X-ray absorption

When passing matter, X-rays are absorbed. If an X-ray beam of the

intensity I passes an absorber of the thickness x with a photon energy dependent
linear absorption coefficient µ(E), the intensity loss will be in good approximation
proportional to the intensity and the absorber thickness:

Integrating this expression delivers the part I(x) of the incident intensity I0 found
behind the absorber:

The linear absorption coefficient µ is correlated with the absorption coefficient β via

where β (listed values e.g.) is the imaginary part of the complex index of
refraction n*:

There are three effects involved in X-ray absorption: the Compton-effect, the
photoelectric effect and the pair production. Each of them contributes to the
absorption cross section σtotal , giving the probability for a photon to interact when
passing a certain thickness of matter:
For most X-ray optical applications with photon energies below 1 MeV are used, the
greatest part of absorption is photoelectric absorption.

Fig. 1: The total mass absorption coefficient for Pb with contributions of photoelectric
absorption, Compton scattering and electron-positron pair formation [Eng 1966]

Photoelectric absorption occurs, when an X-ray photon transfers energy to an

electron in the absorber. As electrons bound in an atom show discrete energy levels,
there are only certain possible portions of energy to undergo transitions between the
different levels. These are shown in fig. 2.
Fig. 2: Relation between electron binding energies, atomic number Z and electronic
transition: download the data [Hen 1993]

For the inner levels, the binding energy grows approximately proportional to the
square of the atomic number Z. This is known as the Moseley's law (Henry Moseley,
1913):

With Planck constanth, the frequency f of the photons absorbed (or emitted) during a
transition of an electron between the electron levels with the main quantum
numbers m and n, Rydberg constantRy, the atomic number Z and a screening
constant K (correction to account for the screening effect of electrons between the
considered electron and the nucleus, screening the charge of the nucleus). Ry is

with the fine structure constant and the Compton wavelengthλC,e of the electron.
Monochromatization and Collimation of X Rays

Nearly all of the data collection experiments require that the energy of the X-ray
radiation be limited to as narrow a band of energies (and hence wavelengths) as
possible. Using a narrow wavelength band of X rays significantly reduces the
fluorescent radiation given off by the sample and makes absorption corrections much
simpler to perform. It has been noted that when the applied voltage for K excitation
occurs, both the Kα and Kβ lines as well as the white radiation curve are observed.
Usually the Kα band is selected for diffraction experiments because of its greater
intensity.

Also, typical data collection methods require that the incident beam be a parallel
beam of photons. To assure that the beam is as parallel as possible (lacking
divergence), the incident beam path is collimated to produce an incident beam that
is about 0.5 mm in diameter for normal focus sources and 0.1-0.3 mm for micro
focus sources.

Filters

When the energy of a photon beam is just above the excitation

potential or absorption edge of a material, that material strongly absorbs the given
photon beam. If another substance can be found that has an absorption edge between
the Kα and Kβ lines of the incident photon beam, this other substance can be used to
significantly reduce the intensity of the Kβ line relative to the Kα line. The
absorption edges of elements with ZFilter = ZTarget - 1 (or - 2) meet this requirement.
The thickness of the filtering material is usually chosen to reduce the intensity of
the Kβ line by a factor of 100 while reducing the intensity of the Kα line by a factor
of 10 or less.

The absorption of X rays follows Beer's Law:

I / Io = exp(-μ × t)

where I = transmitted intensity, Io = incident intensity, t = thickness of material, μ =

linear absorption coefficient of the material. The linear absorption coefficient
depends on the substance, its density, and the wavelength of radiation. Since μ
depends on the density of the absorbing material, it is usually tabulated as the mass
absorption coefficient μm = μ / ρ.

Monochromators

An alternative way to produce an X-ray beam with a narrow wavelength distribution

is to diffract the incident beam from a single crystal of known lattice dimensions. X-
Ray photons of different wavelengths are diffracted from a given set of planes in a
crystal at different scattering angles according to Bragg's Law. Therefore a narrow
band of wavelengths can be chosen by selecting a particular scattering angle for the
monochromator crystal. Crystal monochromators need to have the following
properties.

