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COMPARISON OF POLE FIGURE DATA OBTAINED BY X-RAY DIFFRACTION
AND MICROHARDNESS MEASUREMENTS ON ZIRÇALOY-2*
BINI - AIC - OSSICIAL
P. L. Rittenhouse and M. L. Picklesimer
Metals and Ceramics Division
Oak Ridge National Laboratory
Oak Ridge, Tennessee
ABSTRACT
A rapid and semi quantitative method of determining preferred orientation
on large numbers of Zircaloy-2 specimens was desired. Knoop microhardness
measurements were investigated as a solution to this problem.
The variation of Knoop microhardness measurements on selected planes
as a function of indenter exis relative to crystallographic or fabrication
directions was determined for four lots of polycrystalline Zircaloy-2, on which
both conventional and loverse po.le figures had been determined, and seven
Zircaloy-2 single crystals. Data from the single crystals was used to
construct a polar coordinate hardness contour map. With use of an empirical
relationship between the single crystal hardnesses and those of the poly-
crystalline material conventional pole figures could be constructed which
compare favorably with those determined by X-ray diffraction. A quantitative
relationship with Inverse pole figure data was also obtained.
To determine preferred orientation qualitatively from hardness data
requires a minimum of twelve measurements per plane on three, preferably
orthogonal, planes. The exact procedure requires attention to grain size,
specimen preparation, and indenter load. The time required for preparation,
measurement, and analysis 18 of the order of 45 to 60 min.
-LEGAL NOTICE
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The moment moppure u Nomat of Covenant sponsored work. Malther the ind
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Commentar, ar No en toyut with much contentor.
www
LT 13 APPROVED. PROSEDURES
· ARE ON FILE IN THE REVYT
.
ORNI - AEC - OFFICIAL
visionho
"Research sponsored by the U. S. Atomic Energy Commission under contract
with the Union Carbide Corporation.

INTRODUCTION
The design of structures from a-Zr alloys requires consideration of
preferred orientation and the resulting anisotropy of wechanical properties.
Rapid and semi quantitative methods of evaluacing anisotropy and of determin-
ing preferred orientation are needed for quality control and for examining
the large number of test specimens required in development programs. An
Investigation of the microhardness anisotropy in Zircaloy-2 was undertaken
to ascertain whether these measurements could be used for this task.
EXPERIMENTAL PROCEDURE
Single crystals of Zircaloy-2 were grown by an Q-B-a annealing sequence
using electron-bear heaüing.The orieatation of the crystals was determined
by a conventional back-reflection Laue technique: The crystals were then
mounted in a goniometer head and the desired crystallographic faces were
milled and chemically polished. Polycrystalline Zircaloy-2 specimens were
prepared from fabricated sheets or plates. Inverse pole figures for these
materials were obtained using the x-ray diffraction technique described by
Jetter, McHargue, and williams.?
A Wolpert-Greis Micro-Reflex hardness testing machine was used to make
the Knoop microhardness measurements. The single-crystal aná polycrystalline
specimens were loaded to 0.5 and 2.0 kg, respectively. Seven crystallographic
planes of the single crystals were examined, while six planes of examination
were used in studying Zircaloy-2 polycrystals. The specimens were rotated 10
to 15º after each measurement and from 1 to 8 Impressions made at each :
angle of rotation.
RESULTS
The two angles which were used to relate crystallographic directions
and planes in the hcp cell to the planes of examination of the single crystals
are shown in Fig. 1. Beta is the angle between the g axis, (0001), and the
normal to the plane of examination. Alpha is the angle between the long
diagonal of the Knoop Indenter and the projection of the c axis on the plane
of examination. For example, 17 B = 908 and a = 0°, the plane of examination
is of the (hk10) family and the long diagonal of the indenter 18 parallel to
the (0001).
Knoop microhardness data for the single crysta).g is shown in Table I.
The minimum hardness on any plane with 8 > Ô occurs when a = 0° (the long
diagonal of the indenter 18 parallel to the g axis projection). At constant
values of Q, the hardness is a minimum on the prism planes and increases as
the plane of examination is taken closer to the basal plane, (0001). These
data are consistent with the deformation systems known to operate in Zircaloy-2.
The planes of examination for polycrystalline specimens are shown in
Fig. 2. The R, T, and Ñ planes are perpendicular to the roiling, transverse,
and normal directions, respectively. The TN plane 1s 45 deg from the trans-
verse and normal directions and parallel to the rolling direction. The other
two planes are similarly defined.
Knoop microhardness numbers are plotted against an angle e, which 18
defined as the angle between the long diagonal of the Knoop Indenter and a
reference fabrication direction (see Fig. 2). Two such plots prepared from
data compiled in Table II are given in Fig. 3.
With the hardness data for both single-crystal and polycrystalline
Zircaloy-2 on hand, there remains the task of correlation of this data with
preferred orientation. As a first step it should be recalled that the
1
hardnesses for both the first and second order prism planes, (1010) and
(1120), were essentially identical. This identity of hardnesses has also
been observed in single crystals of iodide-Zr: where data on threr planes,
(1010), (1120), and (3170), Pitted the game hardness curve. We felt it not
11logical to assume that the hardness variation on planes equally inclined
from the prism planes toward the basal plane is a function only of the
angle between the long diagonal of the indenter and the (0001) projection
and not of the particular crystallographic plane. For example, it 18
assumed that the hardness and hardness variation 18 the same on the (1074),
B = 24.6°, for which data were not taken, as on the (127), B = 24.5*, for
which measurements were made.
With this assumption we may plot the hardness data for the single
crystals on polar coordinates and obtain a map of constant hardness contours
as a function of a and B. Such a map is shown in Fig. 4.
From a plot of the polycrystalline data, the angle e for the minimum
hardness in a plane is located and designated 02. An angle vi is read from
the B scale of Fig. 4 at the measured hardness corresponding to 0, along the
line of a = 0°. Similarly, V2, corresponding to 02 = 0+ 10, 18 read from
the hardness at 82 and a = 10°. This process 18 repeated for successive
angular intervals over 90° and the values of " for the different angles are
averaged to give for the plane. We define us the average angle between
the plane of examination and the basal plane, (0001).
The procedure is repeated for each of the specimens and the results are
plotted on a standard Wulff net, as shown in Fig. 5, to define two areas that
contain equal numbers of basal poles. The line separating these two areas.
defines an "average" basal pole figure for the material. The results of the
procedure, together with x-ray diffraction pole figure data, are shova in
Fig. 6, for schedules 9 and J."

