Deformation modes of zirconium at 77°K, 300°K, 575°K, and 1075°K

/ by E.J. Rapperport, C.S. Hartley.

Rapperport, E. J.

http://hdl.handle.net/2027/mdp.39015095018159

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3. At 7 AFC NMI-1221
A nºt-lºº ESEARCH
REPORTS METALLURGY AND CERAMICS

ºº
DEFORMATION MODES OF ZIRCONIUM AT
77 K, 300 K, 575 K, AND 1075'K

By

E. J. Rapperport
C. S. Hartley
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August 12, 1959

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Nuclear Metals, Inc.

Concord, Massachusetts

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UNIVERSITY
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UNITED STATES ATOMIC ENERGY COMMISSION

Technical Information Service |||||
3 9015 09501 8159
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 iii

NMI-1221

Deformation Modes of Zirconium

at 77°K, 300°K, 575°K, and 1075°K

E. J. Rapperport and C. S. Hartley

August 12, 1959

Nuclear Metals, Inc.

Concord, Massachusetts

Contract No. AT (30-1)-1565

A. R. Kaufmann
Technical Director
iv

Deformation Modes of Zirconium

at 77°K, 300°K, 575°K, and 1075°K

E. J. Rapperport and C. S., Hartley

ABSTRACT

A study has been made of the deformation processes active in zirco

nium crystals de formed at 77°k, 300°K, 575°k, and 1075°K. The specimens

were large-grained samples of relatively high purity and wide orientation

distribution.
The only slip system observed at any of the temperatures was of the
form (1010) [1210) with a critical resolved shear stress of about 1.0 kg/m.”
in tension at 77°k, 0.65 kg/m.” in compression at 300°k, 0.20 kg/m.” in
tension at 575°k, and 0.02 kg/m.” in tension at 1075°K. The slip planes

were found by the usual two-trace techniques and the slip direction found
from a detailed analysis of Laue spot asterism which is appended.
active twin planes were {1012}, {1121}, {11223 and {11233 with
The
varying frequencies at the different test temperatures. The most active

at all temperatures was with {1122}, {11233 and {101.23 twins unob
£11213,
served at 1075°K. The absolute thicknesses of the twin families at each

temperature were measured and compared with the twinning shears for the
contributing families to yield deviations from the generalization that
the twinning shear is inversely related to the twin breadth.
 TABLE OF CONTENTS

Page No.

ABSTRACT iv.

I. INTRODUCTION

II. SPECIMEN PREPARATION

A. Material

B. Crystal Growth

C. Orientation Determination

III. EXPERIMENTAL METHODS

IV. EXPERIMENTAL RESULTS

A. Slip
B. Twinning 10

W. DISCUSSION 10

A. Slip 10

B. Twinning 20

WI. SUMMARY 22

VII. ACKNOWLEDGMENTS 24

VIII. REFERENCES 25

IX. APPENDICES - A. Single-Trace Technique for

Determination of Slip or
Twin Planes 27

Determination of Slip Direction

from Asterism on Laue Spots 29
I. INTRODUCTION

Nearly a 11 metals of the hexagonal close-packed structure exhibit

basal slip, i.e., slip. This is true of magnesium”,
(0002) <1120) type
zine”, cadmium", beryllium”, titanium”, yttriun”, and rhenium”.
Some of these, such as titanium and beryllium, display other slip modes

even at room temperature, and nearly all have been reported to slip on
other systems under particular loading or temperature conditions of test
ing. A summary of the active slip and twinning planes in various hexagonal
close-packed metals is given in Table I.
As will be shown in this paper, basal slip was not found at any of
four test temperatures from 77°k to 1075°k in hexagonal close-packed zir
conium under the simple loading conditions of tension and compression,

even though in one case the resolved shear stress on the inactive (0002)

<11202 system was twenty-five times higher than the critical resolved shear
stress on the active (1010) [1210) system.

II. SPECIMEN PREPARATION

A. Material

The zirconium used in this work was of two types: (1) as

deposited reactor grade crystal-bar, and (2) arc-melted and forged reac
tor grade crystal-bar. II
typical chemical and spectrographic
Table shows
analyses of these materials as received, and after hydrogen removal and
crystal growth.

B. Crystal Growth

*
The zirconium was machined into rectangular parallelepipeds
about 0.2-inch square in cross-section and 2 inches long. These were

hand polished through 4/0 abrasive paper, electropolished, given a hydro

gen removal anneal, and to long-time anneals at 840°C in vacuo

to produce usable crystals : A second technique used to obtain large

crystals was to cycle the samples two or three times between 1200°C and
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 Table I (Cont'd.)

