E228-11 (Reapproved 2016)
E228-11 (Reapproved 2016)
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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3. Terminology the derivative of the expansion curve when plotted versus
3.1 Definitions—The following terms are applicable to this temperature, at the temperature T. It has a rather limited utility
test method and are listed in Terminologies E473 and E1142: for engineering applications, and therefore it is more common
coeffıcient of linear thermal expansion, thermodilatometry, and to use the average coefficient of thermal expansion, than the
thermomechanical analysis. instantaneous one.
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5.3 For accurate determinations of thermal expansion, it is the sample holder and the push-rod(s) shall be made of the
absolutely necessary that the dilatometer be calibrated by using same material, having been proven to exhibit thermal expan-
a reference material that has a known and reproducible thermal sion characteristics within 61 % of each other. Illustrations of
expansion. The appendix contains information relating to typical tube and rod-type configurations are given in Fig. 1. It
reference materials in current general use. is often practiced to configure specimen holders that are not
5.4 The measurement of thermal expansion involves two shaped as a tube, but serve the same structural purpose. This is
parameters: change of length and change of temperature, both an acceptable practice, as long as the shape is mechanically
of them equally important. Neglecting proper and accurate stable and is not prone to reversible configurational changes
temperature measurement will inevitably result in increased (such as twisting, etc.) upon heating and cooling.
uncertainties in the final data. NOTE 2—The tube and the push-rod beyond the specimen, while
parallel to each other, are expected to have identical thermal gradients
5.5 The test method can be used for research, development, along them, thereby identical thermal expansion. This is a critical factor,
specification acceptance, quality control (QC) and quality as differences in net expansion between the tube and the push-rod will
assurance (QA). appear very much like expansion produced by the specimen. To a limited
extent, calibration (see Section 9) can be used to account for these
6. Interferences differences in the thermal expansion of the two parts, however, it is noted
that this is one of the most fundamental of all practical limitations for
6.1 Materials Considerations:
dilatometers. To minimize this effect, the tube and the push-rod shall be in
6.1.1 The materials of construction may have substantial close proximity of each other and heated slowly enough to prevent
impact on the performance of the dilatometer. It is imperative substantial thermal gradients that occur radially.
that regardless of the materials used, steps be taken to ascertain 7.1.2 Test Chamber, composed of:
that the expansion behavior is stabilized, so that repeated 7.1.2.1 Furnace, Cryostat, or Bath, used for heating or
thermal cycling (within the operating range of the device) cooling the specimen uniformly at a controlled rate over the
causes no measurable change. temperature range of interest, and able to maintain the tem-
6.2 General Considerations: perature uniform along the sample during its heating, cooling,
6.2.1 Inelastic creep of a specimen at elevated temperatures or just equilibrating.
can often be prevented by making its cross section sufficiently
NOTE 3—Extreme care must be exercised in using furnaces for high
large. temperatures, to prevent interaction with the dilatometer’s parts or with
6.2.2 Avoid moisture in the dilatometer, especially when the specimen. In many instances, it is necessary to protect the specimen
used at cryogenic temperatures. and the dilatometer from oxidation and in some cases this may be
6.2.3 Means to separate the bath from the specimen are accomplished with the use of a muffle tube. If it is necessary, the furnace,
in such cases, shall contain provisions to provide inert atmosphere or
required when the dilatometer is immersed in a liquid bath. vacuum environment, as well as provisions to protect against air back-
6.2.4 Support or hold the specimen in a position so that it is streaming on cooling.
stable during the test without unduly restricting its free NOTE 4—Unless it is absolutely necessary to have the specimen tested
movement. in vacuum, measurements of thermal expansion in vacuum are not
6.2.5 The specimen holder and push-rod shall be made from recommended due to extreme thermal gradients, thermal lags, etc.
between various components of the dilatometer and the specimen, that are
the same material. The user must not practice uncontrolled caused by the very poor heat transfer that occurs in the absence of a gas.
substitutions (such as when replacing broken parts), as serious
increase of the uncertainties in the measured expansion may 7.1.2.2 Temperature Controller (or circuitry with equivalent
result. function) capable of executing a specific temperature program
6.2.6 A general verification of a dilatometer is a test run by operating the furnace(s) between selected temperature limits
using a specimen cut from the same material as the push rod at rates programmed, and supported by the furnace(s)’s thermal
and specimen holder. The resultant mean coefficient of linear performance. Temperature control of a constant rate shall be
thermal expansion should be smaller than 60.3 µm/(m·°C) for
a properly constructed system (after applying the system’s
correction).
