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**The Strain-rate, Temperature and Pressure
**

Dependence of yield of Isotropic

Poly(methylmethacrylate) and

Poly(ethylene terephthalate)*

R. A. D U C K E T T , S. R A B I N O W I T Z t , I. M. W A R D

Department of Physics, University of Leeds, Leeds 2, UK

**The yield behaviour of poly(methylmethacrylate) (P M M A) has been investigated in tension
**

and compression over a range of testing temperatures and strain-rates. Both tensile and

compressive yield stresses were found to increase monotonically with increasing strain-

rate and decreasing temperatures. Compressive yield stresses were in general found to be

more dependent on strain-rate.

The results of this investigation have been correlated with previous published data for

the dependence of the torsional yield stress of P M M A on hydrostatic pressure. This was

done by a modification of a theory proposed by Robertson which uses the internal viscosity

approach to yield in glassy polymers. The modified theory clearly explains the temperature

and strain-rate dependence of the yield stress and provides a quantitative explanation of

the differences in behaviour between tension and compression in terms of the dependence

of yield on the hydrostatic component of the applied stress.

The tensile yield behaviour of isotropic amorphous poly(ethylene terephthalate) (PET)

sheets has also been investigated over a wide range of temperatures and strain-rates. No

torsion or compressive yield stresses are available because of the sheet form of the PET,

but the results obtained in tension are shown to be fully consistent with the above theory,

and with other published work.

**1. Introduction drawn between a pressure dependent von Mises
**

Many workers have attempted to extract from yield criterion and the Coulomb criterion used

the complex non-linear mechanical behaviour of widely in soil mechanics [2, 3]. However, a

isotropic glassy polymers simple failure criteria modification of the yon Mises criterion proposed

which can be used to predict yield behaviour by Hill [5] to allow for anisotropy has been used

under the combined stresses of constant strain- successfully to describe the tensile yield of aniso-

rate and temperature e.g. [1-3].These approaches tropic polymers [6-8].

draw on experience obtained in investigations of Other papers have concentrated on the depend-

the yield behaviour of metals and soils. The yon ence of tensile stress on testing temperature and

Mises criterion, successful for describing the strain-rate. Many of the discussions centre

yield of metals [4], has been found to be inade- around the problem of establishing time-

quate for dealing with polymeric materials temperature superposition, e.g. [9-12]. All the

because of the observed difference in yield stress polymers investigated show a monotonic increase

between tension and compression. The latter has of yield stress with increasing strain-rate and

been attributed to a dependence of yield stress some authors assert that there is an approximately

on the hydrostatic component of stress, but the linear relationship between stress and the

limited range of experimental data presently logarithm of strain-rate. The yield stress for most

available does not allow a clear distinction to be glassy polymers decreases linearly with increas-

*Paper presented at Cambridge, April 1970, during conference on "Yield, Deformation and Fracture of Polymers".

~Present address: Ford Motor Co, P.O. Box 2053, Dearborn, Michigan 48121, USA.

9 1970 Chapman and Hall Ltd. 909

R. A. DUCKETT,S. RABINOWITZ,I. M. WARD

ing temperature over a wide range of tempera- sion type load cell, and also using a compression

tures below the glass transition temperature. cage in conjunction with a tensile load cell.

In this investigation an attempt has been made True yield stresses were obtained by relating

to link together the two approaches to yield out- the maximum observed load to current cross-

lined above. The tensile and compressive yield sectional area. A correction to all measurements

stresses of poly(methylmethacrylate) have been was made to allow for deformation of the

measured over a range of temperatures and machine and compression cage.

strain-rates. It was found that the compressive

yield stress was more sensitive to strain-rate than 3, Results

the tensile yield stress. The theory for yielding of The results obtained are shown graphically in

isotropic glassy polymers proposed by Robertson figs. 1 and 2. Fig. 1 represents the variation of

[13] has been modified to allow for the effect of tensile and compressive yield stresses of P M M A

hydrostatic pressure. Using this modified theory with log10 (strain-rate) at various temperatures.