Slip

Ҽ.
Systems
Ele Test T
Critical Resolved
Twin
Cla Ref. Shear Stress for Ref.
ment Direc- slip (kg/m2) Planes
Plane
tion

(0.002)|[1120) 7 - {10I2}
Re 1.615 || 300
(1010)|[1210) || 7 - {112.1%
{11223
(10Io)|[I2][o] | 20 10 20
83 -
(1122)|[1100] | 21

(0.002)|[1120) 1 0.0778 22 {1012} 10

Mg
300 - -
(1010)|[1210)
-- 20 4 20
{1011 3 23
24
1.6235 || {30343
(1010)|[I2][o] | 20 1.6 20 £30343 24
425
(1011)|[1210] | 20 1.4 20 £1013} 24

(1010)|[I2][o] | 20 0.13 20 £30343 24

560
(1011)|[1210] | 20 0.1 20 $1013? 24

(0002)|[1120) || 22 0.0655 22
603
(1011)|[1210] 22 0.400 22

(0.002)|[1120) 2 0.0184 25 $101.23 26,27

Zn 1.8563. 300 -
(1122)|[1123] 28,29
Col. 1.8856. 300 (0002)|[1120) 3 0.058 30 {101.23 10

A: Slip direction not determined.

Reported in this paper.

 Table II
Typical Chemical and Spectrographic Analyses of the Zirconium Used.

-
Analyses Given for Material As-received and After Heat Treatment
(Numbers indicate impurity content in parts per million by weight.)

Reactor Grade | Crystal Bar, Arc-melted Arc-melted,

Element Crystal Bar, After Hydrogen | Crystal Bar, After Hydrogen
As-received Removal Anneal | As-received Thermal Cycling
=
Oxygen 235 200 190 185

Carbon 110 30

Nitrogen 6 6 5

Hydrogen 40 2 46

Aluminum 40 20
Calcium 30 30

Chromium 30 30

Copper 20 25

Hafnium 320 320

Iron 220 230 75
Magnesium 6 8

Manganese 5 6

Molybdenum < 10 10

Nickel 40 30

Lead 10 9

Silicon 20 30 <20
Tin 8 15

Titanium < 5 <20

Vanadium <20 < 20
840°c, allowing them to remain at the higher temperature for about 4 hours
and at the lower temperature for 5 days.” These techniques yielded

some grains which occupied the entire cross-section of the bar and were
as long as 3/4 inch.

C. Orientation Determination

After the growth of large crystals by thermal cycling, the

samples repolished with extreme care through 4/0 abrasive paper and
were
electropolished. Metallographic examination after polishing showed the
surfaces to be free of visible deformation traces.
x-ray techniques were used to find
Standard Laue back-reflection
the crystallographic orientations of selected large grains with respect
to a specimen face and edge. Figure 1 shows the stereographic projections
of stress axes for the crystals used. The sharpness of the spots on
the

the Laue photographs indicated that the crystals were of good quality.

III. EXPERIMENTAL METHODS

Nine crystals were deformed in tension at 77°k, nine in tension

and five in compression at 300°K in previous tests,"? fifteen in ten
sion at 575°k, and eleven in tension at 1075°k. All specimens were

stressed by load increments. After a applied, the

predetermined load was

specimen was removed from the loading apparatus and metallographically

examined for deformation traces.

An attempt was made to stress each bar so that some crystals

slipped a small amount and others not at all This was done to bracket
.

the critical resolved shear stress. Some bars of special orientation

(B-11 and B-14) were repolished and annealed at 1075°K for one hour after
lower temperature deformation, their final deformation at 1075°k.
before
In the other bars the loading by increments, followed by metallo
graphic examination, was continued until the surface distortion would
interfere with analysis, or until fracture. One example of a crystal
pulled to fracture is shown in Figure 2. This photograph shows a crystal
 33%
OOO2

<loſox
{loſo) • Tension samples {lizo)
x COMPRESSION SAMPLES
3oo"K

ſoooz] OOO2
(OOO2) 83%

->
º
15D

B15C
<IOIOX <II2O> <IOTo» <IIzo
{Iolo) {II2O) {Ioſo) {lizo)
575°K

Fig. 1 - Orientations of crystals of zirconium. Points indicate

stereographic projections of applied stress directions.
Curved line near (0002) is the locus of points where the
resolved shear stress on the basal system is three times
that on the prism system.
 C

3.2
+ 8, 12 15 2-O 24, 28 - B -- 15 -O 24, 28

Fig. 2 - Sample bar B-14, which failed in crystal B-14C by shear on

tWO symmetrically located {1010} slip planes. The two parts
are rotated 90 with respect to one another about the stress
axis to show both the sharp point projection (right) and the
long edge projection (1eft) of the failure. The approximate
crystal orientation of this grain is indicated by the line
drawings above each part.
(B-14c.) which pulled at 1075°K and failed by slip on two £1010; planes.
was

The approximate orientation of this crystal is illustrated in the Figure .

