Properties of X-rays

Cullity Chapter 1
Electromagnetic Spectrum
X-rays are electromagnetic radiation of exactly the same nature as light
but of very much shorter wavelength

Unit of measurement in x-ray region is Å and nm.

1 Å = 10-10 m, 1 nm = 10 Å = 10-9 m

X-ray wavelengths are in the range 0.5 – 2.5 Å.

Wavelength of visible light ~ 6000 Å.
Properties of Electromagnetic Waves
Intensity – the rate of flow of electromagnetic
Electromagnetic radiation can be radiation energy through unit area
considered as wave motion in perpendicular to the direction of motion of the
accordance with classical theory. wave.

E = A exp(iωt − ϕ )

A – amplitude of the wave

ω – frequency (ω = 2πν)
ϕ – phase (ϕ = νt)

According to the quantum theory

electromagnetic radiation can
also be considered as a particles
called photons. Each photon has
associated with it an amount of Relationship between wavelength and frequency:
energy:
E = hν λ = c/ν

h = 6.63×10-34 Js c – velocity of light (~3×108 m/s)

X-ray Spectrum

X-rays are produced when accelerated

electrons collide with the target.
The loss of energy of the electrons
due to impact is manifested as x-rays.
X-ray radiation is produced in an x-ray
tube.
Most of the kinetic energy of the
electrons striking the target is
converted into heat, less than 1%
being transformed into x-rays.

1 2
EK = eV = mv
2

e – electron charge (1.6×10-19 C)

EK – kinetic energy, V – applied voltage,
m – mass of the electron (9.11×10-31 kg),
v – electron velocity (m/sec) X-ray spectrum of Mo at different voltage
Continuous X-ray Spectrum
E0 hν = E3
Continuous spectrum arises due to
the deceleration of the electrons
hitting the target.
E0
This type of radiation is know as
bremsstrahlung, German for hν = E1 E0 – E3
“braking radiation”. E0
It is also called polychromatic,
continuous or white radiation.

Some electrons lose all the energy

in a single collision with a target
atom.
E0 – E1
hν = E2 E0 – E2
atom

electron

x-ray
Properties of the Continuous Spectrum

Smooth, monotonic function of intensity vs wavelength.

The intensity is zero up to a certain wavelength – short wavelength limit

(λSWL). The electrons transfer all their energy into photon energy:

eV = hν max
c hc
λSWL = =
ν max eV
12.398 × 103 λ- in Å
λSWL = V – in volts
V
Properties of the Continuous Spectrum

The total x-ray energy emitted per second depends on the atomic
number Z of the target material and on the x-ray tube current. This
total x-ray intensity is given by

I cont . = AiZV m

A – proportionality constant
i – tube current (measure of the number of electrons per
second striking the target)
m – constant ≈ 2
 The Characteristic Spectrum

Discovered by W.H. Bragg and

systematized by H.G. Moseley.

Hole in
K-shell

X-ray
Ejected K-shell
electron
Incident
electron Hole in
Scattered L-shell
incident electron
The Characteristic Spectrum

The characteristic peak is created in when a hole in the inner shell,

created by a collision event, is filled by an electron from higher energy
shell.
Let a K-shell electron be knocked out -- the vacancy can be filled by an
electron from the L-shell (Kα radiation) or the M-shell (K β radiation).
Properties of the Characteristic Spectrum

Usually only the K-lines are useful in x-ray diffraction.

There are several lines in the K-set. The strongest are Kα1 , Kα2 , Kβ1 .
α1 and α2 components are not always resolved – Kα doublet. Kα1 is always
about twice as strong as Kα2 , while ratio of Kα1 to Kβ1 averages about 5/1.

