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• Goniometer: the platform that holds and moves the tube, sample, detector, and optics if presented
• X-ray Tube: the source of X-rays
• Detector: count the number of X-rays scattered by the sample
• Incident-beam optics (primary optics): condition the X-ray beam before it hits the sample
• The sample & sample holder
• Receiving-side optics (secondary optics): condition the X-ray beam after it has encountered the
sample

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 Divergence (‫ )התבדרות‬limitation of the X-
ray beam:
• Divergence slit
• Parallel plate collimator
• Soller slit

Refocusing of the X-rays into parallel paths:

• Parallel beam optics
• Göbel (parabolic) mirror
• Focusing mirror and lens
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Removal of unwanted wavelengths:
• Monochromator
• Kβ filter

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• Bragg-Brentano para-focusing geometry (Θ-Θ) – the tube and the detector
move along a circular path centered on the sample. The detector and the tube
maintain a constant angle Θ relative to the sample
• Goniometer radius – a larger goniometer radius improves angular resolution
and enhances the accuracy of peak positions. However, it results in longer
data collection times due to a weaker X-ray beam
• The sample remains stationary in a horizontal position, while the X-ray tube
and detector move simultaneously

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• Electrons from the filament (cathode), usually made of the W, strike the target
anode, producing characteristic radiation
• The material of the anode determines the wavelength of characteristic radiation.
Possible anodes: Fe, Cr, Ni, Co, Cu, Mo, W
• The anode must be cooled because most energy transfers to the heat

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• Only 1% of all electrons that strike the anode generate X-rays, and the rest
lose their energy as heat

• The anode scatters X-rays in all directions, and only about 1.5% are heading in
the right direction
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• 90% of the X-rays transmitted through Be (beryllium) window

• While X-rays leave the tube, they pass through the air, which scatters the
beam from its original path, so about 65% of the intensity reaches the sample

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1% 1.5%  90%  65% = 0.0088%
• Only 0.0088% of the tube energy reaches the sample surface as X-rays

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 Anode Most common use Atomic Wavelength (Å)
material number

K1 K2 K1

Cr For materials with the large unit cell 24 2.290 2.294 2.085
dimensions (organic)
Mn For Ni, Co and Cu alloys 25 2.102 2.106

Fe For applications where Cu and Co tubes 26 1.936 1.940 1.757

cause undesired sample fluorescence
Co For specimens containing Fe in order to 27 1.789 1.793 1.621
avoid fluorescence from Cu Kα radiation

i s Cu Normal powder diffraction work 29 1.540 1.544 1.392

Mo For materials with the small unit cell 42 0.709 0.714 0.632
dimensions (metals). Used for structure
determination for single crystals
W For the medical use. The short wavelength 74 0.209 0.219 0.185
can pass through the human body

Wavelength decreases as the Z number of the anode increases. The higher energy radiation produced from
the anode made of heavier atoms

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• The lifetime of an XRD tube is about 10,000 h 78162700
• At the stationary anode, the cathode shadow is about 10 mm2
• To increase the intensity of X-rays, the current should be increased. Possible
solution: application of a rotating anode at ~ 3,400 rpm. This way, the
generated heat dissipates over the larger surface with a total irradiation area of
about 1500 mm2

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The beam attenuator is an absorber8
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its intensity by a specific factor to a value low enough to be accepted by the
detector. Usually used at small angle diffractions
• Attenuation factors:
Copper 0.1mm ~ 100
Combined copper + nickel (0.2 / 0.02 mm) ~ 10,000

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• Soller slit is a series of closely spaced parallel metal plates where a line source of
X-rays passes through. It collimates )‫ (מקביל‬the incident beam
• It limits the beam spread in the diffraction plane. A set of 0.04 rad Soller slits will
only permit beams less than 0.04 rad away from the diffraction plane
• The distance between the plates is about 0.5 mm 2 app
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• Soller slit made of metals with a large atomic number (Mo, Ta) due to their high
absorption ability
• Usually, the same Soller slit is used in both incident and the diffracted beam

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• Divergence slit is used to limit the divergence (‫ )התבדרות‬of the incident
X-ray beam or to determine the irradiated length on the sample
• Narrow divergence slit:
• reduces the intensity of the X-ray beam
• reduces the length of the X-ray beam hitting the sample
• increases peaks’ sharpness
• improves instrumental resolution so that closely spaced peaks can be
resolved

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As the incident beam angle increases, the

irradiated area decreases, while the X-rays
penetrate deeper into the sample

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• If the slit is too narrow, the insufficient 9627
intensity may be collected at high angles
• If the divergence slit is too wide, the beam
may extend beyond the sample at low angles

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• A beam mask is used to control the irradiated width of the sample
• Beam mask is located just after the divergence slit

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• Anti-scatter slit determines the observed length of the sample

• Reduces the background radiation
• Improves the peak-to-background ratio
• The receiving slit is placed just after the anti-scatter slit and used to limit the
X-ray beam that reaches the detector; it controls the resolution

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XRD patterns of Fe3O4 obtained using Cu tube

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• Selects only Kα radiation by selecting a single crystal with the d-spacing to focus
only the desired radiation (Si, Ge, LiCl)
• Monochromator can be used in primary or diffracted beam geometries
• Combination of the receiving slit with the monochromator removes over 99% of
the unwanted wavelengths

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• A β filter is used to keep as much as

possible of a characteristic Kα
radiation from the tube and to
suppress Kβ and white radiation
• Typically, the material of the β filter
has an atomic number that is one or
two units lower than that of the
anode material in the X-ray tube

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• X-ray solid materials absorbance is described on the plot where µ is an
absorption coefficient
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• Absorption edge (‫ )קצה בליעה קריטי‬is a wavelength correspondingp to the
energy needed to knock an electron out of an atomic orbital
• X-rays are highly absorbed in β filter when the filter’s material wavelength is
slightly higher than the wavelength of the undesired radiation
• A Ni filter, used with Cu radiation, absorbs about 99% of the Kβ radiation but
also about 50% of the Kα
• Kβ material should be with the absorption edge between Kα and Kβ
Cu radiation Kα = 1.542 Å; Kβ = 1.387 Å
Ni filter Ni absorption edge = 1.488 Å
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• The parabolic X-ray mirror (Göbel mirror) converts the divergence X-ray beam
from a tube to an intense monochromatic quasi-parallel beam
• The mirror is usually applied to measure polycrystalline thin films, stressed and
irregularly shaped materials
• The mirror consists of multilayers with laterally graded thickness, deposited with
extreme accuracy onto a prefigured surface made of W/C, W/B4C, Cr/Sc, Au, Ir
• The Kβ radiation is suppressed to less than 0.5% of its original level; making the β
filter unnecessary for analysis conducted with a mirror

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• A diffracted beam collimator used in a quasi-parallel beam geometry to define

the equatorial acceptance angle of the diffracted beam
• Used in thin-film phase analysis and reflectivity
• A collimator consists of a set of parallel plates oriented perpendicular to the
diffraction plane, with variation in the spacing between the plates

20
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• There are three common types of detectors:
➢ Gas proportional 7931012sd
➢ Scintillation (‫)נצנצים‬
➢ Semiconductor

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Detectors consist of two main parts:
➢ Transducer – converts X-ray photon energies mikwad exam current
to an electric
➢ Pulse formation circuit – converts a current into voltage pulses that are
counted, performing a visual indication of X-ray intensity
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• Detectors make the ability of X-ray to ionize the matter

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• X-ray photon interacts with inert gas atoms, ionizing them and generating an ion pair (combination of an
electron and positively charged ion). In a typical detector gas such as Xe, the energy required to remove
an outer electron is about 20.8 eV. Given that each photon from Cu Kα radiation carries an energy of
about 8.04 keV. Thus, the primary ion pairs produced per photon can be calculated as 8040/20.8=387

