER AND TEST FORCE

FIG. X5.14 (continued)

(1) Appendix X5 was added.

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