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Selected aspects of evolution properties of oxygen free copper for high-

advanced electrotechnical application

Article  in  Przeglad Elektrotechniczny · January 2011

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 Tadeusz KNYCH1, Beata SMYRAK2, Monika WALKOWICZ3
AGH University of Science and Technology, Faculty of Non-Ferrous Metals (1) (2) (3)

Selected aspects of evolution properties of

oxygen free copper for high-advanced electrotechnical application
Abstract. The shaping of properties of metallic materials in the process of continuous casting takes place through changes in the parameters of the
technological process, i.e., the temperature of liquid metal, casting rate, flow size and crystallizer cooling water temperature. In this work,
characterization of the influence of parameters of the casting process has been carried out, especially that of the casting rate on formation of
material structure in terms of the quantity, size and shape of grains. The properties of copper wires for highly advanced electro-technical applications
(audio-video cables, fireproof cables, car bundles) have also been characterized.

Streszczenie. Kształtowanie własności materiałów metalicznych w procesie ciągłego odlewania odbywa się na drodze zmiany parametrów procesu
technologicznego tj. temperatury ciekłego metalu, prędkości odlewania, wielkości przepływu i temperatury wody chłodzącej krystalizator. W pracy
dokonano charakterystyki wpływu parametrów procesu odlewania, a w szczególności prędkości odlewania na kształtowanie się struktury materiału
pod kątem ilości, wielkości oraz kształtu ziaren, a także własności drutów miedzianych przeznaczonych do wysokozaawansowanych aplikacji
elektrotechnicznych (kable audio-video, kable ognioodporne, wiązki samochodowe). (Wybrane zagadnienia oceny własności miedzi beztlenowej
pod kątem jej zastosowania w wysokozaawansowanych konstrukcjach elektrotechnicznych).

Keywords: oxygen free copper, continuous melting and casting line, wires, audio-video cables.
Słowa kluczowe: miedź beztlenowa, proces ciągłego topienia i odlewania, druty, kable audio-video.