• The photoelectron loses its energy by ionizing other gas atoms, a process known as secondary ionization
or “avalanche”. The released electrons are attracted to the positively charged W wire (anode), giving rise
to a charge pulse. The pulse height is directly proportional to the energy of the incident X-ray photons

• The detector’s operational lifetime is limited because a portion of the gas gradually escapes through the
window, which is composed of a thin, low-absorbing organic film

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• A scintillator converts incoming photons into flashes of light by absorbing radiation at a specific
wavelength and re-emitting it at a longer wavelength. A commonly used scintillator is NaI doped
with Tl, which emits light photons with wavelengths of around 420 nm (indigo-blue)
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• The emitted light is converted into voltage pulses using a photomultiplier tube. When light photons
strike the CsSb photocathode, each photon generates a burst )‫ (צרור‬of electrons that are then
focused onto a chain of typically 10 sequential photosurfaces, known as dynodes (Ni, stainless steel
or CoBe alloy coated by MgO, GaP, GaAsP). On reaching the dynode, each electron from the
photocathode ejects two electrons, which are then accelerated to the next dynode and so on
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• After the last dynode, the anode collects the accumulated electrons, generating a voltage pulse

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• The Si(Li) detector diode is the most commonly used semiconductor detector. It consists of a p-
type Si doped with Li to increase electrical resistivity. The region infused with lithium atoms
functions as a p-type due to an excess of free electrons

• When X-ray interacts with the Si crystal, they excite electrons from the valence band to the
conductivity band, creating an electron-hole pair. The number of these pairs increases
proportionally with the energy of the incident X-rays. The electrons are then swept from the Si by
an applied potential difference, and a Field Effect Transistor (FET) is then employed to generate a
suitable signal to pass to the main amplifier and subsequently to the counting circuit

• To minimize noise and reduce the motion of Li⁺ ions, the detector must be maintained at liquid
nitrogen temperature (80 K)
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Gas-proportional Scintillation Semiconductor

Working principle Electron – ion pair Conversion to light, Generation and

cascade electrons and their separation of electron –
multiplication hole pairs
Transuding medium Xe NaI:Tl Si, Ge

Noise rate (cps) 1 0.1 – 10 < 0.1

Maximum count rate (cps) 105 – 106 105 – 106 104

Resolution ΔE/E (%) 18 – 20 40 – 50 ~2

Costs Low Medium High

Energy resolution – the ability of the detector to distinguish between energies. The lower the %,
the better the resolution

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• 1D and 2D detectors are used to increase the intensity and reduce measurement time
• In a 1D detector, diffracted signals at different 2Θ angles are simultaneously captured by a strip,
allowing for faster data collection
• A 2D detector incorporates a charge-coupled device (CCD), which provides additional positional
information and further decreases the overall measurement time. However, a drawback of this
detector is its relatively lower resolution

26
• Θ-Θ goniometer with a radius of 150 mm
• X-ray generator with a maximum operating voltage
of 60 kV and a maximum current of 60 mA
• Copper X-ray tube
• Xenon proportional detector
• Secondary curved crystal monochromator
• Prefix X-ray mirror
• Thin film parallel plate collimator
• Beam attenuator
• Ni β filter
• Variety of divergence slits, anti-scatter slits,
receiving slits, Soller slits

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• Θ-Θ goniometer say
• X-ray generator with a maximum operating voltage
of 60 kV and a maximum current of 60 mA
• Copper X-ray tube
• D/teX Ultra250 1D semiconductor strip type
detector (106 cts/line) or 0D scintillation counter
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kitssize 400 µm)
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• Micro-focus optics
• X-Y-Z motorized stage
• Graphite monochromator
• Thin film parallel plate collimator
• Variety of divergence slits, anti-scatter slits,
receiving slits, Soller slits

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