Physical structure of matter X-ray Physics

5.4.27-00 Diffractometric Debye-Scherrer measurements for the examination

of the texture of rolled sheets

What you can learn about

 Wavelength
 Crystal lattices
 Crystal systems
 Bravais-lattice
 Reciprocal lattice
 Miller indices
 Structure factor
 Atomic scattering factor
 Lorentz-polarization factor
 Multiplicity factor
 Debye-Waller factor
 Absorption factor
 Bragg scattering
 Characteristic X-rays
 Monochromatization
of X-rays

Principle:
A polycrystalline, cubic face-cen-
tered crystallizing copper powder
sample and a thin copper sheet are
separately irradiated with the radia-
tion from a Roentgen tube with a
copper anode. A Geiger-Mueller

What you need:

X-ray basic unit, 35 kV 09058.99 1
Goniometer for X-ray unit, 35 kV 09058.10 1
Plug-in module with Cu X-ray tube 09058.50 1
Counter tube, type B 09005.00 1
Lithium fluoride monocrystal, mounted 09056.05 1
Universal crystal holder 09058.02 1
Probe holder for powder probes 09058.09 1
Diaphragm tube with nickel foil 09056.03 1
Micro spoon, special steel 33393.00 1
Vaseline, 100 g 30238.10 1
Copper powder, 50 g 30119.10 1
Copper sheet, 0.1 mm, 100 g 30117.10 1
Crucible tongs, l = 200 mm 33600.00 1
Bunsen burner LABOGAZ 470 47536.00 1
Butane-cartridge C206 without valve 47535.00 1
* Software X-ray unit, 35 kV 14407.61 1
* RS232 data cable 14602.00 1
* PC, Windows 95 or higher

Debye-Scherrer diagram of a rolled copper sheet.

* Alternative:
XYt-recorder
Connecting cable, l = 100 cm, red
Connecting cable, l = 100 cm, blue
Complete Equipment Set, Manual on CD-ROM included
Diffractometric Debye-Scherrer measurements for the
examination of the texture of rolled sheets P2542700
11416.97 1 counter tube is automatically swiv-
07363.01 1 elled to detect the radiation that is
constructively reflected from the
07363.04 1
various lattice planes of the crystal-
lites. The Bragg diagrams are auto-
matically recorded. The evaluation
allows the Bragg reflexes to be as-
signed to the individual lattice
planes. In contrast to the powder
sample, the rolled thin sheet gives a
spectrum showing an alignment of
the crystallites (rolled texture), that
is made even more complete by
heating the sheet.
Problems:
1. Record the intensity of the Cu X-rays
back scattered by a cubic crystal-
lizing copper powder sample as a
function of the scattering angle.
2. Assign the Bragg reflexes to the
individual lattice planes.
3. Record the Bragg spectrum of a
thin sheet of copper.
4. Repeat the measurements made in
Task 3 after the sheet of copper
has been subjected to annealing.

258 Laboratory Experiments Physics PHYWE Systeme GmbH & Co. KG D - 37070 Gttingen
 Diffractometric Debye-Scherrer measurements LEP
for the examination of the texture of rolled sheets 5.4.27
-00