Analysis of the problem characterized by excellent deformability, as well as

The rapid development of electronics and broadly resistance to atmospheric corrosion and hydrogen
understood electro-technology imposes a need for the embrittlement [3÷6]. In electronic applications, a variant of
search for new materials allowing for rapid lossless oxygen free copper is used with specially shaped grains
transmission of electric signals. The universality of use of and, first and foremost, the smallest possible amount of
electronic systems and electro-technical elements has grains per unit of length. Examples of such solutions are
caused the emergence of a new group of products with Long Grain Crystal Copper (LGC) and Long Crystal Copper
highly advanced properties, such as cables, conductors, (LCC). In the above mentioned grades of copper, the
microwires and connecting elements used in the electro- amount of grains is reduced to a level of 200 per meter of
technical industry. Depending on the application, the ideal length, thanks to which the transmission of an electric signal
transmission cable should guarantee high sound and image in audio-video applications is not as lossy, and the
quality (audio-video cables), optimal data transmission elimination of drawbacks of connections has become
speed (cables for information technology applications), possible. LGC and LCC surpass OFE copper, in which the
appropriate signal strength and minimization of attenuation amount of grains is equal to about 500/mb [7, 8].
and the risk of occurrence of interference. The above Properties similar to those of LGC and LCC copper are
requirements create the need for use of a material allowing possessed by OCC copper obtained according to Ohno
for an electron flow that is as lossless as possible. Continuous Casting Technology, the main purpose of which
Modern material solutions in this field of applications are is the decrease of the amount of crystals in the conductor.
mainly concentrated on copper. Although this functional In highly specialized applications, such as electron
material has been known to mankind for 10,000 years (and technology (elements of particle accelerators, cryogenics),
as an excellent conductor of electricity, since the XVIII 6N grade copper with a purity of 99.99997 % is used. The
century), the search for new possibilities of its utilization has highest grade of purity for copper obtained industrially is
not ceased. This is visible in the large amount of work and currently 8N grade purity (99.999999 %). High quality
achievements in this field. The modern study of copper has cables are often made from copper with a purity grade of 6-
two main directions of development: the first, still valid since 7N. The traditionally used ETP copper, in which oxygen
the discovery of electricity, is the pursuit of a constant content is at a level within 200÷600 ppm. wt., does not
increase in electric conductivity, as well as deformability, for guarantee such properties [9, 10]. The assortment of
wires and microwires. The second direction is a new trend oxygen free copper products is very broad and is
that has become visible over the last few years, i.e., studies concentrated mainly on highly advanced products.
on high strength copper alloys for electric purposes, with a According to the data included in Table 1., oxygen free
strength reaching up to 1,200 MPa and electric conductivity copper of the highest quality (according to JISH 2123 grade
at a level of 80 % IACS. This second group of work includes C1011) is mainly used in electron technology (accelerator
numerous worldwide studies carried out at institutions of elements and electron tubes), vacuum apparatus,
higher learning and laboratories, especially in Japan and cryogenics (elements operating at low temperatures),
the United States. superconduction, cable technology (connecting elements,
The subject matter undertaken in this article regards the microwires, enamelled conductors, transmission
first of the above mentioned matters, that is, work on conductors, conductors for applications in information
functionally perfect copper for the most sophisticated technology, audio-video conductors).
applications in the electronic and electro-technical industry. Interest in the dynamically developing oxygen free
A standard for conductors of this type is Oxygen Free copper electro-technical industry, its production technology,
Electronic Copper (OFE) or Oxygen Free High Conductivity as well as its physical and mechanical properties, is a result
Copper with high chemical purity (OFHC). OFE copper with of the wide applications of this material. One application of
a purity grade of 4N (99.99 % Cu) contains about 1÷3 ppm. oxygen free copper is the production of wires and
wt. of oxygen and total impurities in an amount of no more microwires with diameters of less than 0.1 mm. Such
than 25 ppm wt. [1, 2]. Copper of this type is additionally capacity for use of oxygen free copper in the drawing

PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011 285

process is related to the limited potential of the traditionally company, which is based on constant melting of the high
used ETP grade copper for electric applications, purity cathode, oxygen reduction and constant casting of
characterized by its content of hard copper oxides (Cu2O) OFE oxygen free copper in the form of a rod wound in
with sizes of 5÷10 µm, which, for very small wire diameters, circles.
significantly decrease their ductility. The feedstock are high purity Cu-CATH-1 grade (LME
Grade A) copper cathodes that are subjected to constant
Table 1. Classification of oxygen free copper according to melting in an induction furnace. According to the ASTMB
international standards 170 standard, Cu-CATH-1 grade copper cathodes should
Country Japan USA Germany not have a total impurity content of more than 25 ppm. Next,
the liquid copper is subjected to the deoxidation process.
Standard JISH 2123 ASTM B170 DINI 787 The role of the deoxidizer is fulfilled by charcoal with a
Grade1 Grade 1 OF-Cu decreased Fe and S content, a layer of which covers the
Designation liquid copper. Metal solidification takes place in a special
C1011 C10100 2.0040
Cu vertical crystallizer immersed in liquid copper. The solidified
min. 99.99 99.99 99.95 ingot is pulled up with a given speed by means of drawing
Chemical % rollers and subsequently wound into circles by means of a
composition O2 system of winders. The above method makes it possible to
ppm. 10 max. 5 max. - produce oxygen free copper wire of high conductivity and
wt. plasticity with diameters ranging from 8-24 mm and with a
Standards applying speed of 4 m/min (for a diameter of 8 mm), which allows for
JIS H3510 ASTM F68 DIN 40500 the achievement of an average yearly output of about
to products
elements of system
15,000 tons.
electron tubes elements in conductive Oxygen free copper is also produced using other
®
microwires, electron material for methods, e.g.: Rautomead , which is based on a principle
Products ®
similar to that of the Upcast method, which is constant
audio-video technology, electric
cables, tapes, microwires, applications melting and upward casting, with which the processes of
tubes cables, melting, oxygen reduction and casting are carried out, in
contrast to the Upcast® method, in the same furnace
The dynamic evolution of electronics and broadly [11,12].
understood electro-technics taking place these last few
years is determined by the most recent technical and
technological solutions in the field of metallurgy and
processing of metallic materials, especially copper. Super-
standard requirements expected of wires for the most
sophisticated current applications are transferable to the
high technological regime of perfect control over the entire
production system, from control of the type and chemical
composition of the concentrate and quality of anodes and
cathodes through processes of casting and hot rolling, to
multi-stage drawing combined with heat treatment, up to
obtaining of the final product. The presence and improper
quantitative proportions of foreign atoms in the cathode,
being the feedstock in the wire production process, play a
negative role in shaping the properties of copper in the
processes mentioned above. It is the assortment and
quality of feedstock used for production of electronic
products that determine their construction and the
production technology used in a significant way and
therefore, also properties of use, including durability and
reliability of products. However, taking into account the fact
that the feedstock in the production process of ETP and
OFE grade copper is a high purity Cu-CATH-1 grade
Fig. 1. Apparatus for continuous casting in schematic perspective
cathode with the same chemical composition, obtaining ®
view – own design DCC-AGH [13]
oxygen free copper in a way that secures it a place in the
centre of interest of modern electronics requires the Dynamic scientific studies of a laboratory method of
utilization of highly advanced production techniques. obtaining copper with increasing chemical purity, being
Techniques making it possible to produce a material that carried out simultaneously worldwide, have led to the
not only possesses high chemical purity, but also a development and start-up of an installation for production of
beneficial structure, in terms of electro-technical feedstock of Cu-OFE grade with an oriented structure
applications, characterized by a minimal amount of defects, characterized by grain size being as small as possible [13,
including the property of grain boundaries being places ®
14]. The unique DCC-AGH casting station designed for
where conducted electrons are scattered. this purpose, and made based on international standards at
the AGH University of Science and Technology in Cracow,
Methods of constant melting and casting of oxygen free facilitates the complete study and analysis of the effect of
copper the structure as well as chemical purity of the material on
One of the most modern methods making possible the the properties of the wire, analysed from the angle of loss of
production of feedstock from oxygen free copper for direct transmission of an electric signal. Figure 1. presents a
processing through the method of drawing wires and scheme of the device shown in perspective. The process of
®
microwires is the Upcast technology of the Outokumpu constant casting of oxygen free copper realized on the