6.2.7 Conditioning of specimens is often necessary before
reproducible expansion data can be obtained. For example,
heat treatments are frequently necessary to eliminate certain
effects (stress caused by machining, moisture, etc.) that may
introduce irreversible length changes that are not associated
with thermal expansion.
7. Apparatus
7.1 Push-Rod Dilatometer System, consisting of the follow-
ing:
7.1.1 Specimen Holder—A structure of thermally stable
material constructed in a fashion such that when a specimen of
the same material is placed into it for a test, the qualifications
given in 6.2.7 are satisfied. In any push rod dilatometer, both FIG. 1 Common Forms Specimen Holders
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may be, but are not limited to, thermocouples, pyrometers,
resistance thermometers, thermistors, mercury thermometers,
etc.
7.1.4.2 Manual, Electronic, or Equivalent Readout, such
that the indicated temperature can be determined without
additional degradation to the sensor’s performance.
NOTE 5—In all cases in which thermocouples are used, they shall be
referenced to 0°C by means of an ice water bath or equivalent electronic
reference.
NOTE 6—Special attention must be paid to prevent contamination of the
thermocouple by the specimen or even by the dilatometer tube itself (for
example, type C thermocouple in a graphitic environment). Interaction
between atmosphere and the thermocouple (for example, type S thermo-
couple in hydrogen atmosphere) can also be extremely detrimental.
NOTE 7—Placement of thermocouples is important, and the user is
frequently given a choice. It is often a practice to bring the bead of a
FIG. 2 Suggested Shapes of Specimen’s and Push-Rod Ends thermocouple in contact with the specimen, or even embed it in a hole, as
opposed to having it laying on top of it or in its proximity. While the
former seems better, it is actually sometimes the cause of mechanical
monotonous within 62°C (exclusive of the approximately 5 % interference with the specimen, source of contamination, and while it
of instrument’s maximum temperature of its operating range). registers a more true specimen temperature, it neglects the temperature of
The control of equilibrium temperatures shall be within 61°C the specimen holder around it. A good practice is to have the bead of the
or 60.05 % of maximum temperature of the dilatometer’s thermocouple reside equidistant between the specimen holder and the
operating range, whichever is larger. specimen itself, ensuring that it is shielded from direct view of the heater
or muffle tube (if one is employed).
7.1.2.3 Means to cool furnace(s) or cryostat for operation NOTE 8—The thermocouple positioning during the test should be the
below ambient. same as was used in the instrument’s calibration. Frequent verification of
7.1.2.4 Means to seal the space occupied by the dilatometer, thermocouple performance is highly recommended.
contain pressurized gas, or evacuated, without collapse or 7.2 Measuring Tool, such as a vernier micrometer or cali-
gradual deformation with time and temperature, or without pers capable of reading to at least 625 µm in order to
bursting when pressure is applied within specified limits. determine the initial and final lengths of the test specimen.
7.1.3 Transducer—A device to convert and magnify the
minute mechanical translation conveyed by the push-rod(s) 8. Test Specimens
resulting from the expansion of the specimen, into visually
discernable or electrically measurable signals, with a constant 8.1 The specimen length shall be such that the accuracy of
and defined functionality. determining ∆L/L0 is at least 620 µm/m. Where possible, the
7.1.3.1 Visually readable devices, such as dial gauges, specimen should be between 25 and 60 mm long and between
optical levers, rulers, etc. 5 and 10 mm in diameter (or equivalent, if not cylindrical),
7.1.3.2 Electromechanical devices with a defined electrical however, there is no fundamental limitation on either
output corresponding to a defined mechanical displacement dimension, as long as the dilatometer can accommodate the
input. Examples of these are: linear variable differential specimen with a maximum thermal gradient of 2°C, either
transformers, digital absolute or incremental encoders, capaci- determined in 50 mm intervals over the entire specimen, or
tive sensors, optical displacement sensors, etc. maintained uniformly within 62°C/50 mm.
7.1.3.3 The transducer must be selected such as to cover the 8.2 The cross sectional shape of the specimen, the cross
expected displacement within its linear range. sectional uniformity along its length, or the condition of the
7.1.3.4 Transducers employed in dilatometry must have a surface along its length, have no bearing on the test. The ends,
resolution (visible or sensible) of not less than 0.1 % of their however, must be smooth and parallel. The cross section must
linear range, with an attendant proven linearity of at least be robust enough to prevent buckling or creep.
60.1 % of their range. 8.2.1 In the instances when limitations of the source mate-
7.1.3.5 The linearity band of a transducer limits the maxi- rial precludes the forming of a cylinder or slab, irregular
mum resolution that can be assigned to the dilatometer. (Since shaped samples may be tested. However, care must be exer-
the band bound by linearity is considered unresolvable, even cised not to have the sample form a point contact with the
with special calibrations, resolution cannot be ensured much dilatometer, as it may lead to deformations during the test.
beyond the transducer’s range of linearity.) Adding empty 8.2.2 Thin sheets of materials can be formed into a speci-
amplification (extra digits to the readout), may give the men by being rolled into a tube or bent into a “V” shaped piece
impression of more sensitivity, but in reality it does not. for increased stiffness.
Nonlinearity errors cannot be effectively accounted for with 8.2.3 Smaller pieces may be stacked to obtain a longer
calibration. specimen, often without any cementing, as long as all inter-
7.1.4 Temperature Measurement System, consisting of: faces are kept flat and parallel, and no wobble is observable
7.1.4.1 Calibrated Sensor or Sensors, to provide indication when the push-rod is raised and lowered to contact it.
of the specimen temperature 60.5°C, or 61 % of the overall 8.2.4 Hollow (tube) or irregular shaped specimens often
temperature range, whichever is larger. Temperature sensors require the use of a cover plate between them and the push-rod
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for well defined contact. Such plate is preferred to be made out 9.4.1.4 Observe the direction of progress as to heating or
of the same material as the dilatometer, to neglect its contri- cooling, as they cause different thermal lags. Using a calibra-
bution in the calculations. Alternately, a very thin sheet of a tion function obtained on heating for a test involving cooling
stiff material, other than the dilatometer’s, may be used, but will inevitably bring in differences.
with proper accounting for its contribution. 9.4.1.5 Reliance on statistically averaged multiple (repli-
8.2.5 Specimens of semi-rigid materials that would deform cate) calibration runs is recommended for each heating sched-
when in contact with the tip of the push-rod can be successfully ule.
tested according to 8.2.4, aimed at reducing the pressure on the 9.4.2 Because a dilatometer always indicates the difference
specimen (counterweights, etc.), provided the material is able in expansion between the specimen and the portion of the tube
to maintain its shape otherwise. This is an extension of the that is positioned parallel to it, a calibration constant, ATi
method and care must be exercised when practiced. (defined in Eq 4), has to be determined at each temperature
interval between Ti and T0, with T0 < Ti < T. The calibration
9. Calibration constants determined through Eq 4 can be used as either
9.1 Calibrate the transducer by imposing a series of known point-by-point corrections at discrete temperatures, or can be
displacements with a precision screw micrometer, gauge converted into a function and used to correct data expressed as
blocks, or any other device that is more accurate than the expansion versus temperature.
transducer that is being calibrated. This step may be omitted for
absolute transducers.
NOTE 9—Any transducer system, however, including digital encoders,
A Ti 5 FS D S D G
∆L
L0 t
2
∆L
L0 m Ti
(4)
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distribution. The extent to which radial gradients exist is determined by starting from a common reference temperature (20°C, by
the characteristics of the specimen. Users must select heating rates and/or convention) to T. Clearly indicate if other reference tempera-
equilibration (soak) times prudently, to ensure that no lag occurs and that
data truly represents that for the whole specimen at a uniform temperature.
ture was used.
A good practice is to test large samples in stepwise fashion and monitor 12.1.8 Complete description of any unusual behavior of the
the approach to a constant value of the expansion as an indication of specimen, such as a permanent change in specimen length at
thermal equilibrium. the reference temperature following testing, excessive
10.7 A retest should be considered if the length of the oxidation, scaling, discoloration, deformation, cracking,
specimen at the end of the test differs from that at the beginning spalling, etc., all of which may be of value in interpreting the
by more than 20 µm/m. Alternately, this permanent deforma- test results; and
tion should be taken into account when reporting the expansion 12.1.9 Any additional information required by a particular
values. This retest, however, is not relevant for tests involving material specification.
sintering, softening point determinations, etc., where perma- 12.1.10 Specify the dated version of this method, used for
nent deformation is part of the expected behavior. performing the measurements.
F G FS D G
∆L
L0 Ti
5
∆L
L0 m
1A
Ti
(5)
relative length.
13.1.1 Random error is usually associated with the precision
11.2 Using the calculated values of the linear thermal and bias of repeated length and temperature measurements, but
expansion, calculate the mean coefficients of thermal expan- other variables may also intrude on the measurements. For
sion by dividing the thermal expansion values by the appro- instance, a specimen may change position or the voltage
priate temperature range ∆T = Ti – T0. applied to the measurement transducer may fluctuate.
13.1.2 Systematic error is usually larger and can result from
F 1 ∆L
@ α m # Ti 5 ∆T · L
0
G Ti
(6) many sources. These include the following: accuracy of the
length and temperature measurements; deviation of the speci-
11.3 Instantaneous coefficients of thermal expansion may be men mean temperature from that indicated by the sensor;
determined graphically by laying a tangent to the ∆L/L0 curve deviation from linearity of the transducer; temperature gradi-
at the desired temperature points, or by differentiating a ents between the dilatometer tube and push-rod. Little can be
function fit to the data, at the desired points. done to improve the random errors, once the transducer and
11.4 In calculation of the relevant quantities, carry all temperature sensor have been selected, except to follow good
available decimal places for each input parameter measured to experimental practice. However, systematic errors can be
its actual level of precision through to the final result (but not reduced by careful calibration of the individual components
beyond), and report the data to three significant figures. and the total system.
13.2 Repeated measurements on many different materials
12. Report have confirmed that the precision with which linear thermal
12.1 Report the following information: expansion, ∆L/L0, is measured with a vitreous silica dilatom-
12.1.1 Description of the material, manufacturer, chemical eter can be estimated from the precision of the length and
composition (if known), thermal and mechanical history; temperature measurements. This estimate is determined from
12.1.2 Method of test specimen preparation, and axis the following:
orientation, if material is anisotropic, together with details of
any subsequent thermal, mechanical, moisture, or other condi- δ S D
∆L
L0
2
5 6 @ ~ δE ! 2 1 ~ α T L 0 δT ! 2 # 1/2
L0
(7)
tioning;
12.1.3 Form and dimensions of the test specimen, including where:
initial length, L0, and reference temperature, T0; δE and δT = precisions of the single measurements of length
12.1.4 Brief description of the apparatus, including dis- and temperature.
placement and temperature measuring systems, estimation of 13.2.1 The error in measuring L0 is usually so small that it
precision, heating and cooling rates, temperature controls and does not contribute to this estimate. For example:
atmosphere;
12.1.5 Listing of the reference material(s) and procedure L 0 5 0.1 m, δE 5 61 µm, d T 5 20 µm ⁄ ~ m · °C! and δT 5 60.5°C
used to calibrate the dilatometer system, including the trans- 13.2.2 The precision in determining (∆L/L0) is estimated to
ducer and temperature sensor; be as follows:
12.1.6 Tabulation of the data, showing linear thermal
expansion, test temperatures and values for mean coefficients
of linear thermal expansion for selected temperature intervals;
δ S D
∆L
L0
56
2
0.1
@ ~ 1 ! 2 1 ~ 20·0.1·0.5! 2 # 1/2 5 28 µm/m (8)
12.1.7 Curves plotted as: ∆L/L0 versus T, αm versus T, αt 13.2.3 It has been shown that the maximum difference to be
versus T, where: αm is computed for the temperature range expected from repeated tests is estimated by the following:
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δ S D
∆L
L0 max
56
2
L0
~ δE1α T L 0 δ T ! (9)
temperatures, it is estimated that precision and bias similar in
magnitude exist for those instruments at least up to 2000°C.
13.3 Tests of linear thermal expansion of borosilicate glass, 13.5 An interlaboratory test will be conducted for determin-
copper and tungsten over the range of 25°C to 400°C have ing the repeatability and reproducibility of this test method.
indicated that a vitreous silica dilatometer can be accurate to
4 % when carefully calibrated. This corresponds to a precision 14. Keywords
of approximately 0.8 % as calculated from the example in 13.2. 14.1 contraction; dilatometer; dilatometry; expansion; ex-
13.4 Based on identical operating principle and similar pansivity; linear thermal expansion; mean coefficient of ther-
observations using alumina and graphite dilatometers at higher mal expansion; push-rod
APPENDIX
(Nonmandatory Information)
X1.1 In the absence of certified standards, usual industry large volume of published data in the literature (or generally
accepted practice is to use secondary references. In this group respected reference works) indicating expected performance
there are two levels: first, material specimens that are some- within certain limits. While references are listed for all such
times available with data that are traceable to NIST (they were suggestions, it is incumbent upon the user to sort out whether
tested on instruments calibrated with NIST Certified SRM), the references are convincing, or which among deferring
and secondly, generic, but well characterized materials with a datasets are more persuasive.
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TABLE X1.1 Thermal Expansion of Various Standard Reference Materials
SRM 731 (Borosilicate Glass)A SRM 738 (Stainless Steel)A SRM 739 (Fused Silica)A
Temperature Expansion Expansivity Expansion Expansivity Expansion Expansivity
(K) ∆L/L293 α ∆L/L293 α ∆L/L293 α
(µm/m) (10-6 K-1) (µm/m) (10-6 K-1) (µm/m) (10-6 K-1)
80 –819 ... ... ... –1 –0.07
100 –771 2.64 ... ... –13 –0.53
120 –714 3.07 ... ... –22.5 –0.38
140 –649 3.43 ... ... –28.5 –0.24
160 –578 3.72 ... ... –32 –0.10
180 –501 3.97 ... ... –32.5 0.02
200 –419 4.17 ... ... –31 0.13
220 –334 4.34 ... ... –27.5 0.23
240 –246 4.48 ... ... –22 0.32
260 –155 4.60 ... ... –14 0.39
280 –62 4.71 ... ... –6 0.45
293 0 4.78 0 9.76 0 0.48
300 34 4.82 69 9.81 ... ...
320 131 4.91 ... ... 13.5 0.53
340 230 4.99 466 10.04 24.5 0.56
380 432 5.11 872 10.28 47.5 0.60
420 638 5.19 1288 10.52 72 0.62
460 847 5.23 1714 10.76 97 0.63
500 1057 5.26 2149 11.00 122 0.63
540 1267 5.27 2593 11.23 ... ...
560 1372 5.27 ... ... 159 0.61
580 1478 5.27 3048 11.47 ... ...
600 1583 5.27 ... ... 183 0.59
620 1689 5.28 3511 11.71 ... ...
640 1794 5.29 ... ... 206 0.56
660 1900 ... 3984 11.95 ... ...
680 2007 ... ... ... 228 0.54
700 ... ... 4467 12.19 ... ...
720 ... ... ... ... 249 0.51
740 ... ... 4959 12.42 ... ...
760 ... ... ... ... 269 0.49
780 ... ... 5461 12.66 ... ...
800 ... ... ... ... 228 0.47
840 ... ... ... ... 307 0.44
880 ... ... ... ... 324 0.42
920 ... ... ... ... 340 0.40
960 ... ... ... ... 356 0.38
1000 ... ... ... ... 371 0.37
A
Limited or exhausted availability from NIST, Gaithersburg MD, USA. Values in table are from relevant certificate for the reference material. Certificate values are not
representative of generic materials of similar description.
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TABLE X1.3 Linear Thermal Expansion of Industry Accepted
Materials: Lucalox,A Thermographite
LucaloxB,C ThermographiteB,C
Temperature Expansion Expansion
(°C) ∆ L/L20 ∆L/L20
(µm/m) (µm/m)
100 { 402
200 { 1031
300 { 1667
400 { 2313
500 3570 2971
600 4440 3643
700 5340 4332
800 6260 5040
900 7200 5766
1000 8160 6513
1100 9130 7270
1200 10120 8069
1300 11130 8878
1400 12160 9707
1500 13200 10555
1600 14270 11422
1700 { 12304
1800 { 13201
1900 { 14111
2000 { 15029
2100 { 15954
2200 { 16882
2300 { 17810
2400 { 18732
2500 { 19645
2600 { 20544
2700 { 21425
2800 { 22280
A
Lucalox is a product and trademark of General Electric Company, Cleveland,
OH.
B
Available from commercial sources. Tabulated values are from cited references.
C
See Refs (9, 10).
REFERENCES
(1) Hahn, T.A., and Kirby, R.K., “Thermal Expansion of Platinum 293 to Cryogenic Laboratory Report OSU-TR-264-27, 1954.
1900 K,” AIP Conference Proceedings, No. 3, 1972. (8) Hidnert, P., and Krider, H.S., “Thermal Expansion Measurements,”
(2) Nix, F.C., and MacNair, D., “Thermal Expansion of Pure Metals,” Journal of Research National Bureau of Standards, Vol 48, 1952, p.
Physical Review, Vol 61, 1942, p. 74. 209.
(3) White, G.K., “Expansion Coefficients of Coppers at 283K and (9) Apostolescu, D.E., Gaal, P.S., and Chapman, A. S., “A Proposed High
Oxygen Atmospheres,” Journal of Physics, Vol 26, 1972, p. 30. Temperature Thermal Expansion Reference Material,” Proceedings of
(4) Nix, F.C., and MacNair, D., “Thermal Expansion of Pure Metals,” the 24th International Thermal Conductivity Conference / 12th
Physical Review, Vol 60, 1941, p. 597. International Thermal Expansion Symposium, P.S. Gaal, D.E. Apos-
(5) Simmons, R.D., and Bullutfi, R.W., “Measurements of Equilibrium tolescu eds., 1999, p. 637.
Vacancy Concentrations in Aluminum,” Physical Review, Vol 117, (10) Stroe, D.E., Hebrank, T.R., and Jacobs R.A., “Linear Thermal
1960, p. 52. Expansion of a Very Fine Grain Graphite,” Proceedings of the
(6) Fraser, D.B., and Hollis-Hallet, A.C., Proceedings of the 7th Interna- International Thermal Conductivity 26 / 14th International Thermal
tional Conference on Low Temperature Physics, 1961, p. 689. Expansion Symposium, R. Dinwiddie ed., 2005, p. 510.
(7) Altman, H.W., Rubin, T., and Johnson, H.L., “Coefficients of Thermal (11) Omega Engineering Complete Temperature Measurement Handbook
Expansion of Solids at Low Temperatures,” Ohio State University and Encyclopedia.
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