International Tables for Crystallography (2012). Vol. F, Section 6.1.2.1, p. 159.

PART 6. RADIATION SOURCES AND OPTICS

Chapter 6.1. X-ray sources

U. W. Arndt

6.1.1. Overview averaged X-ray intensities from these sources are very low, so
In this chapter we shall discuss the production of the most their application will probably remain limited to time-
suitable X-ray beams for data collection from single crystals of resolved studies (Kleffer et al., 1993).
macromolecules. This subject covers the generation of X-rays and X-rays also arise in the form of channelling radiation resulting
the conditioning or selection of the X-ray beam that falls on the from the bombardment of crystals, such as diamonds, by electrons
sample with regard to intensity, cross section, degree of paralle- with energies of several MeV from a linear accelerator (Genz et
lism and spectral composition. The conclusions drawn do not al., 1990) and in the form of transition radiation when multiple-
necessarily apply to smaller-unit-cell crystals or to noncrystalline foil targets are bombarded by electrons in the range 100–
samples. 500 MeV (e.g. Piestrup et al., 1991). It will be some time before
these new sources can compete with the older methods for
routine data collection.
6.1.2. Generation of X-rays
X-rays are generated by the interaction of charged particles with 6.1.2.1. Stationary-target X-ray tubes
an electromagnetic field. There are four sources of interest to the A section through a permanently evacuated, sealed X-ray tube
crystallographer. is shown in Fig. 6.1.2.1 The tube has a spirally wound tungsten
filament, F, placed immediately behind a slot in the focusing cup,
(1) The bombardment of a target by electrons in a vacuum tube
C, and a water-cooled target or anode, T, approximately 10 mm
produces a continuous (‘white’) X-ray spectrum, called
from the surface of C. The filament–focusing-cup assembly is at a
Bremsstrahlung, which is accompanied by a number of
negative voltage of between 30 and 50 kV, and the target is at
discrete spectral lines characteristic of the target material.
ground potential. The electron beam strikes the target in a focal
The most common target material is copper, and the most
line, which acts as a line source of X-rays. There are usually two
frequently employed X-ray line is the copper K doublet with
pairs of X-ray windows, W, through which the source is viewed at
a mean wavelength of 1.542 Å. X-ray tubes are described in
a small angle to the target surface, thus producing a fore-
some detail in Chapter 4.2 of IT C (2004). We shall consider
shortened effective source, X, which is approximately square in
only the most important points in X-ray tube design here.
one plane and a narrow line in the other. Focus dimensions on the
(2) Synchrotron radiation is produced by relativistic electrons in
target and maximum recommended power loading are shown for
orbital motion. This is the subject of Part 8.
a number of standard inserts in Table 6.1.2.1. None of these are
(3) The decay of natural or artificial radioisotopes is often
ideal for macromolecular crystallography. The assembly of a
accompanied by the emission of X-rays. Radioactive sources
cathode, anode and windows – the tube insert – is inserted in a
are often used for the testing and calibration of X-ray
shock- and radiation-proof shield which is fixed to the table.
detectors. For our purposes, the most important source is
Attached to the shield are X-ray shutters and filters, and some-
made from 55Fe, which has a half-life of 2.6 years and
times brackets for bolting on X-ray cameras. A high-voltage
produces Mn K X-rays with an energy of 5.90 keV.
connection is made to the tube by means of a flexible, shielded,
(4) Ultra-short pulses of X-rays are generated in plasmas
shock-proof cable; nowadays, this high voltage is almost invari-
produced by the bombardment of targets by high-intensity
ably full-wave rectified and smoothed DC.
sub-picosecond laser pulses (e.g. Forsyth & Frankel, 1984). In
earlier work, the maximum pulse repetition frequency was
much less than 1 Hz, but picosecond pulses at more than 1 Hz 6.1.2.2. Rotating-anode X-ray tubes
are now being achieved with mm-size sources. The time- The sealed tubes described above are convenient and require
little maintenance, but their power dissipation, and thus their
X-ray output, is limited. For macromolecular crystallography,
the most commonly used tubes are continuously pumped,
demountable tubes with water-cooled rotating targets [see the

Table 6.1.2.1
Standard X-ray tube inserts
Recommended power loading
Figure 6.1.2.1 Focus size on target (mm  mm) (kW)
Section through a sealed X-ray tube. G, glass envelope; F, filament leads
(at negative high voltage); C, focusing cup; T, target (at ground 8  0.15 0.8
8  0.4 1.5
potential); W, one of four beryllium windows. The electron beam forms a
10  1.0 2.0
line on the target, which is viewed at a small take-off angle to form a 12  2.0 2.7
foreshortened effective source X.

Copyright © 2012 International Union of Crystallography 159 references