it has been possible to correlate quantitatively In order for easy comparison to be made

the tensile and compression data from this between tension, compression and torsion data

investigation with the data obtained on the same and also with the Robertson theory, the shear

material in torsion tests under an overall hydro- component of the yield stress is plotted as the

static pressure [14]. ordinate and log10 (shear strain-rate) as the

The tensile yield stress of isotropic amorphous abscissa. In fig. 2 the results obtained for the

poly(ethylene terephthalate) sheet has also been tensile yield of P E T at -- 25, 20, 40, 50 and

measured over a wide range of temperatures and 6 0 ~ are plotted as the tensile component of

strain-rates and fitted to the above theory using stress versus log10 (tensile strain-rate).

parameters deduced from the literature. Fig. 3 is taken from Rabinowitz et al [14] and

represents the variation of torsional yield stress

2. Experimental of P M M A at constant (room) temperature and

The poly(methylmethacrylate) ( P M M A ) tensile shear strain-rate (4 • 10-4 sec-1) with super-

and compression specimens were machined out posed hydrostatic pressure. (The material used

of 1 in. (2.54 cm) thick sheets of I C I "Perspex". was identical to that used in the current investiga-

The tensile specimens were approximately4.3 mm tion.)

in diameter with a straight gauge length of 2.5

cm. Compression specimens were circular i ] I I I t l

cylinders with a diameter of 6.4 mm and length YIELD STRESS OF POLYME,rHYLMETHACRYLATE

of 12.8 cm. 1.0 vs LOG~0 (STRAIN-RA,rE!

The poly(ethylene terephthalate) (PET) was

0.9 o COMPRESSION "r=23~

supplied by I C I Plastics Ltd with a thickness of o 9 TENSION T=60*C

approximately 0.64 ram. The optical birefrin-

(18

gence of the material was measured as less than u)

FIT FROM THEORY~

LU

5 • 10-5 and the yield stress in the plane of the 0.7

sheet was found to be isotropic within experi- Q

**mental error. The tensile specimens were dumb-
**

bell shaped with a straight gauge length of 2.5 cm

width 4 mm. ~0.5

z

tll

All tests were performed on an Instron tensile ~0.~

testing machine, inside an environmental cham-

ber within which the temperature could be con- ~0.3

trolled to within -t- 0.5 ~ C both above and below ul

**room temperature. Tensile tests over a wide 0.2
**

range of strain-rates were performed on P M M A

at 60 and 90 ~ C and on P E T at -- 25, 20, 40, 50 0.1

and 60 ~ C. A minimum of 20 rain was allowed 1 I I I [ I I

for each specimen to reach thermal equilibrium. -6 -5 -& -3 -2 -1 0

Compression tests on P M M A were conducted LOG10

at room temperature, both in direct compression Figure I The variation of tensile and compressive yield

between the machine crosshead and a compres- stresses with strain-rate and temperature, P M M A .

910

YIELD OF ISOTROPIC PMMA AND PET

**GRAPH OF TENSILE YIELD STRESS VS LOGlo 4. D i s c u s s i o n
**

( STRAIN" RATE/ sec) The present results confirm, at least for P M MA,

]SOTROPIC PET what is already well established, namely that the

-25~ yield stress of an isotropic polymer depends on

(1) temperature, (2) strain-rate and (3) hydro-

static pressure. It is believed, however, that they

represent the first set of data to link these three

2o~ 3.8q aspects on the same material. Let us discuss first

~ o.' points (l) and (2) above.