An independent check on the values of " calculated from the hardness
.
data was undertaken using quantitative inverse pole figures determined by
x-ray diffraction. The percent of reference direction axes present in
10-deg increments from the basal pole was calculated. This was summed
and plotted as a function of the angle from the basal pole (see Fig. 7).
The X-ray diffraction value of F 18 the angle, measured from the basal
pole, which divides the inverse pole figure into two areas each containing
50% of the reference directions. Table III compares the vis determtued by
X-ray diffraction with those calculated with the hardness map for five
schedules of Zircaloy-2.
There are a number of points to consider before one attempts to use
this method for relating Knoop hardness. to preferred orientation. One
desires to make the fewest possible hardness measurements consistent with
obtaining satisfactory data. In considering this we must look at the
number of planes, the indenter orientations per plane, and the number of
impressions per orientation required.
In no Instance is examination of less than three planes (preferably
orthogonal) acceptable. The hardness curves have always been observed to
be symmetrical about some value of 0, and we have averaged the data over
90°. To find the point of symmetry, indentations must be made at no less
than four indenter orientations over a spread of 135º on each plane.
Generally, 95% of the hardness values for a particular orientation
will fall within a spread of £8; greater than 90% within 15. The spread,
however, depends on the perfection of texture (the greater the perfection
the less the spread), the grain size (less spread for smaller size), and
the specimen preparation (less spread for chemically polished specimens
than for mechanically polished ones). Increasing the load causes a decrease
in the spread related to all these factors. Most importantly, one should
always have 50 or more graias under the indenter. . .
ORNI. ALCOINICIAL
Two examples that show the very minimum effort that we could recommend
are given in Fig. 8. Both examples show a total of 12 impressions per plane
or a minimum requirement of 36 per specimen material. The time required for
measurement and analysis 18 of the order of 45 to 60 min. More impressions
at more orientations will, of course, give a more trustworthy, but perhaps
no more satisfactory, result. Little' advantage is seen in increasing the
number of measurements above what we used, approximately 200 per specimen
material.
CONCLUSION
...
tu
LIONA
Knoop hardness data for polycrystalline Zircaloy-2 can be used to
rapidly determine an "average" basal pole figure for the material when used
in conjunction with single crystal data. The method should be applicable
to any anisotropic material. The results are semiquantitative but quite
useful in quality control and for rapid approximations of the anisotropy
and preferred orientation in polycrystalline Zircaloy-2.
1
**
CRNI - AEC - OFFICIAL
HY
4*
*
.
*
FILT
T*
Table I
-
-
-
Knoop Microhardness of Zircaloy-2 Single Crystals
-
-
-
210 4 3
191 1 3
170 4
132 + 3
115 5
112 1 3
271 1 5
271 1 2
220 6 6
196 3
180 t6
143 43
127
130 4
275 4 3
Au w
229 46
204 6
193 4.6
158 + 5
141 1 3
148 4
266 $ 4
231 1 5
213 + 5
204
178 1 3
161 6 3
265 1 6
276 £ 4
234 1 4
217 4
210 1 5
195 6
184 3
178 # 3
240 + 5
224 64 213 1 3
204 + 3
193 1 4
196 1 1
268 $ 4
264 1 2
244 4 3
224 + 2
218 + 3
209 2
198 1 3
198 1 3
US
ORNI - AEC - OFFICIAL