Related topics Diaphragm tube with nickel foil 09056.03 1

Crystal lattices, crystal systems, Bravais-lattice, reciprocal lat- Copper powder, 50 g 30119.10 1
tice, Miller indices, structure factor, atomic scattering factor, Copper sheet, 0.1 mm, 100 g 30117.10 1
Bragg scattering, characteristic X-rays, monochromatization Crucible tongs, l = 200 mm 33600.00 1
of X-rays, fiber textures, sheet textures, annealing texture, Bunsen burner LABOGAZ 470 47536.00 1
recrystallization. Butane-cartridge C206 without valve 47535.00 1
Micro spoon, special steel 33393.00 1
Principle Vaseline, 100 g 30238.10 1
A polycrystalline, cubic face-centered crystallizing copper
powder sample and a thin copper sheet are separately irradi- Recording equipment:
ated with the radiation from a X-ray tube with a copper anode. XYt-recorder 11416.97 1
A Geiger-Mueller counter tube is automatically swivelled to Connecting cable, l = 100 cm, red 07363.01 1
detect the radiation that is constructively reflected from the Connecting cable, l = 100 cm, blue 07363.04 1
various lattice planes of the crystallites. The Bragg diagrams or
are automatically recorded. The evaluation allows the Bragg
reflexes to be assigned to the individual lattice planes. In con- Software X-ray unit, 35 kV 14407.61 1
trast to the powder sample, the rolled thin sheet gives a spec- Data cable, 2 x SUB-D, 9 pin 14602.00 1
trum showing an alignment of the crystallites (rolled texture), PC, Windows 95 or higher
that is made even more complete by heating the sheet.

Equipment Tasks
X-ray basic unit, 35 kV 09058.99 1 1. Record the intensity of the Cu X-rays back scattered by a
Goniometer for X-ray unit, 35 kV 09058.10 1 cubic crystallizing copper powder sample as a function of
Plug-in module with Cu X-ray tube 09058.50 1 the scattering angle.
Counter tube, type B 09005.00 1 2. Assign the Bragg reflexes to the individual lattice planes.
Lithium fluoride monocrystal, mounted 09056.05 1 3. Record the Bragg spectrum of a thin sheet of copper.
Universal crystal holder 09058.02 1 4. Repeat the measurements made in Task 3 after the sheet
Probe holder for powder probes 09058.09 1 of copper has been subjected to annealing.

Fig. 1: Experimental set-up

PHYWE series of publications Laboratory Experiments Physics PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen 25427-00 1
 LEP
Diffractometric Debye-Scherrer measurements
5.4.27
for the examination of the texture of rolled sheets
-00

Set-up and Procedure ed rays will only be subject to constructive interference when
Preparation of the copper powder sample Braggs condition is fulfilled, i.e.:
A relatively high sample concentration is obtained when the
powder is mixed with a little vaseline. To do this, transfer a lit- 2 d sin q = l (n = order of diffraction) (1)
tle of the copper powder onto a sheet of paper and use a
spatula to knead it to a firm paste. To achieve the highest con- Copper crystallizes in a cubic face-centered lattice, the unit
centration of material as possible, use very little vaseline (a cell of which has 4 atoms at the coordinates 000, 1/2 1/2 0, 1/2
spatula tip of it). Fill the relatively solid paste into the specimen 0 1/2 and 0 1/2 1/2. For a face-centered lattice consisting only
for powder samples and smooth it flush. Use the universal of one sort of atom, the structure factor, which determines
crystal holder to hold the specimen. which lattice planes contribute to constructive interference of
Preparation of the copper sheet sample the partial waves scattered at the individual lattice elements,
For better handling, use scissors to cut the copper sheet to a the following is valid:
size of (2.5 x 4) cm. The surface of this sample sheet that is to
be examined must be completely free of oxide and brightly | F |2 = 16 f2 with h k l only even or only odd
polished. To achieve this, first use very fine emery paper | F |2 = 0 with h k l mixed (2)
(1,000 grain) to carefully remove any oxide, then use polishing
paste to brightly polish the surface. Clamp a strip of paper where h, k, l = Miller indices of the reflecting lattice planes.
under the sample to firmly fix it in the universal crystal holder. The atomic scattering factor f describes the scattering power
After having carried out the experiment with the brightly pol- of an individual atom and is defined as the scattering ampli-
ished sample, initiate recrystallization of the sample as fol- tude of an atom divided by the scattering amplitude of a free
lows: Heat the sample carefully to a bright redness (approx. electron.
700C) for about 2-3 seconds with a Bunsen burner flame,
then allow the sheet to cool slowly in air. Again carry out the For the cubic crystal system, the spacings d of the individual
subsequent measurement on the bright sample surface. lattice planes with the indices (h k l) are obtained from the
X-ray unit settings: quadratic form:
Acceleration voltage Ua = 35 kV, anode current Ia = 1 mA. Use
the 2 mm diameter double pinhole. Set the goniometer block

