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Low Temperature Creep of Titanium

R.

ZEYFANG,

R. MARTIN

AND H. CONRAD

Metallurgical Engineering and Materials Science Department, University of Kentucky, Lexington, Ky. 40506 (U.S.A.)

(Received March 9, 1971)

S UMMA R Y

Strain hardenin9 and the deformation dynamics of polycrystalline titanium with 0.20//00eq" total inter- stitial content were investioated over the range of 77°K to 350°K by incremental loadin9 and tempera- ture-change creep tests. The stress-strain curves, thermal activation parameters and force-distance curve derived from the creep tests agree dwith those

obtained from constant strain rate and stress relaxa- tion tests, indicating the equivalence of the three types of test. The present results provide additional support to the concept that the rate controlling

process durin9 the low temperature deformation

of

s-titanium is thermally activated overcoming of inter- stitial solute obstacles.

RESUMF.

Le durcissement par ~crouissage et raspect dyna- mique de la dOformation du titane contenant une teneur en impuretOs interstitielles #quivalente d 0,2°//0 d'oxyg~ne ont ~t~ ktudi#s ~ raide d'essais de fluage diff#rentiels (petites variations brusques de la temperature ou de la contrainte en cours aressai). La temp#rature dtait comprise entre 77° et 350°K. La relation contrainte-d#formation, les paramOtres de l'activation thermique et la courbe force-distance

d~duits des essais de fluage sont les mOmes que ceux qui ont #t~ dOterminOs par traction ~ vitesse con- stante ou par relaxation; ces trois types d'essais sont done #quivalents. Les rOsultats obtenus ren- forcent l'idOe selon laquelle le processus qui rOgle la cinktique de la dOformation du titane ~ basse tem- p#rature est le franchissement avec raide de ragita- tion thermique des obstacles constituks par les atomes en solution d' insertion.

ZUSAMMENFASSUNG

Die Verfestigun9 und Verformungsdynamik vonpoly- kristallinem Titan mit einer Zwischengitteratom- konzentration yon 0.2 % Oeq.wurden im Temperatur- bereich zwischen 77° K und 350° K durch Last-und Temperaturwechsel beim Kriechversuch untersucht. Die aus den Kriechkurven abgeleiteten Verfestigungs- kurven, thermischen Aktivierungsparameter und die Kraft-Abstand-Kurve stimmen mit jenen iiberein, die

aus Verformungsversuchen bei konstanter Abgleitye- schwindigkeit und aus Spannungsrelaxationsexperi - menten erhalten wurden; d.h. alle drei Verformungs- experimente sind dquivalent. Die vorliegenden Ergeb- nisse sind eine weitere Stiitze der Vorstellung, daft der 9eschwindigkeitsbestimmende ProzeJ3 bei der Tieftemperaturverformung yon ~-Titan das thermisch aktivierte Uberwinden interstitieller Fremdatome ist.

INTRODUCTION

including constant strain rate tests 1, changes in strain rate or in temperature during an otherwise constant strain rate test 2-5 and stress relaxation experiments6'7. These investigations indicate that the flow stress can be split in the usual manner s into

The deformation dynamics in unalloyed c.p.h. ~- titanium have been studied extensively in recent years employing a number of testing techniques

Materials Scienceand Engineering

American Society for Metals, Metals Park, Ohio, and Elsevier Sequoia S.A., Lausanne-Printed in the Netherlands

LOW TEMPERATURE CREEP OF TITANIUM

135

a

temperature sensitive component z* and a tem-

(where k is the Boltzmann constant and ~0 contains

perature insensitive

component zu :

the mobile dislocation density, their vibrational frequency, the barrier arrangement and the entropy

 

=

z* IT, ~,

Ci] + z,, [#(T),

?, C D d].

(1)

of activation), the activation volume v* may be ob-

z

is the applied stress resolved in the slip system,

tained from changes in stress during a creep test through the relation

the resolved shear strain rate and # the shear modulus. Both z* and z, depend on the concentra- tion Ci of interstitial impurities; zu also depends on the shear strain 7 and in polycrystalline specimens on the grain size d, whereas z* is relatively independ- ent of strain and grain size. On the basis of thermal activation analysis of test data obtained from changes in strain rate and in temperature during otherwise constant strain rate tension tests, Conrad 3'9 concluded that the rate controlling process during the plastic deforma- tion of unalloyed a-titanium at temperatures below 0.4 the melting temperature is thermally activated overcoming of interstitial solute atoms by disloca- tions gliding on the first order prism planes. Stress relaxation tests at room temperature 6 yielded thermal activation parameters which agreed with those from the constant strain rate type tests, in- dicating the equivalence of the two types of test, and provided additional support for the proposed mechanism. Moreover, the strain hardening which occurred during the stress relaxation was found to agree with that in a constant strain rate test I°. The principal objective of the present investiga- tion was to determine whether strain hardening and thermal activation parameters derived from constant stress creep tests also agree with those obtained when the deformation takes place at a constant strain rate. An agreement would provide additional support for the assumptions underlying the previ- ous analysis 3'9 and the conclusions based thereon. Such agreement has previously been obtained for c.p.h. Mg 11,12 f.c.c,metals ~3,14and b.c.c, metals15, ~6,

but has not yet been demonstrated for unalloyed c.p.h, titanium. In the present study, differential-type: creep tests are employed. Stress-strain ~urves can be derived from incremental loading creep tests by

plotting the sum of the stress increments versus

the

described previously 13,15,18 Assuming that the shear strain rate is given by

sum of the strain

increments

in the manner

v, =kT(Oln ~

\

8z

Jr

(3)

if ~0 and the temperature are constant during the change. The enthalpy of activation can be derived by making a temperature change during a creep test with constant ~o19:

H=kT2F(Oln~

L\

t~T ~/, +

(01n~

\

~z

zu d#] )T ~- ~

"

(4)

The equivalent expression for differential constant strain rate type tests iS 19

H=-kT2\

(3

In ~)

{3z*]

&c }T\~T /~"

(5)

Equation

(5) can

also be used

for creep tests by

deriving

~-),

from the effect of temperature on

the stress-strain curves deduced from the incre- mental loading creep tests.

EXPERIMENTAL PROCEDURE

1. Material

The titanium used in this investigation was a special lot prepared by Battelle with the composition given in Table 1; the oxygen equivalent was calculated takingN=20 and C= ] O as described previous- ly9. Specimens of 2.5 micron grain size were pre- pared by swaging 6 nun diam. rod to 1.5 mm diam.

TABLE

1 : COMPOSITIONOF THE BATTELLETITANIUMIN p.p.m.*

0

C

N

H

Fe

Oeq"

 

at. fi'act.

330 (370)

25 (80)

140 (40)

62

(90)

2 × 10-a

* p.p.m. = parts per million by weight. Numbers in parentheses indicate manufacturer's analysis.

Mater. Sci. Eng., 8 (1971) 134-140

136

R. ZEYFANG, R. MARTIN, H. CONRAD

wire at room temperature without intermediate annealing, and then heating the wire for 30 minutes at 500°C in a vacuum of <10 -5 Torr. Tensile specimens of 50 mm length were cut from the wire and chemically polished in a solution of 30 ~o HF + 70 ~ HNO3 before being tested.

2. Creep tests

Creep tests were performed on the wire specimens with 25 mm gauge length in an Instron machine using the constant load control. The specimens

creep strain was determined by measuring the crosshead displacement with an extensometer of 10-4 cm sensitivity. Typical incremental creep curv-

es for a specimen tested at 193°K are shown in Fig. 1. Load increments of 5 kg and time intervals of 5 to 15 minutes were continued until necking of the specimen occurred. Temperatures below room temperature were established by liquid baths; above room temperature

a resistance furnace was used with temperature

controlled to within _ 2 deg K. Temperature-change

tests were only carried out between 273°K and

0.14

I

I

I

I

 

m

0.12

--

~)

--

o

0.10

-

/

 

A,= 3.3 ram'

 

0.08

006

 

5

~

004

002

 

i

 

I

i

I

I

TIME

--

-

Fig. 1. Typical incremental loading creep curves.

were initially loaded at a constant strain rate of ,,~10 -4 sec-1 to a stress of about 90~ of the yield stress. Incremental creep tests were then started, the load being added in increments of 5 kg. This was accomplished by setting the load controller at a certain starting position and adding the load in- crements with the selector switch of the zero sup- pression unit. The creep curves for each load level were recorded for intervals of 5 to 15 minutes. The

293°K. They were accomplished by alternating between a Dewar flask containing a water and ice mixture and a container with water at room tem- perature. True stress a and true strain e were calculated from the engineering stress and strain in the usual manner using a computer; whenever shear values were needed for analysis they were obtained by taking z=½a and ~=2 e.

Mater. Sci. Eng., 8 (1971) 134-140

LOW TEMPERATURE CREEP OF TITANIUM

137

70

I

I

I

I

I

 

~

m

m

6O

 

_

 

°"

 

:-

o

°

o

 

o

 

_

 

.,~'f~"~-

O

O

~tl~lle

Ti (02% 0~1.1

 
 

o

2.5/~ G.S.

 
 

,~

10-4see-'

 

m

Solid Lines: Constant

Strain

Rote Tests

 

20

Data

Points:Creep Tests

--

ic

I

I

I

I

I

o.oe

0.04

0o6

o.oa

o.~

o.m

Fig. 2. Comparison of stress-strain curves derived from creep tests with those obtained in the usual manner.

EXPERIMENTAL RESULTS

1. Stress-strain

curves

Stress-strain curves derived from the creep curves by plotting the accumulated sum of the stress in- crements versus the sum of the strain increments are shown in Fig. 2. The stress values immediately before and after the load changes are plotted; they correspond to strain rates of about 10 -5 sec -1 and 10 -4 sec -1 respectively. An indication of

the reproducibility of the creep results is provided

by the two sets of data at 193 °K, which

specimens. For comparison, constant strain rate tensile tests at a strain rate of about 10 -4 sec -1 have also been carried out at the same temperatures; these are given by the solid lines in Fig. 2. The stress- strain curves derived from the creep tests are in reasonably good agreement with those determined in the usual manner. From the constant strain rate tensile tests the stresses at 0.2 % true strain have been determined and are shown in Fig. 3 as a function of temperature. Also plotted are the values of o* at 0.2 % true strain determined in the usual manner 2- 4

are for two

~*

=

~-

0650(E~/E6so)

,

(6)

where E is Young's modulus 2°. The values of 0" given here are in accord with those derived in- dependently 4'21 for this material. Similar to the

behavior noted previously 3'9, tT* varies in a linear manner with the square root of the temperature; see Fig. 4. ~ince the stress-strain curves derived from the creep tests are in good accord with those from the constant strain rate tests, it is concluded *

that the effect of temperature

depicted in Figs. 3 and 4 applies to creep as well.

on ~0.2O/o and

(TO.2°/o

E"

4o \

u~

Battelle

(02%

Ti

zs~,Gs

Oeq.)

-

e~2Oo

0

I O-o.*,.~

200

400

600

T (°K)

Fig. 3. The 0.2 % yield stress and effective stress ~*.2O/oas a func- tion of temperature.

Mater. Sci. Eng., 8 (1971) 134-140

138

E"

E E

60

40

*~ 2c

0(~

R. ZEYFANG, R. MARTIN, H. CONRAD

 

I

I

I

I

I

 

Battelle

Ti

(0.2% Oeq.)

~'~

2.5 F

G.S.

 
 

[

I ~°I

I x,'~ Io

 
 

I0

20

T~

--

 

T"'

(*K ''=)

Fig. 4.

*

0"0.20/0 /)S.

TL

2. Stress changes

30

E

E

oo

Fig.

 

I

I

J

I

 

o

o

 

=o~.

iK

I

 

Bottelle

Ti (0.2*/. Oeq.)

2.5p. G.S. a=3.x I0"= sec "l

 

n,

,

I

,

I

-0

0.02

004

i

I

'

I

'

 

13

 

0

 

[]

[3

 

i

 

~bo

 

v

 

o

77

*K

ov

19:5*K

 

BOA

298

*K

 

548

*K

,

I

t

]

t

A=

0.06

008

0.10

6. Th.e strain

rate

sensitivity

parameter

B

strain at various temperatures.

'

=

[0 In'Z\

~-~--a_),r

vs.

From the creep curves of Fig. 1 the strain rates have been derived graphically for each stress increment and plotted as a function of the true strain in Fig. 5. The strain rate sensitivity of the flow stress can be described by the change in strain rate induced by a stress increment:

B_ln~2-1n~l r~(~ln~ ~ ~(~ln~ (7)

=\

The quantity B is shown as a function of the true strain for various test temperatures in Fig. 6. Except for the lowest temperature (77°K), B is almost independent of strain. For the thermal acti- vation analysis to follow an extrapolated value of B at 0.2 ~ true strain is used.

3. Temperature changes

Some specimens were deformed in creep by alternate load and temperature changes; this is illustrated in Fig. 7. The temperature is changed by a small amount (20 deg K) and the resulting change in creep rate determined. Before the change, the spec- imen is unloaded to about 20 ~o of the creep load; the temperature bath is then changed and after the new temperature has been reached, the specimen is reloaded to the stress prior to the change. The term in eqn. (4)

0 In ~

In ~2-1n el

_

(8)

10-4

I

Ti

2.5p. G.S.

193.0K

AL

Battelle

(0.2% Oeq.]

=5Kg

Ao = 3.3mm =

~2

I

\

I

"X

iN

I

\

I

I

i

I

I,

\,

\

I

i0-~

_

Fig.

I

0.02

5. Creep

i I

rate

I

004

vs.

creep

I

0.06

E

strain

during

I

Q08

incremental

I

0.10

loading

I

0.12

creep tests.

0.i4

Mater. Sci. Eng., 8 (1971) 134-140

10-4

--

--

--

_

:

_~

ca I0-B

/

|

0.012

LOW TEMPERATURE

CREEP OF TITANIUM

I

Battelle Ti (0.2% Oeq.)

G.s=2.5~,

x

x

x

-

I

0.014

i

i

i

i

I

I

-

AL:5Kg

i

0,016

I

"2~

I

]

x

I

I

I

I

i

i.

AT= 2

I'

=i=

i

0.018

I I I -- - -- x x x o xx x x x -
I
I
I
--
-
--
x
x
x
o
xx
x
x
x
-
-
I
I
I
0,020
0.022
0.024

139

Fig. 7. Incremental loading and incremental change in temperature during creep.

is then determined by extrapolation in the manner shown in Fig. 7.

4. Thermal activation parameters and force-distance curve

The activation volume v* derived from the creep tests using eqn. (3) is plotted in Fig. 8 as a function of the effective shear stress z*. z* corresponds to the value of the effective stress extrapolated to 0°K in Fig. 4 and v*ois the extrapolated value of the activa- tion volume from the linear region at high stresses to zero effective stress. The results agree with those derived earlier from strain rate change tests 4, and

material and

with those obtained from specimens with various interstitial contents ranging from 0.06 to 1.0

at. % Oeq.4.

of

temperature is depicted in Fig. 9. Values obtained

by eqns. (4) and (5) using creep data are compared

stress relaxation tests 6, on the same

The

enthalpy

of

activation

as

a

function

 

r*(Kg/rnm')

(Creep)

 
 

5

I0

[5

20

25

I

I

I

I

 

a - Titanium

 

Tensile Tests

(Conrad & danes)

--Various

Interstitial

Conlents

o Battelle

Ti

(0.2% Oeq)

 

150

 

Creep

Tests

(Present)

 

*~

V Battelle Ti (02% Oeq.)

*;

o o

,OOo *"

 

(3(

02

04

06

08

I0

Fig. 8. Activation volume v

r*Iro*

as a function of the effective stress r*.

With those using constant strain rate (tensile) data on the same material and on materials of various interstitial contents. It is noted that there exists reasonably good agreement between the present results and previous data and between results based on creep tests and those on constant strain rate (tensile) tests. The force-distance curve for the interaction be- tween dislocations and interstitial barriers is shown in Fig. 10. It is derived by taking F=z*bl* d*= v*/bl* and 1" = b/C:~ 3,4. Again, there is good agree- ment between the creep results and the earlier constant strain rate (tensile) test data.

1.8

I

I a - Titanium

I

I

Tensile Tests (Conrad& Jones)

 

1.6

--Various Interstitial Contents o Battelle (0.2% Oeq.)

1.4

Creep Tests (Present) Battelle (0.2% Oeq.) vEq. 4

 

1.2 -

[] Eq.

5

o

/

-

,.o-

/

/

~0,8 ~

0,6 -

/

:

o4

/,~

 
 

~lO-4sec

-'

,/

 

O0

]

i

I

I

 

200

400

T(~

600

T(°K)

Fig. 9. Activation enthalpy vs. temperature.

Mater. Sci. Eng., 8 (1971) ]34-140

140

R. ZEYFANG, R. MARTIN, H. CONRAD

7xlO-~

I

I

f

I

I

I

I

 

a

-

Titanium

 
 

6

Tensile Tests (Conrad

 

8~ Jones)

 

--

Various

Interstitial Contents

 
 

5

o Battelle

 

(0.2% Oeq.)

 

Creep Tests

(Present)

 
 

,

(0.2°,° o,q.I

 

u.

3

2

I

C

I

[

I

[

v

i

~

 

I

2

3

4

5

6

7

8

d*/b

Fig. 10. Force-distance curve for the rate controlling dislocation- barrier interaction.

DISCUSSION

In the above it was shown that the stress-strain curves, the thermal activation parameters and the force-distance curve derived from data obtained in creep (plastic deformation under constant stress) are in accord with those for plastic flow under a

constant strain rate (where the rate was approxima- tely equal to the average creep rate). This indicates that the two types of testing are equivalent regarding both strain hardening and the deformation dynam- ics, as has been found previously for other met-

als 11-16. An equivalence in results had also

found previously6' 1° in titanium for plastic deforma- tion under a continuously decreasing stress (stress relaxation) and that under a constant strain rate. Thus, the deformation dynamics in all three types of test (constant strain rate, constant stress and constant total strain) are described by eqns. (1)

earlier

and

been

(2). In

the

case

of strain

hardening,

studies 22'23 based

on

constant

strain

rate

tests

yield

 

z,

-- al~b[p(7, d, Ca)]~ ,

 

(9)

where a is a constant of the order of unity, # the shear modulus, b the Burgers vector and p the dislo- cation density, which depends on the strain, grain size and interstitial content. It is therefore expected that this equation also applies to strain hardening in creep and stress relaxation. Since eqn. (9) applies to most strain hardening mechanisms, the specific one responsible for strain hardening in titanium cannot be identified at this time. In regard to the deformation dynamics, the avail-

able experimental evidence indicates that the rate controlling process is thermally activated over- coming of barriers associated with interstitial solute atoms 3- 5,24. The exact nature of these barriers is still not clear24; they may represent the tetragonal distortions associated with interstitials in the tita- nium lattice 25 or they may result from chemical-type bonds between titanium and neighboring intersti- tial atoms 5'2¢.

ACKNOWLEDGEMENT

Financial support for this investigation was pro- vided under Air Force Materials Laboratory Contract F33615-68-C-1052, Dr. H. Gegel tech- nical monitor. Special thanks are also due to the Olin Corporation for the support of undergraduate student R. Martin with an Olin Summer Research Grant.

1 R.

REFERENCES

I. JAFFE, Progr. Metal Phys., 7 (1958) 65.

2 R. N. ORAVA,G. STONEAND H. CONRAD,Trans. Am. Soc.

Metals, 59 (1966) 171.

3 H. CONRAD,Can Phys., 45 (1967) 581.

L

4 H. CONRAD AND R. JONES, The Science, Technology and Application of Titanium, Pergamon, 1970, p. 489.

5 W. R. TYSON, Can. Met. Quart., 6 (1968) 301.

6 G. SARGENT AND H. CONRAD, Scripta Met., 3 (1969) 43.

7 P. P. TUNG AND A. W. SOMMER,Met. Trans., 1 (1970) 947.

of

8

A.

SEEGER, Dislocations

and

Mechanical

Properties

Crystals, Wiley, New York, 1957, p. 243.

9 H. CONRAD,Acta Met., 14 (1966) 1631.

10 G. SARGENT, G. JONES AND H. CONRAD, Scripta Met., 3 (1969) 481.

11 H. CONRAD,L. HAYS, G. SCHOECKAND H. WIEDERSICH,Acta Met., 9 (1961) 367.

12 H. CONRAD,R. ARMSTRONG,H. WIEDERSICHANDG. SCHOECK,

Phil. Mag., 6 (1961) 177.

13 H. CONRAD,Acta Met., 6 (1958) 339.

14 S. K. MITRA AND J. E. DORN, Trans. AIME, 221 (1961) 1206; 224 (1962) 1062.

15 G.

A. STONE AND H. CONRAD, Acta Met., 12 (1964) 1125.

16 R. J. ARSENAULT,Acta Met., 12 (1964) 547.

17

18 H. CONRAD AND W. D. ROBERTSON, Trans. AIME, 209 (1957) 513.

19 H. CONRAD AND H. WIEDERSlCH, Acta Met., 8 (1960) 128.

20 P. E. ARMSTRONGAND H. L. BROWN, Trans. A1ME, 230

H. CONRAD, J. Metals, 16 (1964) 582.

(1964) 962.

21 OKAZAKI AND H. CONRAD, unpublished results.

K.

 

22 JONES AND H. CONRAD, Trans. AIME,

R.

245

(1969)

779.

23 CONRAD AND K. OKAZARI, Scripta Met., 4

H.

(1970) 111.

24 J. KRATOCHVILAND H. CONRAD, Scripta Met., 4 (1970)

25 R. L. FLEISCHERAND W. R. HIBBARD, The Relation Between

the Structure and Mechanical Properties of Metals, NPL

815.

Symposium, HMSO,

1963, p. 261.

Mater. Sci. Eng., 8 (1971) 134-140