Some Commonly Used X-ray K wavelengths

(Å)
Element Kα (av.) Kα1 Kα2 Kβ1
Cr 2.29100 2.28970 2.29361 2.08487
Fe 1.93736 1.93604 1.93998 1.75661
Co 1.79026 1.78897 1.79285 1.62079
Cu 1.54184 1.54056 1.54439 1.39222
Mo 0.71073 0.70930 0.71359 0.63229
Properties of the Characteristic Spectrum

The intensity of any characteristic line depends both on the tube

current i and the amount by which the applied voltage V exceeds the
critical excitation voltage for that line. For a K-line:

I K −line = Bi(V − VK ) n

B – proportionality constant
VK – the K excitation voltage
n ≈ 1.5

Characteristic lines are also very narrow, most of them less than 0.001
Å wide (Full Width At Half Maximum).
High intensity and narrow K-lines makes x-ray diffraction possible,
since it generally requires the use of monochromatic radiation.
Moseley’s Law

The wavelength of any particular line decreases as the atomic number

of the emitter is increased.
There is a linear relation between the square root of the line frequency
ν and the atomic number Z :

ν = C (Z − σ )

C and σ – constants.

For Cu: λ = 1.5406 Å

X-ray Absorption

When x-rays encounter any form of matter, they are partly transmitted
and partly absorbed.
It was found experimentally that

I∝x
I – intensity
x – distance

In differential form

dI
− = μ × dx
I

where μ - is linear absorption coefficient

X-ray Absorption

After integration
I x = I 0e − μ x
I0 – incident beam intensity
Ix – transmitted beam intensity

Let’s introduce mass absorption coefficient - μ/ρ (ρ - density). It is

constant and independent of physical state (solid, liquid, or gas). Then

I x = I 0e −( μ / ρ ) ρ x

Values of the mass absorption coefficient μ/ρ are tabulated.

Mass Absorption Coefficient

The mass absorption coefficient of the substance containing more than

one element is a weighted average of the mass absorption coefficients
of its constituent elements.

If w1, w2 , w3 , … are the weight fractions of elements 1, 2, 3, … and

(μ/ρ)1, (μ/ρ)2 , (μ/ρ)3 , … their mass absorption coefficients then

μ ⎛μ⎞ ⎛μ⎞ ⎛μ⎞

= w1 ⎜⎜ ⎟⎟ + w2 ⎜⎜ ⎟⎟ + w3 ⎜⎜ ⎟⎟ + ...
ρ ⎝ ρ ⎠1 ⎝ ρ ⎠2 ⎝ ρ ⎠3
Properties of the Absorption Coefficient

There is a sharp discontinuity in the dependence of the absorption

coefficient on energy (wavelength) at the energy corresponding to the
energy required to eject an inner-shell electron.
The discontinuity is known as an absorption edge.
Away from an absorption edge, each “branch” of the
absorption curve is given by:

μ
= kλ3 Z 3
ρ
k – a constant
Z – atomic number of absorber
I x = I 0e −( μ / ρ ) ρ x
Properties of the Absorption Coefficient

Incident x-ray quanta with energy WK can knock out an electron from K atomic
shell.
νK – frequency of the K absorption edge
hc
eVK = WK = hν K = λK – wavelength of the K absorption edge
λK
VK – K excitation voltage

Absorption coefficients of lead

X-ray Filters
Cu radiation
Usually x-ray diffraction experiments
require monochromatic radiation.

Undesirable wavelength can be

suppressed by passing the beam through
an absorber (filter) which absorption
edge lies just above the parasitic
wavelength.

No Filter Ni Filter
X-ray Filters

The filtration is never perfect. Thicker the filter better the suppression
of Kβ component but this also results in weaker Kα. There is always a
compromise.
X-ray Sources

The tube must have:

„ source of electrons
„ high accelerating voltage
„ metal target

X-ray tube types:

„ Gas tube – the original x-ray tube ⇒ obsolete.
„ Filament tube – most common type of laboratory x-ray source.

Target
Filament

– +
V
Filament X-ray Tube

Ceramic Diffraction X-ray Tube – Physical View

Filament X-ray Tube

Invented by Coolidge in 1913.