286 PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011

above mentioned station is based on introduction of the Figure 2 presents a general view of the entire
copper starting element through its passing through an installation, as well as a close-up of the crystallization
isolated crystallizer to a melting furnace until the moment of system and finished rods for special applications cast with
its contact with the liquid metal. Next, its movement is non-industrial speeds.
facilitated by means of an automatic supply system, and A very important aspect of study is the problem of
Cu-OFE grade copper is cast. In the initial stage of the shaping structure during the casting process. As mentioned
casting process, the liquid copper is subjected to a cooling before, this can be done by skilfully controlling casting
process by means of a cooling medium located in a metal speed as well as cooling conditions. During studies,
sleeve which tightly closes off the isolated crystallizer, after through changing casting speed and introducing a
which the circulation of the primary cooling system zone is controlled heat conduction zone in the crystallizer,
closed with the exit of the material from the crystallizer, and conformity of the direction of heat conduction with the
the subsequently cast copper is subjected to cooling by direction of the axis of the cast product is aimed for. Such a
means of the secondary cooling system zone. This zone is method of casting leads to visible changes in the structure
located at the crystallizer output near the surface of the cast of copper, which is shown in Figure 3.
material. After the cast product passes through the
secondary cooling system zone, it is directed towards a
drawing unit made from pressure and guide rolls, the
pressing force of which, on the surface of the finished cast
product, is regulated by screws.
A significant characteristic of the station is the use of a
high-output, isolated crystallizer with a simple and
uncomplicated construction and a secondary cooling
system using, among others, cooling gases such as liquid
nitrogen, which makes it possible to shape the structure of
copper with a limited amount of grains and to control the
direction of grain development. This results from the
characteristics of the solidification process, and more
precisely from the process of conduction of heat (offtake) by
the crystallizer and the distribution of the vector of the
temperature gradient on the front of metal crystallization,
changing from a radial direction to an axial direction (flat
crystallization front). The designed casting system makes it
possible to fulfil the dependency so that the difference of
temperatures between the liquid copper in the crystallizer
and the walls of the isolated crystallizer (∆T1) is smaller Fig. 3. Shaping of copper structure in the continuous casting
than the difference of temperature between the liquid process
copper in the crystallizer and the already solidified part of
the material (∆T2). Therefore, the following dependency is
Cel i zakres pracy. Program badań. Materiał
fulfilled: ∆T1<∆T2. The special construction of the device
The purpose of experimental studies is to determine the
makes it possible to achieve this goal through skilful control
influence of changes in metal crystallization conditions in
of casting speed as well as cooling conditions. Change in
the process of constant casting of oxygen free copper,
casting speed, as well as introduction of a controlled heat
using the Upcast method under industrial conditions as well
conduction (offtake) zone in the crystallizer, makes it
as using a laboratory method using the DCC-AGH® casting
possible to obtain consistency of the direction of heat
station, on shaping the structure of the material, which in
conduction with the direction of the axis of the cast product.
turn determines the physical and technological properties of
the wires. The specificity of constant casting allows for the
utilization of variable parameters of casting speed and flow
size of cooling water in the primary system as well as in the
secondary system. Both of these parameters play a
significant role during the course of the process of
crystallization of liquid metal. Therefore, identification of
materials for study has the purpose of making differences in
structure and the properties of materials obtained using
different parameters during the casting process (casting
speed, expenditure of cooling water) apparent, which will in
turn indicate possible differences resulting from variations in
structure during processes of plastic working and annealing.
For comparative purposes, in order to determine a point of
reference, the same course of study was carried out for Cu-
®
ETP grade copper from the Contirod line, which is
traditionally used for electric purposes. The basis for such
methodology is the fact that OFE and ETP grade copper
are feedstock for the drawing process for obtaining wires
and microwires that have completely different structures,
which is a result of different methods of production.
The objects used for this article are oxygen free copper
rods with a nominal diameter of 8 mm, obtained under
Fig. 2. Vacuum induction melting and casting furnace – own industrial conditions using the Upcast® method and under
®
design DCC-AGH [13] ®
laboratory conditions at the DCC-AGH casting station. The

PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011 287

specificity of both technologies allows for changes of should be paid to the fact that these grains change their
crystallization conditions through the regulation of two orientation from perpendicular to the rod axis, for materials
technological parameters: casting speed and the size and cast at high speeds, to parallel to the rod axis for materials
manner of flow of cooling water. For studies, ten materials cast at low speeds. It was observed that the material, for
were obtained: five Upcast rods obtained with different which the lowest casting speed was used, exhibits a two to
casting speeds under industrial conditions, i.e.: 0.5 m/min., three grain structure of arbitrary length, since this a process
1.0 m/min., 2.0 m/min., 3.0 m/min., 4.0 m/min., with a of constant casting. In the lower part of Fig. 4.9, changes in
crystallizer cooling water flow of 60 l/min, and also five rods the directions of grain orientation on the cross–section, as
from oxygen free copper cast under laboratory conditions well as the forecast change in shape of the crystallization
using the above mentioned DCC-AGH® station using the front, were marked. On the left side, the structure of the
following casting speeds: 0.006 m/min., 0.03 m/min., 0.06 ETP rod as a product after 99.99 % hot deformational
m/min., 0.15m/min., 0.2 m/min. with cooling water flow at a strengthening (elongation factor 144) is presented and is
level of 0.1÷0.4 l/min. in the primary system and 0.2÷1.0 characterized by a homogeneous, fine-grain structure that
l/min. in the secondary system. In both cases, the cooling is susceptible to the deformation process. Crystals have a
water temperature was equal to 20 °C. In comparison, the size of about 10÷20 μm and are characterized by equal
results of the study for Cu-ETP rods with an output diameter orientation in all directions. In structural terms, the rod is an
of 8 mm obtained from the Contirod line are also presented. isotropic material.
In this way, eleven types of materials obtained using
different technological processes were selected for study
® ®
(industrial conditions – installations: Upcast , Contirod ,
®
laboratory conditions – DCC-AGH installation), as well as
for different casting conditions (Upcast®, DCC-AGH®). Table
2 illustrates a comparison of the studied materials.

Table 3. Materials for research

Casting process parameters

Water flow
Material Casting l/min.
speed
m/min. Primary Secondary
cooling cooling
0.006
0.03
Cu-OFE
® 0.06 0.1 ÷ 0.4 0.2 ÷ 1.0
(DCC-AGH )
0.15
0.20
Fig. 4. Identification of structure of feedstock
0.50
1.00 Further test results apply to the mechanical properties of
Cu-OFE feedstock for the process of drawing wires and microwires.
® 2.00 60
(Upcast ) The prepared samples, with a base length of 100 mm, were
3.00
subjected to tensile tests on a testing machine made by the
4.00
Instron company with a traverse speed of 70 mm/min. and a
®
Cu-ETP (Contirod ) - rolling speed 25 m/s reading frequency of 5 pts./s. Furthermore, torsion tests
were carried out. The prepared segments were loaded at
their endings with two counterbalanced torques acting in
The material was subjected to testing during each stage
planes perpendicular to the sample axis. The test was
of the drawing process. In this way, experimental research
concluded at the moment of breakage of the rod. Both
was commenced by the identification of macrostructures
mechanical tests differ from one another by the direction of
and mechanical and electric properties of the listed
application of the vector of force. The purpose of carrying
feedstock with diameters of 8.0 mm. Macrostructural
out these two different mechanical tests was to test if the
photographs of cross-sections and longitudinal sections of
apparent structural differences are reflected in material
materials were taken. Static tensile and torsion testing of
properties when the material is subjected to different
ETP and OFE grade copper was carried out, and electric
deformation schemes.
properties of materials were determined.
Figure 5. presents comparative results from tensile
testing of the materials being studied. Through analysis of
Results and analysis of experimental research
the tensile curves, a significant difference in the process of
The first results of testing, i.e., identification of the
strengthening of Cu-OFE and Cu-ETP copper was
structure of feedstock, have been presented in Fig. 4.
observed. The rods are materials obtained from the process
Identification of makrostructures was carried out using
of hot rolling and possess a fine-grain structure typical for
longitudinal and cross sections of Cu-OFE grade rods cast
copper subjected to dynamic recrystallization. It is
at ten different speeds. The materials exhibit a structure
characterized by high tensile strength and a relatively low
that is typical for classic castings, i.e., for copper cast with
yield point. Oxygen free copper rods are, however, obtained
high speeds in a range from 0.5÷4.0 m/min., a clear
from the process of constant casting and exhibit a structure
structure of equiaxial grains and a zone of column crystals
typical for castings, which, in a way, determines the fact that
perpendicular to the axis of the cast material are
their mechanical properties, for a similar yield point value,
distinguishable. Furthermore, analysis of longitudinal
are lower than for the rolled rods. Differences in the
sections indicates that the lower the casting speed, the
chemical compositions of materials also have an effect on
larger the grains found in the castings. Special attention
these properties.