2 1h2k2l2 2 (a = lattice constant)
1 1
with line marking at position 7. To obtain a good angle resolu- 2
(3)
dhkl a
tion, push the counter tube holder to the back stop.
Calibration of the goniometer with the LiF single-crystal:
Exact angular positions of Debye-Scherrer reflections are only From this and equation (1), the quadratic Bragg equation is
to be expected when the goniometer is correctly adjusted. obtained for n = 1:
Should the goniometer be out of adjustment for any reason
whatever, this can be overcome by stepwise carrying out of
l2
the following procedure: In the coupled 2:1 mode, set the LiF sin2q
1 h2k2l2 2 (4)
single-crystal at an angle of q = 22.5. Theoretically, the very 4a2
intense 200 reflection from LiF lies at this angle. Now uncou-
ple the rotation of the crystal and the Geiger-Mller counter Fig. 2 shows the Debye-Scherrer spectrum of the copper
tube. Search for the maximum intensity of the reflection by powder sample (Cu, Z = 29).
turning the crystal and counter tube alternately and separate-
ly through a few 0.1 angular steps. Should the maximum be As no filter is used for the monochromatization of the X-rays,
found at 22.3, for example, i.e. 0.2 below the theoretical the fact that the very intense lines resulting from Ka- radiation
value, then couple the crystal and counter tube together again are accompanied by secondary lines resulting from the weak-
and turn the crystal through -0.2 past the zero position. Save er Kb radiation must be taken into consideration when indi-
this corrected zero position by pressing ENTER. The maxi- vidual lines are evaluated.
mum intensity must now be situated exactly at the angle of Such pairs of lines can be identified by means of equation (1).
22.5. Carry out a corresponding positive zero position cor- It is namely approximately true with l(Ka) = 154.18 pm and
rection should the maximum be found at an angle greater than l(Kb) = 139.22 pm that:
22.5.
l1Ka 2
Further settings:
sinqa 154.18 pm
Scanning range: see the Figure. Stepping 0.1; Scanning


1.11
l1Kb 2
(6)
speed: when only very intense reflex lines are to be recorded, sinqb 139.22 pm
then scanning can be relatively rapid at 10 s/. For the identi-
fication of weaker lines, a scanning speed of at least 30 s/ is This value corresponds with the quotients of the sinq values
required for a better signal-noise ratio. The experiment with (Fig. 2) of the pairs of lines 2-1, 4-3, 6-5, 9-7 and 10-8, show-
the sheet of copper can be carried out using a scanning speed ing that the lines 1, 3, 5, 7 and 8 originate from the Cu Kb radi-
of 20 s/. In addition, for a more exact evaluation, it is recom- ation.
mended that the position of the glancing angle be determined The correctness of this conclusion can be shown by a control
to two decimal places and that the zoom function be used for measurement using the diaphragm tube with nickel foil to
the region where lines are close together. reduce the intensity of the Kb radiation. The reflexes in Fig. 3
that were previously assigned to the Kb lines are no longer to
be seen. As the intensity of the Ka- radiation is also somewhat
Theory and Evaluation weakened by the Ni foil, when this is used the detection of
When X-rays of wavelength l strike a mass of lattice planes of reflexes of weak intensity at larger glancing angles is made
a crystal of spacing d at a glancing angle of q, then the reflect- difficult.