The most widely-used laboratory X-ray source.
Major components are a water-cooled target (anode) and a tungsten filament
(cathode) that emits electrons.
A high potential (up to 60 kV) is maintained between the filament and the
anode, accelerating the electrons into the the anode and generating X-rays.
Cooling water is circulated through the anode to keep it from melting (>99% of
input power generates heat).
Interior of the tube is evacuated for the electron beam; thin beryllium windows
transmit the X-rays.

Ceramic Diffraction X-ray Tube –

Schematic View
Aspects of X-ray tube design and
operation
The electron beam produced and controlled by the current that is passed
through the filament.

Stable high voltage and filament current power supplies are needed (old-style
transformers → high frequency supplies).

Power rating: applied potential × electron beam current (example: 50 kV and 40

mA → 2 kW).

Maximum power determined by the rate of heat removal (without water, a tube
can be destroyed in seconds → flow interlocks).

The anode is electrically grounded, while the filament is kept at negative kV’s
(the water-cooled anode won’t short out, and the filament is protected by glass
insulation).
Aspects of X-ray tube design and
operation
A new tube (about $5000) should last several thousand hours.

A new tube should be brought into operation carefully so that the

release of adsorbed gases proceeds slowly.

An important rule of thumb:

„ When turning a tube up, increase the kV first, and then increase the
mA.
„ When turning a tube down, decrease the mA first, and then decrease
the kV.

Beryllium windows are fragile and toxic:

„ don’t shock (mechanically or thermally).
„ don’t touch (and don’t taste!).
Selecting X-ray tube for Application

The shape of the incident beam depends on the focal projection of the filament onto
and from the anode material.
X-ray beams that are parallel with wide projection of the filament have a focal shape
of a line.
X-ray beams that are parallel with the narrow projection of the filament have an
approximate focal shape of a square, which is usually labeled as a spot.
These two focal projections are 90 ° apart in the plane normal to the filament-anode
axis.
As the angle from the anode surface is increased, the intensity of the beam
increases, but the spot also becomes less focused.
Take-off angles are typically in
the 3 - 6 ° range.
Selection of XRD Tubes According to
Anode Material
Anode Atomic Application
Material Number
Copper (Cu) 29 Suitable for most diffraction examinations - most widely used
anode material.
Moly (Mo) 42 Preferably used for examinations on steels and metal alloys
with elements in the range Titanium (Ti) (atomic No. = 22)
to approx. Zinc (Zn) (atomic No. = 30)
Cobalt (Co) 27 Often used with ferrous samples, the Iron (Fe) fluorescence
radiation would cause interference and cannot be eliminated
by other measures.
Iron (Fe) 26 Examination of ferrous samples. Also for use with minerals
where Co and Cr tubes cannot be used.
Chromium (Cr) 24 Used for complex organic substances and also radiographic
stress measurements on steels.
Tungsten (W) 74 Used where an intensive white spectrum is of more interest
than the characteristic.
Rotating Anode X-ray Generator

The maximum power of an X-ray

generator can be greatly increased if a
new cooled surface is continually
presented to the electron beam

Typical rotating anode generators operate

from 12 kW to 18 kW (60 kV/300 mA);
specialized generators will go up to 90 kW
(60 kV/1500 mA)

Rigaku rotating anode

Rotating Anode X-ray Generator

Rotating anode tube housing Tube housing designs

Aspects of Rotating Anode X-ray
Generators
The anode (about 100 mm diameter × 40 mm wide) rotates at speeds of 2400
rpm up to 6000 rpm.
Exceptional dynamic balancing is required.
Rotating anode resides in a high vacuum environment (better than 10-6 Torr)
with both rotation and water feedthroughs.
Impressive water flow rates are necessary.
Electron beam currents exceeding 0.3 A at 60 kV.