288 PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011

 Furthermore, three groups of materials with different
courses of tensile curves can be observed: the first group
includes materials cast at industrial speeds using the
Upcast installation, the second group consists of materials
obtained in laboratory conditions using the DCC-AGH®
method, and the third group is comprised of material
obtained using the lowest casting speed in laboratory
®
conditions using the DCC-AGH technique. ®
Fig. 8. DCC-AGH wire rod after tensile test

Figures 6 and 7 present material surfaces after tensile

tests. On the basis of analysis of the photographs, it was
observed that insofar as no significant changes in the
surface of the rod after tensile testing are present in Cu-
ETP grade copper, in the case of the oxygen free copper
rod (Figs. 7., 8.), the surface is uneven, which is a result of
deformation of large crystallites.
Another very important group of tests is in regard to
electric properties, which have been illustrated in Fig. 10.
as a chart of the dependency of electric conductivity as a
function of casting speed. It was observed that lowering
casting speed results in an increase in material
conductivity. Furthermore, attention must be paid to the
fact of how significant the influence of casting speed on the
increase of electric conductivity is relative to the difference
Fig. 5. Tensile curves of Cu-ETP rod and Cu-OFE rods
between the electric conductivity of Cu-ETP grade copper,
for which a value equal to 58.67 MS/m was recorded
On the basis of analysis of data on the strength during measurements, and Cu-OFC grade oxygen free
properties of the studied materials, it was stated that the copper rods cast at different speeds. Furthermore, on the
level of strength obtained by the ETP rod equal to approx. basis of analysis of the presented chart, it was observed
220 MPa, which is significantly higher than that for oxygen that the lower the casting speed, the more coarse-grained
free OFE copper, which oscillates in the range of 120÷195 the material’s structure was. The photograph on the left
MPa. However, the fundamental structural difference shows the structure of the cast rod, which possesses only
between the discussed grades of copper should be taken three grains on its axial section. In turn, the photograph on
into account. the right also shows the macrostructure of a rod cast with a
For oxygen free copper obtained under industrial speed that is 50 times greater. It is visible that the casting
conditions using the Upcast installation, a monotonic possesses a large amount of radial grains oriented
increase in tensile strength was observed with a decrease perpendicularly to the surface. Such distribution is
of casting speed. For the material obtained at a casting dependent upon the method of casting.
speed of 1.0 m/min., the value of tensile strength is equal to
approx. 195 MPa; however, for the oxygen free copper
sample cast at a higher speed of 4.0 m/min., tensile
strength was at a lower level of 180÷185 MPa. This is a
significant difference taking into account the change of only
casting speed with no difference in the chemical
composition of the material as well as the general method
of production.

Rys. 9. Wpływ prędkości odlewania na własności elektryczne

miedzi beztlenowej
Fig. 6. Cu-ETP rod after tensile test
Conclusions and final statements
1. A significant influence of casting process parameters
and cooling conditions (amount and temperature of
water at the input/output of the crystallizer) on shaping
material structure in terms of grain amount and
morphology was stated.
2. A change in the direction of grain orientation from a
direction perpendicular relative to the rod axis, for
®
Fig. 7. Upcast wire rod after tensile test materials cast at high speeds, to parallel to the rod axis,
for materials cast with lower speeds and with a special
direction of the vector of the temperature gradient in the
crystallizer. This conclusion applies to the casting

PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011 289

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characterization of oxygen free copper technology production working and physical metallurgy of non-ferrous metals, 30
Mickiewicza Av., 30-059 Cracow, E-mail: [email protected]

290 PRZEGLĄD ELEKTROTECHNICZNY (Electrical Review), ISSN 0033-2097, R. 87 NR 9a/2011

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