7
OINI O ALC - Official
Table II
Knoop Microhardness of Polycrystalline Zircaloy-2
deg:
14
206 16
201 1 3
193 4 5
184 £ 6.
176 1 4
165 $ 5
156 + 2
152 1 1
148 + 2
147 6 5
Schedule ga
152 6 242 €
153 4 244 # 2
156 15 246 1 2
161 16 246 # 3
170 6 246 § 3
179 I 245 # 3
287 24 6
193 I do
de 242
198 $ 5 240 # 3
201 f4 237 14
.
MPA
210 + 3
212 14
211 + 2
210 4 3
207 3
202 + 2
199 12
194 £ 5
193 +4
192 22
219 44
217.13
216 6 3
212 + 3
207 $ 5
201 £ 5
195 1 3
192 $ 3
188 1 3
186 1 3
156 # 3
154 2
161 + 3
166 $ 3
177 3
188 5
194 + 2
198 $ 2
202 + 4
204 + 3
172 £ 3.
171 5
172 £ 6
174 1 6
176 $ 6
179 $ 3
182 + 3
186 5 4
191 1 5
192 14
1 93 lop
Schedule ja
201 1 5 215 $4
202 + 6 216 5
204 + 6 214 # 5
208 + 4 211 4
213 1 6 .204 + 5
218 + 6 200 + 6
222 £ 3 193 1 6
224 6 6 187 69
224 64 183 65
222 4 180 6 3
173 I
177 1 6
182 + 6
188 $ 4
193 1 5
198 1 6
204 • 2
205 1 5
208 $ 6.
220 $ 190 # 3
225 £ 5 190 # 5
226 6 190 + 3
224 9 188 2
219 5 188 + 3
211 6 6 188 + 3
205 6 189 14
200 5: 189
198 64 191 4
196 $ % 190.3
•
60
70
80
90
P. L. Rittenhouse and M. L. Picklesimer, Metallurgy of Zircaloy-2:
Part I - The Effects of Fabrication Variables on the Anisotropy of Mechanical
Properties, ORNL-2944 (Oct. 13, 1960); Part II - The Effects of Fabrication
Variables on the Preferred Orientation and Anisotrow of Strain Behavior,
ORNL-2948 (Jan. 11, 1961).
ONI - ACOSTICTAT
Table III
* Determined by X-Ray Diffraction and Knoop Microhardness
Schedulea
X-Ray, doc, KHN
X-Ray,KUN
X-Ray A
KIN
can co
77
77
71
76
72
77
73
67
70
70
73
22
43
70
40
.76
32
46
71
44
16
48
29
17
26
15
51
26
17
34
I
'p. I. Rittenhouse and M. L. Picklesimer, Metallurgy of Zircaloy-2:
Part I - The Effects of Fabrication Variables on the Anisotropy of Mechanical
Properties, ORNL-2944 (Oct. 13, 1960); Part II - The Effects of Fabrication
Variables on the Proierred Orientation and Anisotropy of Strain Behavior, .
ORNL-2948 (Jan. 11, 1961).
w
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-WHO
..
.
*
.
10
L
References
1. J. C. Wilsoa and M. L. Picklesimer, "Variable-Gradient, Electron-Beam i
Heating Methods for Growing Single Crystals of Zirconium," paper presented at
1964 International Conference on Electron and Ion Rean Science and Technology,
Toronto, Canada, May 6-8, 1966, under joint auspices of the Electrochemical
Society and ATME (proceedings to be published by John Wiley & Sons, Inc., New
York).
2. L. K. Jetter, C. J. McHargue, and R. O. Williams, "Method of Represent
ing Preferred Orientation Data," J. Appl. Phys. 27, 368–374 (1956).
3. P. L. Rittenhouse and M. L. Pickles imer, Metallurgy of Zircaloy-2:
Part I - The Effects of Fabrication Variables on the Anisotropy of Mechanical
Properties, ORITT2944 (Oct. 13, 1960); Part II - The Effects of Fabrication
Variables on the Preferred Orientation and Anisotropy of Strain Behavior,
ORNL-2948 (Jan 11, 1961). .
Tables
1. Knoop Microhardness of Zircaloy-2 Single Crystals
II. Knoop Microhardness of Polycrystalline Zircaloy-2
III. * Determined by X-Ræy Diffraction and Knoop Microhardness
V-INIO -
-
-
-
-
-- -
.
(FAM
A
TIPUTO
-ALC
Figures
TUO
1 (ORNL-DWG 65-2081). The Plane of Ecamination in the CPH Cell.
2 (ORNL-DWG 65-2082). Planes of Examination and Reference Directions for
Polycrystalline Zircaloy-2.
3 (ORNL-DWG 65-2390). Knoop Microhardness of Two Schedules of Polycrystalline
Zircaloy-2.
4 (ORNL-DWG 6.-6106). Constant Hardness Contour Map of Single Crystal
Zircaloy-2.
5 (ORNL-DWG 64-6111). Plotting the values Find and
the Pole Figure.
for Determining
6 (ORNL-DWG 64-6110). Comparison of Hardness and X-Ray Data Pole Figures
for Two Schedules of Zircaloy-2.
(ORNL-DWG 65-2084). Percent of Reference Directions vs Angle from Basal
Pole.
8 (ORNL-DWG 65-2083). Number of Orientations and Impressions Comprising
Minimum EPI ort.
ALL - OFFICIAL
[000]
ORNL-DWG 65-2081
ORNI - AEC - ORFICIAL
OXNI-MIC - OISICIAL