Rotating anode generators are expensive and require high

maintenance but are the most powerful laboratory X-ray source
available – higher X-ray fluxes require a synchrotron.
Synchrotron Radiation Sources

Synchrotron radiation is generated

when the charged particles are
accelerated perpendicular to their
trajectory. This is usually achieved by
magnetic fields, e.g. bending magnets
or periodical magnetic devices (so-
called insertion devices). Due to the
relativistic energy of the particles the
generated light has superior
properties:
„ The emitted continuous spectrum
is of high intensity.
„ The natural divergence of the
radiation is very small and collimators
further reduce these values.
„ Distinct linear or circular
polarization, which can be selected
depending on the application.
Synchrotron Radiation Sources
Synchrotron Radiation Sources
X-ray Safety

Radiation safety depends on YOU!

General

A fundamental precept of radiation safety is that the individuals must

assume the responsibility not only for their own safety, but must
ensure that their actions do not result in hazards to others.
General
X-ray Diffractometers

This is an example of an
unenclosed (open) x-ray
diffractometer. As the open x-
ray beam of such an instrument
can be extremely hazardous, it
is far preferable to enclose the
entire x-ray apparatus.
This is an example of properly
enclosed and interlocked x-ray
diffractometer.
If a panel is opened while the x-
ray diffractometer is being used,
the interlock will either shut off
the x-ray or close the shutter,
preventing accidental exposure
to personnel.
The leaded glass windows not
only afford a view of the x-ray
apparatus, but also provide
shielding against radiation.
Causes of Accidental Exposures

Although most x-ray workers do not receive any measurable radiation

above background, accidents related to x-ray devices have occurred
when proper work procedures have not been followed. Failure to follow
proper procedures has been the result of

„ rushing to complete a job,

„ fatigue,
„ illness,
„ personal problems,
„ lack of communication, or
„ complacency.
Four Main Causes of Accidents

Poor equipment configuration, e.g. unused beam ports not covered,

interlock system is not engaged.

Manipulation of equipment when energized, e.g. adjustment of

samples or alignment of optics when x-ray beam is on.

Equipment failure, e.g. shutter failure, warning light failure.

Inadequate training or violation of procedure, e.g. incorrect use of

equipment, overriding interlocks.
Reducing External Exposure

Three basic ways to reduce external exposure to radiation are to

„ minimize time,
„ maximize distance, and
„ use shielding.
 Monitoring X-ray Exposure

Finger Dosimeters

„ Ring dosimeters provide accurate readings for

the radiation you are receiving.
„ By regularly reviewing Dose Exposure Reports,
you’ll be able to monitor radiation levels and
limit the amount of exposure to your
extremities.
„ All rings consists of one natural lithium fluoride
element and offer immersible, bar coded
single-piece construction.

Let say you are exposed to a dose of 100 mrem/year…

Life Expectancy Days Lost

Average estimated days lost due to daily activities

Occupation Days of Life Lost
Being an unmarried male 3,500
Smoking (1 pack/day) 2,250
Being an unmarried female 1,600
Being a coal miner 1,100
Being 25% overweight 777
Drinking alcohol (US average) 365
Being a construction worker 227
Driving a motor vehicle 207
All industry 60
Being exposed to 100 mrem/year of radiation for 70 years 10
Drinking cofee 6
Exposure Limits

rem/year
General Stanford
Adult workers 5.0 0.5
Eye lens 15.0 1.5
Skin, organ, extremities 50.0 5.0
Minors 0.5 0.05
Declared Pregnant Women 0.5 0.05
Members of the Public 0.1 0.01
Exposure Limits

Common Radiation Exposures

Coast to Coast Flight 3.0 mrem
Natural Background Radiation 150 – 300 mrem/year
Chest Radiograph 15 – 65 mrem/view
Screening Mammography 60 – 135 mrem/view
Computerized Body Tomography (20 slices) 3,000 – 6,000 mrem

Biologically Significant Radiation Exposures

mrem
Risk of contracting cancer increased 0.09% 1,000
Temporary Blood Count Change 25,000
Permanent sterilization in men 100,000
Permanent sterilization in women 250,000
Skin Erythema 300,000
Radiological Signs
http://www.stanford.edu/group/glam/xlab/Main.htm

http://www.stanford.edu/group/glam/xlab/Safety/Authorization.htm