Specimens were de formed at 77°K in liquid nitrogen on a tensile

machine using an insulated bucket with an internal hook to accept a clamped

specimen . At 575°k the specimens were dead-loaded in air with the loading
linkage passing through a tube furnace. The arrangement at 1075°K Wa S

similar to that at 575°K except that it was necessary to enclose the spe
cimen in an evacuated silica tube (Fig. 3) that was inserted into the fur
nace. For critical resolved shear stress measurements the load was fixed
to the linkage within the silica tube and was applied by lifting the sample
and linkage free of the bottom of the tube. This was accomplished by lift
ing the top rod as shown in Fig. 3. Higher loads were applied by means of
a linkage through the sea 1 at the bottom of the tube.

IV. EXPERIMENTAL RESULTS

A. Slip

The slip planes active at each temperature were determined by

stereographic analysis of the slip traces on sample surfaces . On most of
the crystals, traces on two or more adjacent surfaces could be paired,
which permitted unique determination of the slip plane. (31) Traces on a

single surface were analyzed by the method described in Appendix A. The

only active slip planes at the four temperatures investigated were {101.03.
The slip direction was determined crystals deformed at 300°K
on

and 575°K. At 300°K it was determined from metallographic observation of

the step heights across slip traces on of specially
two adjacent surfaces
19
At; 575°K it was determined by the analysis of
(19)
oriented crystals .
asterism on spots in Laue back-reflection x-ray photographs . The analy
sis of Laue spot asterism is given in Appendix B. Both techniques gave
the slip direction as the close-packed direction <11202.
Critical resolved shear stresses (2...) a t 77°k, 575°k, and 1075°K
were determined by calculating the resolved shear stress on a 11 six sys
tems (three of these are identical in magnitude with the other three but
 §
--
THE

-
-:N

Fig. Assembly
£3r tensile
testing
3
-

of crystals at 1075 K. (A) Specimen;

(B) Clamp; (C) Hook; (D) Wacuum port;
(E) Thermocouple port; (F) Wacuum seal;
(G) Holding nut; (H) Loading hook;
(I) Furnace.
LO

different in sense) in each crystal.

At each test temperature 2 ºr WaS
obtained by noting which of the systems were active and which were not
under various resolved shear stresses. Values of
7.
for the tempera
tures investigated are 1.0 kg/m.” at 77°k, 0.20 kg-mm2 at 575°k, and
0.02 kg/m.” at 1075°K. These results have an estimated precision of

about 10 percent for the crystals tested.

The slip data for the critical resolved shear stress determinations
at 77°k, 575°K and 1075°K are given in Table III. The critical resolved
shear stress at 300°K is 0.65 kg/m.” and was found by direct observation
(19)
of the stress associated with the first visible slip trace.

B. Twinning

The active twin planes at all test temperatures were found by

one-trace (Appendix A) and two-trace stereographic techniques referred to
in the section above. The twin planes were found experimentally at a 11

the test temperatures; however, the other twin elements (shear direction,
shear magnitude,
etc.) were found experimentally only on samples deformed
at 300°K“” (Table IV).
Table V and Table WI summarize the occurrence of the various observed
twin planes at each of the test temperatures. *

At each temperature, measurements were made of the absolute thick

nesses of the active twin families and note was made of the relative fre
quency, or activity, of each family. The absolute thicknesses of the
twins were found by multiplying the projected thicknesses by the sine of
the angle between the twin plane and the plane of projection, the speci
men face. This data is summarized in Figure 4 and Figure 5.

W. DISCUSSION

A. Slip

As may be seen in Table I

the only slip system observed at any
of the test temperatures was of the form (1010)[1210]. Since the absence of
basal slip was considered unusual, specially oriented samples which had
 Table III
Resolved Shear Stresses on Each of the Three (1010)

[T210] Type slip systems in zirconium Crystals

Deformed in Tension at 77°K, 575°K, and 1075°K

Resolved
Crystal
Slip Shear Stress Slip Trace
Typek (1010) [1210] Density##
(kg/mm2)

B-12C A 2.46 H
B-12D A 2.32 H
B-12C B 2.31 H
B-12D B 2.23 H
B-12A A 2.15 H
B-12A B 1.90 H
B-11A A 1. 73 H
B-11C A 1,62 H
B-11D A 1.50 M
B-11D B 1.41 ML
B-11C B 1.33 ML
B-11A B 1.06 WL
B-11A C 0.710 None
B-12B A 0.705 None
B-12B B 0.602 None
B-1 1B A 0. 343 None
B-11C C 0.303 None
B-11B B 0.272 None
B-12A C 0.222 None
B-12D C O. 18.8 None
B-11D C 0.120 None
B-12B C 0.101 None
C 0.096 None
B-12c
| B-11B C 0.082 None
L
(Cont'd. on next page)
 Table III (Cont'd.)

Deformed at 575°K

Resolved
Slip Shear Stress Slip Trace
Crystal
Typek (1010)[1210] Density##
(kg/m”)

B-15B A 1. 31 H
B-15C A 0.858 H
B-16C A 0.848 H
B-15C B 0,840 H
B-15D A 0,838 H
B-15D B 0.836 H
B-15B B 0.812 H
B-16D A 0.808 H
B-16E A 0.765 H
B-16B A 0.741 H
B-15C A 0.658 H
B-15C B 0.658 None
B-16D B 0.655 H
B-15F A 0, 606 H
B-15F B 0. 530 H
B-15E A 0. 505 H
B-16B B 0.476 M
B-16C B 0.458 M
B-16C C 0.436 M
B-16E B 0.385 M
B-16E - C 0.384 M
B-16A A 0.377 H
B-15E B 0.335 M
B-14B A 0.318 M
B-16B C 0.249 ML
B-14C A 0.232 ML
B-16D C 0.208 None
B-14B B 0.207 None
A-44A A 0.207 L
B-16A B 0.175 WL
A-44A B 0, 153 None
B-15E C 0.125 None
B-14C B 0,120 None
B-14C C 0, 109 None
B-14B C 0, 102 None
A-44A C 0, 100 None
B-15F C 0,099 None
B-15B C 0.068 None
B-16A C 0.021 None
B-15C C 0.017 None
B-15D C 0.017 None
B-15C C 0.000 None

(Cont'd. on next page)

 l3

Table III (Cont'd.)

Deformed at 1075°K

crystal | *
Typex
Resolved
Shear Stress
(1010)[1210]
(kg/mm3)
| Slip Trace
Densityºk

B-17C A 0.0344 H
B-17A A 0.0329 H
B-17D A 0.0319 H
B-17C B 0.0298 M
B-17A B 0.0270 M
B-17B A 0.0266 M
B-11A A 0.0210 L
B-11C A 0.019.7 WL
B-11D A 0.0180 WL
B-11D B 0.0169 None
B-17D B 0.0169 None
B-11C B 0.0163 None
B-17D C 0.0154 None
B-17B B 0.0139 None
B-17B C 0.01.30 None
B-11A B 0.01.30 None
B-11A C 0.0080 None
B-17C C 0.0053 None
B-17A C 0.0051 None
B-11B A 0.004 None
B-11B B 0.003 None
B-11C C 0.003 None
B-11B C 0.001 None
B-11D C 0.001 None

* Slip System: A - Most favorably oriented prism

slip system in crystal.
B - Next most favorable.

C - Least favorable.

** Slip Trace Density: H - High; M - Medium; ML -

Medium Low; L - Low; WL -
Very Low; None - None
Observed.
ll.

Table IV

Experimentally Determined Twin Elements for

Various Twin Modes in Zirconium. Samples
Deformed in Compression at 300°K.

S
K1 Žl K2 %2

(1012) [TO11] (1012) [10][1] 0.167

(1121) [1126) (11216) [88163] 0.216

(1122) [TT23] (1124) [2243] 0.225

(1123) -- -- - -

plane.
Kl is the twin

K2 is the second undistorted plane in the twinned

a Tea e

7,
1
is the
-
direction in K,1 perpendicular to the inter
section of K. and K. .
1 2

?,2 is the
- direction in K,2 perpendicular to the inter
section of K- and K. .
1 2

S is the macroscopic shear magnitude of the twinned

volume .

Table V

Activity of Twin Planes in Zirconium at Test

Temperatures of 779K, 3000K, 5750K, and 1075.9K

Plane 77°k | 300°k | 575°k | 1075°k

{101.2} (X) (X) (X) -

{1121} (X) (X) (X) (X)

{11223 (X) (X) (X) -

{1123} (X) (X) (X) -

(X) - Plane observed.

 l:5

Table VI

Summary of Twin Planes Observed in Zirconium Crystals

Pulled in Tension at 779K, 575.9K, and 10759K*

Twin Planes
Temperature
(`K)
#101.23 #1121} | {1122} | {11233

B-11D
B-12A
77 B-12B B-12B B-12B
B-12C B-12C B-12C
B-12D B-12D B-12D B-12D

A-44A A-44A
B-14B B-14B
B-14C
B-15C B-15C
B-15D
B-15E B-15E
575
B-15C B-15C
B-16A
B-16B
B-16C B-16C B-16C
B-16D
B-16E B-16E

1075 :#;

All the entries in this table are either from unique

two-trace analyses or from single-trace analyses in
which only one of the above-listed planes was a pos
sibility.
 l6

6O
| | | | |

5O H. -
op

3
§ 40H -
=
Oſ)

§ 3OH -
:9
# 20 H.
{loſ2}
-
z
>
* Iok-
| -
-
{{22}

O
-º-T—H ū; | I-t
O 2OO 4OO 6OO 8OO IOOO |2OO
TEMPERATURE 2K

Fig. 4 - Plot of absolute twin thickness versus deformation temperature

for zirconium crystals.
 17

I.O H.

">
O
5 2-(12}
;
*
g os F. 2–{IoI2}
E
Q)
Or.
-
{123}
{1122}

| | | | |
O
O 4OO 8OO |200

Temperature *K

Fig. 5 - Schematic plot of relative "frequency" or "activity" of

twin families versus deformation temperature for
zirconium crystals.
18

larger resolved shear stresses on basal slip systems than on prism sys
tems were deformed under relatively high loads. The stress axes of such
(15)
samples are to be found near the (0002) poles on the stereographic
triangles of Figure 1. of the other crystals were de formed under
Many

extreme conditions, even to fracture, with no evidence of basal slip . A

summary of the maximum resolved shear stresses obtained on the basal sys
tems of crystals tested at each of the four temperatures is given in

Table VII. Included in this table is the critical resolved shear stress
for prism slip at each temperature and the ratio of maximum shear stress
on the basal system to the critical resolved shear stress on the prism
system. It may be seen from this table that basal slip, if it occurs at
a11, would be far less favored than prism slip, since it was inactive
even when the ratios of shear stresses were as high as those of Table VII.
It should be noted that these ratios do not take into account the harden
ing which slip on the prism systems might introduce, but since this factor
was of minor importance in the stress level at which the secondary and
tertiary prism systems became active (Table III), it was ignored.
In addition to the samples cited in Table VII there were samples
well oriented for basal slip which were squeezed to some 10 percent strain
in vise and did not show evidence of basal slip (e.g. , B-21 at 300°K).
a
Moreover, in the metallographic search for deformation traces attributable
to basal slip, special care was given to the examination of areas of com
plex stress, such as grain boundaries and twin intersections. In none of
the samples tested was there any sign of basal slip. Thus, it is con
cluded that if basal slip occurs in pure zirconium in the temperature
region studied, it must have critical resolved shear stresses much higher
than those reported for prism slip.
churchman"? has related the presence of basal slip in titanium
to the interstitial impurity content. He found that low interstitial

levels favored prism slip against basal slip. This observation is con- .

sistent with the results herein reported, since no basal slip was found
in zirconium crystals of relatively high purity.
 19

Table VII

Tabulation of the Crystals Having the Highest Measured Resolved

*
Shear Stresses on the Basal Slip System for Each Test Temperature.
All values cited are in tension with the exception of the critical
resolved shear stress on the prism slip system at 300°K.

Maximum Resolved
Ratio:
Shear Stress on | Critical Resolved
(Maximum Shear on
*:::::::-
3 *::::::::::..."
X;
(kg/mmº)
Basal System) to
(Critical Shear on
Crystal Prism System)
Stress |

77 4.1 B-12B 1.0 4.1

300 2.4 B-24A 0.65 3.7

575 1.2 B-16A 0.20 6

1075 0.5 B-11B 0.02 25

20

Figure 6 is a plot of critical resolved shear stress for prism

slip versus temperature. The straight lines drawn through the points is
(32) using
the theoretical form derived by Seeger a model of dislocations
in the slip system penetrating a "forest" of transverse dislocations at
temperatures below a critical temperature, and interaction of dislo
To
cations parallel to the moving one, and having the same Burgers vector,
at temperatures above To Seeger's derivation considered only close-packed
slip planes in face-centered cubic and hexagonal close-packed metals. How
ever, the values found at the four temperatures of this study for prism
slip fall very close to a curve of Seeger's form (Figure 6). Fride1(**)
has postulated that the curve of critical resolved shear stress versus tem
perature has an equation of a rectangular hyperbola. The data reported in
this work for prism slip in zirconium deviates markedly from that form.

The values corresponding to Seeger's "critical temperature" (above

which for slip has only the temperature dependence of the elastic con
2.
stants) and activation energy, which may be taken from Figure 6, yield To
of 690°K and rate determining activation energy, Qo, of 56,000 cal-mole.
The calculated value of temperature-independent contribution of the inter
nal stress field is about 0.02 kg/m", which is consistent with the experi
The calculation was made assum
mentally observed value of at 1075°K.
2.
ing a very low dislocation density of 10°/en.” and a geometrical factor of
(32)
0.2.

B. Twinning

As shown in Table VI and Figure 5, the most frequently observed

twin plane at all temperatures was the {112.13 family. This was followed in
frequency by {1012}, {1122}, and £1123}, through 575°K.
At 77°k, it appeared that the greatest twin activity was due to
£11213 twinning.bulk of the remaining twins were £1122} and $ 101.23,
The
the latter occurring principally at grain boundaries, twin interfaces and
other locations of complex stress, while the former occurred in 1arge,
.O.2
O.
O.
26
O.O 8
4
I

|
|

|
|
|

|
H
H

O
O
2OO 4OO 6OO 8OO |OOO

Temperature *K
§

of

-6
Fig. Plot critical resolved shear stress for prism slip, i.e., (1010)[12][o],
in zirconium as afunction of temperature. Solid line has the form of
Seeger's theoretical curve for close-packed slip planes.
22

close groups extending across entire grains, which was true also of {112.13
twins. The £1123} twins occurred in a few isolated but well-defined cases
in areas of complex stress.
At 300°K #11213 twins were again the most frequently observed.
However, {101.23 twins were next, followed by § 11223, which is the reverse