The tensile and compressive yield stresses of

o.6 poly(methylmethacrylate) and poly(ethylene

terephthalate) are observed to increase with

6o

~

"-., 3.5~ increasing strain-rate and with decreasing temper-

0.4~ ature. It should be noted that in general the plots

of yield stress versus log (strain-rate) have a small

but definite curvature, indicating that the theory

/" of Eyring [15] in terms of a single simply

~./ 0.2 activated flow process is not applicable to the

/ present data. Our data differ from those of

/ iF 0.1 Bauwens-Crowet et al [16] and Holt [12] in this

| I I I

respect, but are in general agreement with the

-5 -4 -3 -2 -| data of Roetling [l 8 ]. The theory to be described

LOGlo (STRAIN-RATE/ sec ) predicts a definite curvature in this type of plot

Figure 2 The variation of the tensile yield stress of iso- which we therefore consider to be of greater

tropic PET with temperature and strain-rate. generality than the linear behaviour.

Owing to the brittle nature of P M M A , in

tension at room temperature, it was not possible

to obtain direct comparison between tension and

I I I I I I I

compression, but data from other work [1, 2, 14]

TORSION FAILURE UNDER HYDROSTATIC

t

PRESSURE POLYM E TH'~tETHACRYLATE: / clearly indicates that compressive yield stresses

1.5 T=25"C "~=4x10 "4 SEC-1

/

~" would be higher than tensile yield stresses.

/

/ Further, the data from this paper shows the

/

1.4

/

/ greater sensitivity of the compressive yield to

/o strain-rate than the tensile yield.

(,')1.3

n/ //o/ It will be shown that the difference in behaviour

<

o / between tension and compression can be

attributed quantitatively to the dependence of

yield on the hydrostatic component of stress. The

theory is based on that of Robertson [13].

a: 1.(: The tensile behaviour of PET also shows a

o FRACTURE

3: / 9 YIELD slight curvature in the plots of stress versus log

U~ 02

:E

/ FULL LINE BEST FIT strain-rate. Additionally, at the higher tempera-

FROM THEORY

-~ 0.8 tures, the stress was found to decrease more

x

rapidly with decreasing strain-rate than at the

" 02 lower temperatures. This was accompanied by

the formation of tensile crazes before yielding at

0.6 the high temperatures and low strain-rates, i.e.

the normal shear mode of failure was preceded

0.5

by craze formation.

I [ [ I I I I

0.4~ 1 2 3 4 5 6 7 5. T h e o r y

P HYDROSTATIC PRESSURE, KILOBARS

A phenomenological theory of yielding has been

Figure 3 The variation of torsional yield and fracture stress developed from Robertson's theory [13] which

of P M M A with hydrostatic pressure (from [14]). uses the measured dependence of shear yield

911

R. A. D U C K E T T , S. R A B I N O W I T Z , I. M. W A R D

**stress on hydrostatic pressure to predict the work during the activation event and that the
**

observed difference in absolute magnitudes of energy difference should be

tensile and compressive yield stresses, quantita-

tively and also their different sensitivities to

AE -- .rv cos 0 + p D .

temperature and strain rate. Thus whenp is positive (as in a compression test)

Following Robertson, it is assumed that the effective barrier height between the two states

structural elements of the polymer can exist in is increased and when p is negative (as in a

either of two energy states with a difference in tension test) the effective barrier height is

energy of say AE (N.B. this effectively assumes reduced, p(2 represents the work done by the

the planar zigzag model for the polymer chain). hydrostatic component of the applied stress, v

In equilibrium it is proposed that the fraction in and g2 having the dimensions of volume.

each state is given by the Boltzmann distribution. From this point onward we follow the argu-

(The glassy polymer is considered as being ment of Robertson exactly. Because an increase in

quenched in the state it occupied at the glass the fraction of elements in the upper state implies

transition temperature Tg.) Thus before the a tendency towards a structure characteristic of a

application of stress the fraction of elements in higher temperature, and therefore more mobile,

the high energy state is transitions from high to low energy will occur

exp(-- AE/kOg) infinitely more slowly than transitions in the

Xi = [1 + exp(-- AE/kOg)] (1) opposite direction. (This point is discussed at

length by Robertson.) It is therefore possible to

where 0g = Tg if the test temperature T < Tg calculate the maximum fraction of elements in

and0g=TifT> Tg. the upper state averaged over all orientations and

In the isotropic polymer there will be a uni- this can be shown to be:

form distribution of orientation of the structural

kT

elements whether they be segments of the polymer Xmax = 2v--~

chain or small aggregates of chains. The applica-

tion of shear stress ~- will tend to increase the ( i n ( 1 + exp[--(AE--'rv + pY2)/kT]l

fraction of elements in the upper energy state for

elements in some orientations, and decrease it

for other orientations. According to Robertson + k--T-]- -fiT + kT ~ (4)

the shear component of stress ~- changes the E/kO,) \.

energy difference between the two states to 1 + exp(-- AE/kOg)j

AE--~'v cos0. Here -rv cos0 represents the work

done by the shear stress ~-in the transition, and 0 With this fraction of elements in the upper state

is some angle defining the orientation of the the polymer is structurally equivalent to that of

element with respect to the shear stress. the melt at a temperature 01, where

Therefore the fraction of elements in the upper exp(-- AE/k01)

state, with orientation 0 is Xmax = [1 + exp(-- AE/kO0]" (5)

exp[-- (AE -- -rv cos 0 )/kT] Hence a characteristic temperature 01 can be

Xt(O) = {1 + exp[-- (AE -- -rv cos 0 )/kr]} (2) calculated for the polymer under the influence of

Clearly the fraction increases for orientations a shear stress ~- and hydrostatic pressure p. We

such that then compute the effective viscosity of the poly-

mer at the temperature 01 using the W L F

A E -- -rv cos 0 AE equation, and so the resulting strain rate can be

-- 9 (3)

kT kTg shown to be

If the two energy states are associated with the '7"

trans and gauche chain conformations, trans

~Tg

being the lower energy, then an increase in gauche 01

conformations implies a reduction in density due exp--(2"303 [(01 --Tg+C1C2C2) ~ _ C 1 ] } (6)

to less efficient packing. Hence there will be an

interaction with the hydrostatic component of where Ca, C2 are the "universal" W L F para-

the applied stress. We propose, therefore, that meters and ,?g is the universal viscosity of a glass

the hydrostatic component of stress p also does at Tg. Yield is defined as the load when the

912

YIELD OF ISOTROPIC PMMA AND PET

**displacement rate arising from the viscous strain TABLE I Table of coefficients for P M M A
**

rate p just matches the crosshead speed in a

Optimised values Values suggested by

conventional tensile or compression test (i.e. the Robertson

elastic strain-rate is zero and the load to produce

this viscous strain-rate corresponds to the c1 11.1 ~ C 17.44 ~ C

55.9~ C 51.6~ C

observed value of m a x i m u m load), c2

AE 0.88 kcal/mole 1.44 kcal/mole

In addition to the parameters AE, v, Tg, C1, C2 Tg 1050 C 105~ C

and r/g required by the conventional Robertson "qg 10~2poise 1018 -- 10~4-6poise

treatment, the model includes the additional v 109 A3 140/~3

parameter s An approximate relationship o/v 0.175 0

between f2 and v may be obtained from the

results of Rabinowitz et al, [14]. As we have seen

d'c/dp exists for amorphous P E T owing to the

their results show that for P M M A the shear

difficulty of making tubular specimens from thin

yield stress, at constant shear strain rate, is an

sheet material, and so we are forced to estimate

approximately linear increasing function of

a value from several sources. Rabinowitz et al

hydrostatic pressure. Reference to equation 6

[14] and Bowden and Jukes [2] observed that

indicates that over the range of shear stresses

the yield stress of P M M A can be described by

observed by Rabinowitz et al at constant ~7

(0.5 kilobar < "c < 1.1 kilobar) 01 must be "r = "co -}- k P

approximately independent of pressure. Exam-

where k = 0.204 from Rabinowitz (data from

ination of equation 4 indicates that if"cv - - pg2 =

torsion under hydrostatic pressure) and k = 0.175

constant then this condition is satisfied. We

from Bowden and Jukes (data from plane strain

therefore suggest that ~2/v -- (dz/dp)~, and from

compression). The latter technique produced a

fig. 3 take (d'c/dp)~ = 0.2.

value of 0.172 for isotropic amorphous P E T

The data obtained from tension and compres-

(private communication), whereas the former

sion at various strain-rates and temperatures and

yielded k = 0.075 for isotropic crystalline P E T .

the data of Rabinowitz et al were analysed

We therefore choose rather arbitrarily f2/v = O. 1

according to this modified Robertson treatment.

for this amorphous P E T sheet.Treating the other

For the tensile and compression tests "c and p

six coefficients as independent variables the

were taken to be ~/2 and :k ~r/3 respectively,

curves shown in fig. 2 were obtained. A list of

where (r is the axial yield stress ~ is assumed to be

coefficients for P E T is shown in table II. No

equal to half the applied axial strain-rate. The

attempt was made to fit the data in the region of

maximum shear stress on the specimen and

applied hydrostatic pressure were used for "c and

TABLE II Table of coefficients for P E T

p in the torsion tests. The values for AE, v, C1,

C2, ~g, Tg suggested by Robertson, together with Optimised values Values suggested by

= 0.2v do not give an acceptable fit to the data. Robertson

Therefore these values were used as starting cx 15.1 ~ C 17.44~ C

points and all the coefficients were adjusted c2 75.7 ~ C 51.6 ~ C

independently by computer to give a "least AE 1.91 kcals/mole 1.38 kcals/mole

squares fit" using a procedure developed by Tg 90 ~ C 70~ C

Murgatroyd [17]. In the spirit of the Robertson v 234/~ 215 ~8

treatment the shear and hydrostatic components o/v 0.10 0

1014"~poise 1013 -- 10146poise

of stress and temperature were treated as ~g

independent variables, which minimised the

deviations between the predicted and actual rapidly changing stress at 60 ~ C where crazes

shear strain-rates for the tension, compression were observed to precede yield. With regard to

and torsion tests, by adjusting the constants in the values of the coefficients obtained the follow-

the equation independently. The following table ing observations seem relevant; (71 and C~ lie well

(table I) shows the final values obtained for the within the range of values obtained from dyn-

coefficients and those predicted by Robertson amic-mechanical experiments for both P M M A &

for P M M A . These calculated coefficients were and P E T (see for example [19, 20]). The values

used to generate the full curves in figs. 1 and 3. for v, Tg and 9g also compare favourably with

N o such direct data to determine a value for published data. However the values of A E for

913

R. A. D U C K E T T , S. R A B I N O W I T Z . I. M. W A R D

**both P M M A and P E T are in some disagree- The slight disagreement between the data for
**

ment with independent measurements. The only P M M A and the theory may arise in part

comparison for P M M A is with the value because of the use of a crude planar zig-zag

predicted from Tg using the Gibbs-DiMarzio model of the polymer chain and from the

relationship A E = 3.81 Tg cals/mole. It can be approximation used for calculating X maximum.

seen that the value obtained from this investiga- However, we believe that the fit is sufficiently

tion is only about 60 ~ of this prediction. Our good to warrant three tentative conclusions.

value of A E for P M M A should be compared (1) The difference between tensile and com-

with the value of 0.9 kcals/mole for polystyrene, pressive yield stresses for P M M A may be

obtained from ultrasonic measurements [21]. attributed to interaction with the hydrostatic

For P E T we calculate A E = 1.91 kcals/mole. component of stress. N . B . In principle this

This should be compared with the Gibbs- technique should be capable of distinguishing

DiMarzio value of 1.38 kcals/mole. However, between a modified von Mises and a Coulomb

the work of Riveros and Bright Wilson [22] criterion, i.e. between the expressions

using microwave spectroscopy yields a value of A E - - "rv q- P g 2 and d E - - r v - - err.g2' respect-

0.186 4-0.060 kcals/mole for the difference in ively, for the stress-modified energy difference

energy between the rotational isomeric states of between the two states. For the torsion tests

ethyl formate, separated by a barrier height of p = -- er~rand so/2 = g2' to explain the pressure

1.1 :k 0.25 kcals/mole for upward transitions. dependence in torsion correctly. However, for

The value of 0.186 kcals/mole was used by the axial tests erN = zk cr/2 and p ---- 4- or/3, so

Walker and Semlyen [23] for the methyl group d E - - ~-v + p g 2 ~ A E - - -rv - - c~sg2. It is not

rotation, in a calculation which accurately felt, however, that from the present results we can

predicted the measured cyclic trimer concentra- choose unequivocally between these criteria.

tion in the melt of poly(ethylene terephthalate). (2) The general features of the rate dependence

The results would imply that the barriers to of yield stress may be represented in terms of an

conformational changes at yield are higher than effective viscosity, that is pressure, temperature

those measured in the melt. This might be and shear stress dependent.

because the stiffness of the terephthaloyl units is (3) The effective viscosity relates directly to the

more effective in the denser material. low strain relaxation behaviour through the

constants which appear in the W L F equation.

6. C o n c l u s i o n This is at first sight surprising, in view of the fact

A modification of Robertson's molecular theory that yield occurs at much higher levels of stress

of yielding has been presented which allows the and strain than is usual in linear visco-elasticity.

hydrostatic pressure, temperature and rate-

dependence of yield to be discussed within a Acknowledgements

common formalism. Although the details of the One of us (R.A.D.) is grateful for support from

theory are complex the theory is attractive for an S R C Fellowship throughout the course of

several reasons. Firstly because it emphasizes this work, and S.R. was supported by the

that yield is not a unique point on the stress- National Science Foundation.

strain curve, but merely the point at which the

plastic strain-rate produced by the stress just References

matches the machine displacement rate and 1. w. WHITNEYand R. D. ANDREWS,J. Polymer Sei.

secondly, it does not require that a horizontal log C 16 (1967) 2981.

strain-rate shift will produce a yield master curve. 2. P. B. BOWDEN and J. A. JUKES, J. Mater. Sci. 3

Thirdly, it predicts that yield is governed by a (1968) 183.

temperature dependent activation energy (form- 3. S. S T E R N S T E I N , L. O N G C H I N , and A. S I L V E R M A N ,

ally introduced via the W L F equation). It also Applied Polymer Symposia No. 7, p. 175 Interscience

suggests a possible molecular mechanism of yield (1969).

4. yon MISES, See R. Hill "The Mathematical Theory

in polymers. of Plasticity" (Oxford U.P., 1950)p. 20

The accuracy of the fit obtained is very promis- 5. R. HILL, Proc. Roy. Soc. A. 193 (1948) 281.

ing, but clearly it is desirable to find a material 6. N. B R O W N , R. A. D U C K E T T , a n d I. M. W A R D , Phil.

with which it is possible to do tensile and com- Mag. 18 (1968) 483.

pression tests over a wider temperature range 7. c . B R I D L E , A. B U C K L E Y , a n d J . S C A N L A N , J.Mater.

and also torsion tests under hydrostatic pressure. Sci. 3 (1968) 622.

914

JOURNAL OF MATERIALS SCIENCE 5 (1970) 9 LETTERS

**8. J . G . R I D E R a n d E. H A R G R E A V E S , J . Polymer Sci. 18. J. A. ROETLING,Polymer 6 (1965) 311.
**

A2 7 (1969) 829. 19. s. SAITO, KotloidZ. 189 (1963) 116.

9. Y U . S. L A Z U R K I N , ibid30 (1958) 595. 20. J. o. FERRY, "Viscoelastic Properties of Polymers"

10. R. E. ROBERTSON,Jr. Appl. Polymer Sci. 7 (1963) 443. (J. Wiley and Sons, 1970) p. 316.

l l . C. B A U W E N S - C R O W E T , J. V. B A U W E N S , and G. 21. H. J. B A U E R , H . I-IASSLER, M. I M M E N D O R F E R , and

HOMES, J. Polymer Sci. 7 (1969) 735. W . P E C H O L D, u n p u b l i s h e d p r o c e e d i n g s o f c o n f e r e n c e

12. D. L. HOLT, J. Appl. Polymer Sci. 12 (I968) 1653. on "Polymer Chain Flexibility", University of Essex,

13. R. E. ROBERTSON,J. Chem. Phys. 44 (1966) 3950. Janualy, 1970.

14. s. R A B I N O W I T Z , I. M. W A R D , and J. S. C. PARRY, 22. s. M. R I V E R O S a n d E. B R I G H T W I L S O N , J. Chem,

J. Mater. Sci. 5 (1970) 29. Phys. 46 (1967) 4605.

15. H . E Y R I N G , J. Chem. Phys. 4 (1936) 283. 23. G. R. WALKERand s. A. SEMLYEN(in press).

16. J. c. B A U W E N S , C. B A U W E N S - C R O W E T ,

and G.

HOMES, J. Polymer Sci. 7 (1969) 1745. Received 22 July and accepted 28 August 1970

17. P. N. MURGATROYD, Electronics Letters 5 No, 26

(1969).

Letters

A Thermoelectric Method for Measuring electrode a nickel-plated martensitic sewing

Inhomogeneities in Metallic Solid needle was used, whose tip was ground on a

Solutions precision lathe from the original 0.04 to 0.06 m m

radius down to 0.005 to 0.008 ram. Heat was

In the study of many metallurgical phenomena, supplied by focusing the light of a projection

measurements of fine scale solute variations are bulb with condenser (not shown) by means of a

necessary. Generally, the more common methods short-focus convex lens, transparent to infrared,

o f direct analysis which can be applied to very onto a blackened copper target soldered to the

small volumes suffer f r o m low sensitivity, par- needle together with an output copper wire. The

ticularly when the base concentration level of the sample was shielded (against heating and solder

solute to be analysed is small. Fine scale measure- evaporation) from the light target by a thin

ments of mechanical properties (e.g. micro- Teflon sheet. Provided that the bulb power was

hardness) are not directly related only to solute stabilised and air draughts avoided, a uniform

concentIation. probe temperature between 250 and 350~

In connection with a program of non- could be obtained. To avoid conductive heat

equilibrium grain-boundary segregation studies, losses to the hardness tester, the needle was

the use of microscopic electrical point measure- mounted in a holder of machineable ceramic and

ments was reconsidered. There have been the original mount for the hardness indenter was

attempts to measure the local thermoelectric replaced by an acrylic fitting. The moving lever

e m f between a fine point and the specimen sur- of the tester was equilibrated by the auxiliary

face [1, 2], which, however, were not repro- loads and was loaded in the range of 1 to 10 g

ducible enough to obtain a satisfactory calibra- by means of laboratory weights.

tion of emf versus concentration [2]. We present The instrument stage was moved uniformly

here the design of a comparatively simple experi- with the speed of about 0.1 to 1 m m / h by means

ment based on the thermoelectric emf method of a geared timing m o t o r and the micrometric

which provided quite satisfactory results. shift of the tester (not shown). The output

Similarly as in [1, 2] a modified microhardness thermoelectric emf was recorded by the potentio-

tester ( L E I T Z " D u r i m e t " ) was used, but in this metric recorder with 1 mV full scale sensitivity.

case the thermoelectric probe was heated by This low thermoelectric emf represents the

means' of a focused light source (fig. 1). After difference-signal resulting from the individual

insulating the compound stage, the sample was voltages of different joints in the chain and pro-

mounted on a holder and both were fastened by vides enough sensitivity for following slight

Plasticine to the stage, and provided with the thermoelectric emf changes caused by changing

soldered output copper wire. F o r the heated composition of the specimen in the place of the

9 1970 Chapman and Hall Ltd. 915

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