WE
OLRD
ORNL-DWG 65-2082
ORNI - AIC - OFFICIAL
ORNI - AIC - OFFICIAL

VIDIA10 - 330 - INO
1151110 - IV - INIO |
ORNI-DMG 65-2390
KNOOP HARDNESS
300
SCHD. 9 ZIRCALOY - 2
KNOOP HARDNESS
300 -
| SCHD. J ZIRCALOY - 2


260
260
220. IN
220----
| .....RT...…........
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100 0
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30 50
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ORNI - AIC - OFFICIAL
ORNI - AEC - OFFICIAL
OANI - ACC-OSSICIAL
ORNL-OWG 64 - 6106
0-90

0-90°
260
240
220
200
180
091
140
0-900
120
Q-100
QRO
ORNI - AEC - OFF
ORNI - AEC - OFFICIAL
ORNI - ACC - OFFICIAL
NVIDILO - DIV-INIO
Fig.5
ND
0
TO
RD
ORNL-DWG 64-6114
ORNL - AIC - OFFICIAL
ORNI - AEC - OFFICIAL
Ruth
Hitit. +-2.

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WID110 - ĐIV - INYO.
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ORNL-DWG 64-6110
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SCHEDULE 9
SCHEDULE J
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H HIGH INTENSITY
M MEDIUM INTENSITY
L LOW INTENSITY
O ZERO
RD
KHN
OINI - AIC - OFFICIAL
ORNI - AIC - OFFICIAL
ORNAIC - OINICIAL
ORNI - AEC - OFFICIAL
OR NL-DWG 65-2084


Schedule 9
% OF REFERENCE AXES
WITHIN V DEG. OF 0001]
0
10 20 30 40 50 60 70 80 90
y-dog.
ORNE - AIC - OFFICIAL
ORNI - AEC - OFFICIAL
O-IV-INIO
- OFFICIAL
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30°
30°
30°
ORNL-DWG 65-2083
ORNI-AIC - OFFICIAL
ORNI - AIC - Ornicial



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DATE FILMED
5 / 26 /65






-
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4
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1.
- LEGAL NOTICE -
This report was prepared as an account of Government sponsored work. Neither the United
States, nor the Commission, nor any person acting on behalf of the Commission:
A. Makes any warranty or representation, expressed or implied, with respect to the accu-
racy, completeness, or usefulness of the information containod in this report, or that the use
of any information, apparatus, method, or process disclosed in this report may not infringe
privately owned rights; or
B. Assumes any liabilities with respect to the use of, or for damages resulting írom the
use of any information, apparatus, method, or process disclosed in this report.
As used in the above, "person acting on behalf of the Commission” includes any em-
ployee or contractor of the Commission, or employee of such contractor, to the extent that
such employee or contractor of the Commission, or @wiployee of such contractor prepares,
disseminates, or provides access to, any information pursuant to his employment or contract
with the Commission, or his employment with such contractor.

END



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