of the case at 77°K. All three families tended to occur in well-defined

groups frequently extending entirely through a crystal. As before, £11233
twinning was seen much less frequently than the others and was found only
at highly stressed locations.
At 575°K twinning was much less in evidence than at the lower tem
peratures. The £11213 family was still predominant, with £101.23 twins found
only after severe deformation. Both #1122? and $1123; were each found only

a few times, and each time after deformation to fracture of the specimen.
At 1075°K the only twin family found was #1121}. These twins were
observed only after extensive deformation of the specimen.
Figure 4 shows the variation of absolute twin thickness with tem
perature for the observed twin planes. It will be noted that the thick
ness of the £11213 twins remains relatively constant while the £11223 and
{101.23 both become thinner as the temperature deviates from room tempera
ture. The {11233 twins seem to have the same thickness at 77°K and 300°K.
It was not possible to measure the thickness of £1123? twins at 575°K
because of the distortion of the specimen surface.
It may be seen from the plot of Figure 4 and the data in Table IV
that the {1121}, {11223 and {101.23 twins present
deviation from the a
generalization that twin thickness is inversely proportional to the twin
ning shear. (13,34) At room temperature the # 11213 family is substantially
thinner than the {1122} family which has a larger shear. At 77°K the
{1122} family is thicker than either the #101.23 or £11213, both of which
have smaller twinning shear magnitudes .

VI. SUMMARY

1. The only slip system found active in relatively high purity

zirconium was (1010) [I2][o] with a critical resolved shear stress of
 23

about 1.0 kg/m.” in tension at 77°k, 0.65 kg/m.” in compression at 300°K,

0.20 kg/m.” in tension at 575°K, and 0.02 kg/m.” in tension at 1075°K.
Although some specimens were oriented so as to favor basal slip over prism
slip, and stressed so that the resolved shear stress on the basal system
was many times the critical resolved shear stress on the active prism sys
tem, no evidence was found of basal slip.
2. The slip direction for prism slip was experimentally found to
be the close-packed direction.<11207. This was determined both metallo
graphically by examination of step heights of slip traces on specially
oriented crystals, and by analysis of the asterism in Laue back-reflection
x-ray photographs of heavily slipped crystals.

3. It was found that plot of the critical resolved shear stress

a

on the prism systems of zirconium as a function of temperature is in agree

ment with Seeger's predictions for this relationship on close-packed slip
systems. The critical temperature at which the rate of decrease of flow
stress with temperature drops sharply is found to be 690°K. Calculations
for the rate-determining activation energy for the plastic flow process
based on Seeger's theory yield
value of 56,000 cal-mole. A similar
a cal
culation for the temperature-independent contribution of the internal
stress field gave 0.02 kg-mé, the experimentally observed value.

4. Four twin planes were found to be active in zirconium--the

{1121}, {11223, [1123} and {101.23. The £11213 twins were evident at all
test temperatures and were the most abundant. The § 1122} and {101.23 twins
were found 2 approximately the same degree at test temperatures below
1075°K. The #1123} twins were found at test temperatures below 1075°K
in only a few instances, and these were at grain boundaries and other posi
-
tions of complex stress.
The thickness of the #11213 and {1123} twins remained rather con
stant with temperature while the {101.23 and {1122} twins were thickest at
room temperature. The generalization that twin thickness is inversely
proportional to shear does not appear to hold true for the case of the
{1121} and #11223 twins at room temperature and for the # 1121}, #1122}
and #1012} twins at 77°K.
2l,

VII. ACKNOWLEDGMENTS

The authors are indebted to E. Field for helpful experimental sug

gestions aid in angle measurements, and to P, Pointu for enlightening
and
discussion on the techniques for the analysis of Laue asterisms of small
angles. This work was sponsored by the Research Division of the United
States Atomic Energy Commission under Contract No. AT (30-1)-1565.
 25

VIII. REFERENCES

1. E. Schmid, Z. Electrochem., 37, 447 (1931).

2. H. Mark, M. Polanyi, and E. Schmid, Z. Physik, 12, 58 (1922).

3. W. Boas and E. Schmid, Z. Physik, 54, 16 (1929).

4. G. L. Tuer and A. R. Kaufmann, "Ductility of Beryllium as

Related to Single Crystal Deformation and Fracture", The Metal
Beryllium, Editors D. W. White, Jr. and J.
E. Burke (ASM, Cleve
land, 1955), 372.

5. E. A. Anderson, D. C. Jillson, and S. R. Dunbar, Trans. AIME,

Vol. 197, 1191 (1953).
6. E. J. Rapperport and C. S. Hartley. To be published in Trans.
AIME.

7. A. T. Churchman, personal communication. Data to be published.

8. R. I. Garber, I. A. Gindin, and V. V. Shubin, "Slip in Single

Crystals of Beryllium at Low Temperatures, III", Journal of
Experimental and Theoretical Physics, Vol. 36, No. 2, 1959.