2 25427-00 PHYWE series of publications Laboratory Experiments Physics PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen
 Diffractometric Debye-Scherrer measurements LEP
for the examination of the texture of rolled sheets 5.4.27
-00

The Table shows the evaluation of the spectrum shown in
Fig. 2.
Column D of the Table lists the glancing angles q found in the
experiment alongside the individual reflex lines to which they
belong. As it has already been assumed that copper forms a
face-centered lattice, only the permissible hkl triplets for this
type of lattice have been taken into consideration in column B.
Column G lists the lattice plane spacings d calculated using
equation (1), and column H contains the values of the lattice
constant a calculated using equation (3).
The mean value of a obtained is: a = (361.04 0.52) pm;
a/a = 0.15%.
(Literature value: a = 361.52 pm).
The intensities of the individual reflex lines correpsond with
those theoretically expected. With powder samples, the 111
reflex should have the greatest intensity, and the 200 reflex the
next highest intensity. The 220 reflex has a lower intensity.
When the same experiment is carried out on the copper sheet
sample, and this sample aligned to the direction of the prima-
ry radiation, so that this impinges on the sample parallel to the
rolling direction (small recognizable striations run vertically to
the rolling direction), then it is found that the intensity relation-
ships of the individual reflex lines are almost reversed (see
Fig. 3). The 220 reflex now has the greatest intensity, followed
by the 200 and the 111 reflexes. The intensity of the 311 reflex
remains about the same with both samples. These results
remain unchanged when the flat copper sheet sample is
moved round through 90, so that the primary radiation is ver-
tical to the rolling direction.
The rolling process has done away with the previous random
distribution of the individual crystallites. These are now par-
tially unidirectional (rolling texture). It is shown here that for the
most part the crystallites are so directed that both the 100
cube faces as well as the 110 planes lie preferentially parallel
to the rolling direction (see Fig. 4). Whether a further crystallo-
graphic direction lies additionally parallel to the rolling direc-
tion, e.g. whether a 110 direction (i.e. a cube face diagonal) is
directed parallel, cannot be decided here. The formation and
type of the texture of sheet metal is very dependent on the
degree of rolling, among other factors.
When the copper sheet is now briefly heated to redness, the
subsequent analysis shows that the relationships have
changed even more drastically (see fig. 5). The crystallites are
now almost completely aligned as, apart from the weak
remains of a 111 reflex signal (line 2), only the 200 reflex has a
very strong intensity. Annealing has resulted in recrystalliza-
tion, which has resulted in the crystallites being almost com-
pletely aligned with their 100 cube faces parallel to the rolling
plane (see Fig. 4b).

Table 1: Evaluation of the Ka- and Kb Debye-Scherrer lines of Cu.

A B C D E F G H
Line hkl h2+k2+l2 q/ sinq sin2q d/pm a/pm
1(b) 111 3 19.54 0.334464 0.111867 208.12 360.48
2 111 3 21.73 0.370233 0.137073 208.22 360.65
3(b) 200 4 22.75 0.386711 0.149545 180.00 360.00
4 200 4 25.29 0.427000 0.182500 180.45 360.91
5(b) 220 8 33.00 0.544639 0.296632 127.81 361.50
6 220 8 37.11 0.603347 0.364203 127.77 361.39
7(b) 311 11 39.69 0.638633 0.407853 109.00 361.61
8(b) 222 12 41.85 0.667183 0.445133 105.33 361.42
9 311 11 45.08 0.708093 0.501396 108.87 361.08
10 222 12 47.65 0.739043 0.546185 104.31 361.34

PHYWE series of publications Laboratory Experiments Physics PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen 25427-00 3
 LEP
Diffractometric Debye-Scherrer measurements
5.4.27
for the examination of the texture of rolled sheets
-00

Fig. 2: Debye-Scherrer diagram of a copper powder probe Fig. 4: Alignment of the Cu-grains in the plane of the sheet
(rolling plane);
a.) not annealed Cu-sheet; b.) after annealing

Fig. 3: Debye-Scherrer diagram of a rolled copper sheet Fig. 5: Debye-Scherrer pattern of a rolled copper sheet after
annealing

4 25427-00 PHYWE series of publications Laboratory Experiments Physics PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen