LD
Solid-state physics Physics
Properties of crystals Leaflets P7.1.2.1
X-ray structural analysis
Bragg reflection:
determining
the lattice constants
of monocrystals
Objects of the experiment
Investigating and comparing Bragg reflection at an LiF and an NaCl monocrystal.
Determining the lattice constant a0 of NaCl and LiF.
Principles
Bragg’s law of reflection describes the diffraction of plane set of lattice planes and is often referred to as the glancing
waves at a monocrystal as the selective reflection of the waves angle.
at a set of lattice planes within the crystal. Due to the periodicity
In a cubic crystal with NaCl structure (cf. Fig. 1), the lattice
of the crystal, the lattice planes of a set have a fixed spacing
planes run parallel to the surfaces of the crystal’s unit cells in
d. An incident wave with the wavelength l is reflected with
the simplest case. Their spacing d corresponds to one half the
maximum intensity when the Bragg condition
lattice constant:
n ⋅ l = 2 ⋅ d ⋅ sinq (I)
a0
n: diffraction order d= (II)
l: wavelength 2
d: spacing of lattice planes This lets us use (I) as an equation for determining the lattice
constant a0:
is fulfilled (see experiment P6.3.3.1). The angle q shows the
direction of the incident and reflected wave with respect to the n ⋅ l = a0 ⋅ sinq (III)
In other words, to determine a0 we need to measure the
glancing angle q for a known wavelength l and diffraction
Fig. 1 Three-dimensional representation of the structure of NaCl order n. This method is more precise when the glancing angles
d: Spacing of lattice planes in [1,0,0]-direction are also measured in higher diffraction orders.
a0: lattice constant
In this experiment, the molybdenum x-rays are used as radia-
tion of a known wavelength. Table 1 shows its wavelengths l.
Table 1: Wavelengths of the characteristic x-ray radiation of
molybdenum (weighted means [1])
Line l
pm
Ka 71.08
Kb 63.09
1108-Ste
A Geiger-Müller counter tube is used to detect the x-rays; this
instrument and the crystal are both pivoted with respect to the
incident x-ray beam in 2q coupling – the counter tube is turned
by twice the angle of the crystal (cf. Fig. 2). The zero point q =
08 is characterized by the fact that the lattice planes and the
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P7.1.2.1 LD Physics Leaflets
Apparatus
1 X-ray apparatus . . . . . . . . . . . . . . 554 811
1 End-window counter
for a, b, g and x-ray radiation . . . . . . . 559 01
1 LiF monocrystal for Bragg reflection . . . 554 77
additionally required:
1 PC with Windows 9 x/NT
Fig. 2 Schematic diagram of diffraction of x-rays at a mono-
crystal and 2q coupling between counter-tube angle and
scattering angle (glancing angle)
1 collimator, 2 monocrystal, 3 counter tube
axis of the counter tube are parallel to the incident x-ray beam.
As the lattice planes are seldom precisely parallel to the sur-
face of the crystal, the zero point of each crystal must be
calibrated individually.
Setup
Setup in Bragg configuration:
Fig. 3 shows some important details of the experiment setup.
To set up the experiment, proceed as follows (see also the
Instruction Sheet for the x-ray apparatus):
Safety notes
– Mount the collimator in the collimator mount (a) (note the
The x-ray apparatus fulfills all regulations governing an guide groove).
x-ray apparatus and fully protected device for instructional – Attach the goniometer to guide rods (d) so that the distance
use and is type approved for school use in Germany (NW s1 between the slit diaphragm of the collimator and the
807/97 Rö). target arm is approx. 5 cm. Connect ribbon cable (c) for
The built-in protection and screening measures reduce the controlling the goniometer.
local dose rate outside of the x-ray apparatus to less than – Remove the protective cap of the end-window counter,
1 mSv/h, a value which is on the order of magnitude of the place the end-window counter in sensor seat (e) and
natural background radiation. connect the counter tube cable to the socket marked
Before putting the x-ray apparatus into operation in- GM TUBE.
spect it for damage and to make sure that the high
voltage is shut off when the sliding doors are opened
(see Instruction Sheet for x-ray apparatus).
Keep the x-ray apparatus secure from access by un-
authorized persons.
Do not allow the anode of the x-ray tube Mo to overheat.
When switching on the x-ray apparatus, check to make Fig. 3 Experiment setup in Bragg configuration
sure that the ventilator in the tube chamber is turning.
The goniometer is positioned solely by electric stepper
motors.
Do not block the target arm and sensor arm of the
goniometer and do not use force to move them.
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LD Physics Leaflets P7.1.2.1
– By moving the sensor holder (b), set the distance s2 be- – In coupled scanning mode, move the target back by 10.28
tween the target arm and the slit diaphragm of the sensor (even if this takes you into the negative range!).
seat to approx. 6 cm. – Save the positions of the target and the sensor as the “zero
– Mount the target holder (f) with target stage. position of the measuring system” by pressing TARGET,
– Manually align the target and sensor arm horizontally using COUPLED and b LIMITS simultaneously.
the ADJUST knob and save these positions as the “zero
position of the measuring system” by pressing TARGET, Recording the diffraction spectrum:
COUPLED and b Limits at the same time (see Instruction
– Start the software “X-ray Apparatus”, check to make sure
Sheet for x-ray apparatus).
that the apparatus is connected correctly, and clear any
existing measurement data using the button or the F4
Preparing the PC-based measurement: key.
– Connect the RS−232 output and the serial interface on your – Set the measuring time per angular step Dt = 10 s and the
PC (usually COM1 or COM2) using the 9-pin V.24 cable angular step width Db = 0.18.
(supplied with x-ray apparatus). – Press the COUPLED key to activate 2q coupling of target
– If necessary, install the software “X-ray Apparatus” under and sensor and set the lower limit of the target angle to 48
Windows 9 x/NT (see Instruction Sheet for x-ray apparatus) and the upper limit to 348.
and select the desired language. – Start measurement and data transfer to the PC by pressing
the SCAN key.
– When you have finished measuring, save the measure-
ment series under an appropriate name by pressing the
button or the F2 key.
a) Bragg reflection at an NaCl monocrystal:
– Press the ZERO key to return the target and sensor to the
Carrying out the experiment current zero position.
Notes: – Remove the LiF crystal and carefully mount the NaCl crystal
in its place.
NaCl and LiF crystals are hygroscopic and extremely fragile.
Store the crystals in a dry place; avoid mechanical stresses on Determining the zero position of the measuring system
the crystals; handle the crystals by the short faces only.
– In coupled scanning mode, set the target to about 7.28
If the counting rate is too low, you can reduce the distance s2 using the ADJUST knob.
between the target and the sensor somewhat. However, the – Switch on the tube high voltage with HV on/off.
distance should not be too small, as otherwise the angular
– Leave the target position unchanged and, in sensor scan-
resolution of the goniometer is no longer sufficient to separate
ning mode, manually find the counting rate maximum for
the characteristic Ka and Kb lines.
the first reflection maximum of the Ka line.
– Leave the sensor unchanged in the maximum counting-
rate position and manually find the maximum of the count-
a) Bragg reflection at an LiF monocrystal: ing rate in target mode.
– Switch between sensor and target modes and check
– Loosen knurled screw (g), place the LiF crystal flat on the whether you have found the counting rate maximum.
target stage, carefully raise the target stage with crystal all
– In coupled scanning mode, move the target back by 7.28
the way to the stop and gently tighten the knurled screw
(even if this takes you into the negative range!).
(prevent skewing of the crystal by applying a slight pres-
– Save the positions of the target and the sensor as the “zero
sure).
position of the measuring system” by pressing TARGET,
– Set the tube high voltage U = 35.0 kV and the emission
COUPLED and b LIMITS simultaneously.
current I = 1.00 mA.
Recording the diffraction spectrum:
Determining the zero position of the measuring system
– In coupled scanning mode, set the target to about 10.28 – Start the software “X-ray Apparatus” or clear any existing
using the ADJUST knob. measurement data using the button or the F4 key.
– Switch on the tube high voltage with HV on/off. – Press the COUPLED key to activate 2q coupling of target
– Leave the target position unchanged and, in sensor scan- and sensor and set the lower limit of the target angle to 48
ning mode, manually find the counting rate maximum for and the upper limit to 248.
the first reflection maximum of the Ka line. – Start measurement and data transfer to the PC by pressing
– Leave the sensor unchanged in the maximum counting- the SCAN key.
rate position and manually find the maximum of the count-
ing rate in target mode. – When you have finished measuring, save the measure-
– Switch between sensor and target modes and check ment series under an appropriate name by pressing the
whether you have found the counting rate maximum. button or the F2 key.
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P7.1.2.1 LD Physics Leaflets
Measuring example
a) Bragg reflection at an LiF monocrystal:
Fig. 4 Diffraction spectrum of x-rays in
Bragg reflection to the third diffrac-
tion order at an LiF monocrystal
with logarithmic display of counting
rate R.
Parameters of x-ray tube:
U = 35 kV, I = 1 mA
b) Bragg reflection at an NaCl monocrystal:
Fig. 5 Diffraction spectrum of x-rays in
Bragg reflection to the third diffrac-
tion order at an NaCl monocrystal
with logarithmic display of counting
rate R.
Parameters of x-ray tube:
U = 35 kV, I = 1 mA
Evaluation
– In each diagram, click the right mouse button to access the – For each glancing angle q, calculate the values sin q and
evaluation functions of the software “X-ray Apparatus” and and plot these value pairs in a diagram (see Fig. 6).
select the command “Calculate Peak Center” to evaluate In each case, the results lie along a straight line through the
the diffraction spectra. origin; in accordance with (III), its slope corresponds to the
– Using the left mouse button, mark the “full width” of each lattice constant a0.
peak and write down the center values in a table as the
glancing angle (see tables 2 and 3).
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LD Physics Leaflets P7.1.2.1
Table 3: Glancing angle q of the NaCl crystal
q sin q Line n n⋅l
pm
200
nλ 6.418 0.112 Kb 1 63.06
pm
7.238 0.126 Ka 1 71.08
12.918 0.223 Kb 2 126.12
100
14.578 0.252 Ka 2 142.16
19.558 0.335 Kb 3 189.18
22.158 0.377 Ka 3 213.24
0
0 0,1 0,2 0,3 0,4 0,5
sin ϑ
Results
Fig. 6 Value pairs as a function of sin q
LiF: squares, slope of line = 404.5 pm a) LiF crystal:
NaCl: circles, slope of line = 565.2 pm Measurement result: a0 = 404.5 pm
Literature value [2]: a0 = 402.7 pm
Ion radii [3]: 68 pm (Li+), 133 pm (F–)
Sum of ion radii: 201 pm
b) NaCl crystal:
Measurement result: a0 = 565.2 pm
Table 2: Glancing angle q of the LiF crystal Literature value: a0 = 564.02 pm
Ion radii [3]: 98 pm (Na+), 181 pm (Cl–)
q sin q Line n n⋅l Sum of ion radii: 279 pm
pm
Conclusion: the LiF lattice shows a significantly smaller lattice
constant than the NaCl lattice, as the radii of the ions involved
8.958 0.156 Kb 1 63.06
are smaller.
10.108 0.175 Ka 1 71.08
18.178 0.312 Kb 2 126.12 Literature
[1] C. M. Lederer and V. S. Shirley, Table of Isotopes, 7 th
20.548 0.351 Ka 2 142.16
Edition, 1978, John Wiley & Sons, Inc., New York, USA.
27.918 0.468 Kb 3 189.18 [2] Handbook of Chemistry and Physics, 52nd Edition (1971−
72), The Chemical Rubber Company, Cleveland, Ohio, USA.
31.828 0.527 Ka 3 213.24 [3] Charles Kittel, Introduction to Solid State Physics, John
Wiley & Sons, Inc. New York, USA
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