9. E. J. Rapperport and S. H. Gelles. To be published.

10. C. H. Mathewson and A. J. Phillips, Technical Publication No. 53,

AIME, 1928.

11. R. I. Garber, I. A. Gindin, W. S. Kogan, and B. G. Lazarev, "X-ray

Investigation of the Plasticity of Beryllium Single Crystals",
Bulletin of the Academy of Sciences of the USSR-Physical Series,
Vol. 20, No. 6, 1956, 639 [From Transactions of the Fifth Confer
ence on the Application of X-rays to the Investigation of Mate
rials (Lenningrad, 1955)].

12. F. D. Rosi, F. C. Perkins and L. L. Seigle, Trans. AIME, Vol. 206,

115 (1956).

13. F. D. Rosi, C. A. Dube and B. H. Alexander, Trans. AIME, Vol. 197,

257 (1953).

14. T. S. Liu and M. A. Steinberg, Journal of Metals AIME, Vol. 4,

No. 10, 1043 (1952).

15. A. T. Churchman, Proceedings of the Royal Society, Series A,

Mathematical and Physical Sciences, Vol. 226, No. 1165, 216
(Nov. 9, 1954).

16. C. J.
McHargue and J. P. Hammond, Acta Met., Vol. 1, No. 6,2 700
(1953).
26

17. E. J. Rapperort, Acta Met., Vol. 3, No. 2, 208 (1955).

18. Iu. N. Sokurskii and L. N. Protsenko, The Soviet Journal of

Atomic Energy, Vol. 4, No. 5 (Translation p. 579) (1958), Trans
lated by Consultants Bureau Inc., New York, N. Y.

19 . E. J. Rapperport, Acta Met., Vol. 7, No. 4, 254 (1959).

20. Robert E. Reed-Hill and William D. Robertson, Trans. AIME, Vol.

209, 496 (1957).

21. R. E. Reed-Hill and W. D. Robertson, Trans. AIME, Vol. 212, 256

(1958).

22. P. W. Bakarian and C. H. Mathewson, Trans. AIME, Vol. 152, 226

(1943).

23. E. Schiebold and G. Siebel, Z. Physik, Vol. 69, 458 (1931).

24. R. E. Reed-Hill and W. D. Robertson, Acta Met., Vol. 5, 717 (1957).

25. D. C. Jillson, Trans. AIME, Vol. 188, 1129 (1950).

26. C. H. Mathewson and A. J. Phillips, Proc. Ins. Metals Div. AIME,

Vol. 90, 143 (1927).

27. E. Schmid and G. Wasserman, Z. Physik, Vol. 48, 370 (1928).

28. J. J. Gilman, Trans. AIME, Vol. 206, 998 (1956).

29. J. J. Gilman, Trans. AIME, Vol. 203, 206 (1955).

30. W. Boas and E. Schmid, Z. Physik, Vol. 54, 16 (1929).

31, C. S. Barrett, Structure of Metals, Second Edition (McGraw-Hill
Inc., New York), 1952.

32. A. Seeger, "The Mechanism of Glide and Work Hardening in Face

Centered Cubic and Hexagonal Close Packed Metals", Dislocations
and Mechanical Properties of Crystals, (John Wiley and Sons,
New York, 1957), 243.

33. J. Fridel, "Regarding Seeger's Paper on Work Hardening", Disloca

tions and Mechanical Properties of Crystals, (John Wiley and Sons,
New York, 1957), 330.

34. R. W. Cahn, "Plastic Deformation of Uranium", AERE Report (M/R-740);

Harwell, Berkshire England (July, 1951).

35. R. Maddin and N. K. Chen, "Geometrica1 Aspects of the Plastic

Deformation of Metal Single Crystals", Progress in Metal Physics,
Vol. 5, 53 (Pergamon Press; London), 1954.
 27

IX. APPENDICES

A. Single-Trace Technique for Determination of Slip or Twin Planes

A method is outlined below to infer the active slip or twin

plane causing a trace only on a single specimen face (or on two parallel
faces). Figure 7 details the stereographic solution.
trace, designated D.T., is first plotted on the
The deformation
stereogram, which has as its projection plane the specimen face under con

sideration. Laue photographs allow plotting the relation of the crystal

orientation to the plane of the sample face and a chosen reference direc
tion on the face.
find the locus of the normals of a 11 possible planes which may
To

have caused this trace, the stereogram is rotated into coincidence with
a standard projection and the great circle normal to the rotated trace is

drawn. This great circle is the locus of possible poles since it

all
represents the plane which is normal to the observed trace. Figure 7 shows
the rotated projection with the normal plane drawn.
By superposing a standard projection onto the rotated projection,

one may identify a 11 poles lying on the locus of possible normals. The
ability to observe all the normals of possible de formation planes is one

of the main advantages of this method. From examination of the possible

poles on many single-trace determinations the active deformation planes
may be inferred. Since, in most cases, the plane of normals will inter
sect only a few poles on the standard projection, the method may provide
strong (although not unique) evidence for the activation of one or another
deformation plane.
28

A"

(OOO2) e

(IOI2)e

"(120)

(IOIO)

Fig. 7 - Stereographic projection of a crystal with deformation trace, D.T.