1. The crystal must be mechanically strong and stable in the X-ray beam.
2. The crystal must have a strong diffracted intensity at a reasonably low
scattering angle for the wavelength of the radiation being considered.
3. The mosaicity of the crystal, which determines the divergence of the
diffracted beam and the resolution of the crystal, should be small.

A variety of geometries are possible for crystal monochromators. Most

monochromators are cut with one face parallel to a major set of crystal planes. These
monochromators are then oriented to diffract Kα lines from this major set of planes.
Some monochromators are cut at an angle to the major set of planes in order to
produce a diffracted beam with a smaller divergence. By properly curving the
monochromator crystal, the diffracted beam may be focused onto a very small area.
This curving may be achieved either by bending or grinding or both bending and
grinding. Curved monochromators are usually reserved for special applications such
synchrotrons.

Graphite crystals cut on the (0002) face are the most common crystals used as
monochromators in X-ray diffraction laboratories. Other special purpose
monochromator materials include germanium and lithium fluoride. In all
commercially available single-crystal instruments, the monochromator is placed in
the incident beam path. Powder diffraction instruments with a point detector
typically place a monochromator in the diffracted beam path to remove any
fluorescent radiation from the sample. Crystal monochromators systematically alter
the polarization of the incident beam, requiring different geometric corrections be
applied to the intensity data.

Collimators

Collimators are objects inserted in the incident- or diffracted-beam path to shape the
X-ray beam. Metal tubes are typically used in single-crystal experiments. The inside
radius of the collimators is typically chosen to be somewhat larger than the size of
the sample so that the sample may be bathed in the incident beam at all times.
Incident-beam collimators are usually manufactured with two narrow regions. The
region closest to the X-ray source carries out the collimation functions. The second
narrow region has a slightly larger diameter than the first and is used to remove
the parasitic radiation that takes a bent path due to interaction with the edge of the
first narrow region of the collimator. Diffracted beam collimators only function to
remove any stray radiation from hitting the detector.
The left end of the collimator shown is mounted on the X-ray tube (or incident beam
monochormator). The small yellow-colored region at the left is the part of the
collimator where the size of the beam is determined. The green region at the right is
chosen to have an opening slightly larger than the region drawn in yellow. This green
region removes the parasitic radiation.

Recently, manufacturers have been selling metal collimators with a single or

multiple glass capillaries. These glass capillaries redirect much of the X-ray beam
that would otherwise be blocked by the collimator. Such capillary inserts in a
collimator have been shown to increase the intensity of the incident beam by a factor
of between two and four.

When a very intense and very small point source is needed, such as in protein
crystallography, X-ray mirrors may be used to shape the incident beam. Mirrors are
sometimes made from materials that act as beta filters for the radiation in use.
Mirrors are primarily used with very bright X-ray sources such as rotating-anode
generators or synchrotrons.

Mirrors

X-ray mirrors are sometimes used in the incident beam to shape the beam as is done
by a collimator. Even with Cu radiation, the spots in protein diffraction patterns are
often very close together. The mirrors act to focus the incident beam into an very
small cross section producing very sharp spots in the diffraction pattern. Mirrors are
often constructed to absorb more of the Kβ radiation than the Kα radiation making
the beam approximately monochromatic. Monochromators significantly reduce the
intensity of the incident beam; omitting the monochromator maximizes the incident
beam flux.

Soller Slits

Powder diffraction experiments usually require a line-shaped incident beam that is

produced from a pair of parallel knife edges. A set of Soller slits are used in the beam
path after the knife edges to remove parasitic radiation that scatters from the edges
of the blades. Soller slits are a set of parallel thin foil sheets that absorb nearly all of
the X rays not traveling parallel to the metal sheets.

Multi-Layer Optics
These optics act somewhat as X-ray mirrors that both focus the X-ray beam and
selectively absorb the Kβ wavelengths producing an intense beam of Kα radiation.