Projection has been rotated to coincide with a basal standard
projection, some poles of which have been superposed. Most obvious
active plane possibilities are (1012) and (1122).
 29

B. Determination of Slip Direction from Asterism on Laue Spots

representation of a Laue photograph actually used

A schematic
for slip direction analysis is given in Figure 8. In this Figure only
three spots with asterism are shown.
In order to determine the slip direction asterism of Laue
from the
spots by the method described below it is necessary to make the following
assumption:
Theasterism at the Laue spots arises from a bending of the
crystal lattice under the action of slip. This bending takes
place about an axis, termed the Taylor axis, and gives rise
to a rotation of all crystallographic planes their nor
(and

mals) about this axis. The Taylor axis is usually at, or near,
a direction of low indices lying in the slip
crystallographic
plane and perpendicular to the slip direction.”

1. On a stereographic projection of the crystal, plot

the locus of plane normals contributing to the Laue
spot and asterism at A, Figure &

This may be done by approximating the asterism with a

line through its center (Figure 8) and transcribing this line, point by
point, to the stereogram of Figure 9 in the usual manner by the use of
the Greninger chart. This procedure gives directly the locus of the plane
normals of the spot and asterism at A.
Since the Taylor axis makes an arbitrary angle with the plane
whose reflected spot is at A, the rotation of the plane about the Taylor
axis causes the normal to sweep out a segment of a cone in space. By
transcribing the asterism to the stereographic projection as the locus of
normals, one obtains of the small circle that the cone of nor
a segment

mals would produce on the stereographic projection. The axis of this

small circle is the Taylor axis.
To find the Taylor axis it is first necessary to construct a plane
containing a line on the cone of normals and the Taylor axis.
30

-O
(1126)
A
(OIT5) (IOT5)

C B

Fig. 8 - Schematic representation of Laue back-reflection photograph

showing three spots with asterism.
 3l

S
Slip Direction S
within 4° of [itzo] lu
~
“I
-/
Cl
Slip Direction
within 3° of [I2ſo S.
~!
CO Slip Direction
within 5° of [2][o]

TAYLOR AXIS
within 4° of (OOO2)

Fig. 9 - Stereographic solution of Laue spot asterism to obtain the

slip direction.
32

2. Determine a plane containing the Taylor axis

3 * Rotate the stereogram on a Wulff net until the cen

ter of the small circle segment of plane normals at A is tangent to a
small circle on the net.

b. great circle passing from the pole of the Wulff

The
net through the point of tangency is the plane desired, i.e. , the plane of
the Taylor axis and a line on the cone of normals.

The physical basis of this construction may be seen by noting that

the poles of the Wulff net are the axes of the cones associated with all
the small circles drawn on the net. If two cones are tangent, the plane
defined by the line of tangency and one cone axis contains the other cone
axis. Thus, on the stereographic construction two cones (small circles)
were made tangent and the plane containing one axis and the line of tan
gency was This plane therefore contains the axis of the
constructed.
other cone which, in the case developed, is the Taylor axis.
3. Determine the Taylor axis

The procedure given above for spot A yields one plane

containing the Taylor axis (plane AA' of Figure 9). A second plane con
taining this same axis is obtained by repeating the analysis on a second
Laue spot having asterism (spot B of Figure 9 which gives plane BB' of
Figure 9). The intersection of these two planes gives the Taylor axis
uniquely (T.A. on Figure 9). On Figure 9 a third spot C has been analyzed
as a check.

4. Knowing the Taylor axis and the slip plane find the
slip direction
It was assumed that the Taylor axis lies in the slip
plane and perpendicular to the slip direction. Thus, one need only to
construct the great circle of the slip plane and to locate the slip direc
tion as the line on it which is 90° from the Taylor axis. The slip direc
tion is shown on each slip plane in Figure 9.
 33

Sometimes the asterism of a spot may be quite small in angle,

which would make the analysis given above burdensome. In these cases it
may be possible to approximate the asterism with a great circle and to
plot the asterism (not the plane normals) directly on the stereogram.
One may then obtain an approximation to the small circle of the plane
normals by halving the angles between the center of the projection and
points on the great circle of the asterism in the vicinity of the spot
with its asterism. Although the curve of the normals so obtained is not
rigorously correct, one may use the curve in the same manner as described
above without introducing much of an error. This is true because only
the tangent point of the curve is utilized and the same tangent point
would be found for many different forms of curves going through the neigh
borhood of the asterism normals.

If more than one slip system is operative, the Laue spots may have

asterism in more than one direction. These may each be analyzed in a man
ner similar to that described above. Prism slip in hexagonal close-packed

metals is a special case in that the Taylor axis of all the six slip sys
tems is the same direction, the c direction. Thus any combination of
prism slip would yield only one direction of asterism in a Laue photograph.