ASTM D116-86(1999)
(Test Method)Standard Test Methods for Vitrified Ceramic Materials for Electrical Applications
Standard Test Methods for Vitrified Ceramic Materials for Electrical Applications
SCOPE
1.1 These test methods outline procedures for testing samples of vitrified ceramic materials that are to be used as electrical insulation. Where specified limits are mentioned herein, they shall not be interpreted as specification limits for completed insulators.
1.2 These test methods are intended to apply to unglazed specimens, but they may be equally suited for testing glazed specimens. The report section shall indicate whether glazed or unglazed specimens were tested.
1.3 The test methods appear as follows: Procedure Section Compressive strength 6 C 773 Dielectric strength 13 D 618, D 149 Elastic properties 8 C 623 Electrical resistivity 15 D 618, D 257, D 1829 Flexural strength 7 C 674, F 417 Hardness 9 C 730, E 18 Porosity 5 C 373 Relative permittivity and dissipation factor 14 D 150, D 2149, D 2520 Specific gravity 4 C 20, C 329, F 77 Thermal conductivity 10 C 177, C 408 Thermal expansion 12 C 539, E 228 Thermal shock resistance 11
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precaution statements are given in 11.3, 13.5, and 15.3.
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Designation: D 116 – 86 (Reapproved 1999)
Standard Test Methods for
Vitrified Ceramic Materials for Electrical Applications
This standard is issued under the fixed designation D116; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope C177 Test Method for Steady-State Heat-Flux Measure-
ments and Thermal Transmission Properties by Means of
1.1 These test methods outline procedures for testing
the Guarded Hot Plate Apparatus
samples of vitrified ceramic materials that are to be used as
C329 Test Method for Specific Gravity of Fired Ceramic
electrical insulation. Where specified limits are mentioned
Whiteware Materials
herein, they shall not be interpreted as specification limits for
C373 Test Method for Water Absorption, Bulk Density,
completed insulators.
Apparent Porosity, andApparent Specific Gravity of Fired
1.2 These test methods are intended to apply to unglazed
Whiteware Products
specimens, but they may be equally suited for testing glazed
C408 Test Method forThermal Conductivity ofWhiteware
specimens. The report section shall indicate whether glazed or
Ceramics
unglazed specimens were tested.
C539 Test Method for Linear Thermal Expansion of Por-
1.3 The test methods appear as follows:
celain Enamel and Glaze Frits and Ceramic Whiteware
Procedure Section
Materials by the Interferometric Method
Compressive strength 6 C 773
C623 Test Method for Young’s Modulus, Shear Modulus,
Dielectric strength 13 D 618, D 149
and Poisson’s Ratio for Glass and Glass-Ceramics by
Elastic properties 8 C 623
Resonance
Electrical resistivity 15 D 618, D 257, D 1829
Flexural strength 7 C 674, F 417
C674 Test Methods for Flexural Properties of Ceramic
Hardness 9 C 730, E 18
Whiteware Materials
Porosity 5 C 373
Relative permittivity and dissipation factor 14 D 150, D 2149, D 2520 C730 Test Method for Knoop Indentation Hardness of
Specific gravity 4 C 20, C 329, F 77
Glass
Thermal conductivity 10 C 177, C 408
C773 Test Method for Compressive (Crushing) Strength of
Thermal expansion 12 C 539, E 228
Thermal shock resistance 11 Fired Whiteware Materials
D149 Test Method for Dielectric Breakdown Voltage and
1.4 This standard does not purport to address all of the
Dielectric Strength of Electrical Insulating Materials at
safety concerns, if any, associated with its use. It is the
Commercial Power Frequencies
responsibility of the user of this standard to establish appro-
D150 Test Methods for A-C Loss Characteristics and
priate safety and health practices and determine the applica-
Permittivity (Dielectric Constant) of Solid Electrical Insu-
bility of regulatory limitations prior to use.Specificprecaution
lation
statements are given in 11.3, 13.5, and 15.3.
D257 Test Methods for D-C Resistance or Conductance of
Insulating Materials
2. Referenced Documents
D618 Practice for Conditioning Plastics for Testing
2.1 ASTM Standards:
D638 Test Method for Tensile Properties of Plastics
C20 Test Methods for Apparent Porosity, Water Absorp-
D1829 Test Method for Electrical Resistance of Ceramic
tion, Apparent Specific Gravity, and Bulk Density of
2 Materials at Elevated Temperatures
Burned Refractory Brick and Shapes by Boiling Water
D2149 Test Method for Permittivity (Dielectric Constant)
These test methods are under the jurisdiction of ASTM Committee C-21 on
Ceramic Whitewares and Related Products and is the direct responsibility of Annual Book of ASTM Standards, Vol 04.06.
Subcommittee C21.03 on Test Methods for Whiteware Properties. Annual Book of ASTM Standards, Vol 15.02.
Current edition approved Oct. 31, 1986. Published December 1986. Originally Annual Book of ASTM Standards, Vol 02.05.
e1 6
published as D116 – 21 T. Last previous edition D116 – 86 (1994) . Annual Book of ASTM Standards, Vol 10.01.
2 7
Annual Book of ASTM Standards, Vol 15.01. Annual Book of ASTM Standards, Vol 08.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D116
of Solid Dielectrics at Frequencies to 10 MHz and Tem- 5.3.2 An alternative to MethodA, using gas as a fluid, may
6 11,12
peratures to 500°C be found in the literature.
D2520 Test Methods for Complex Permittivity (Dielectric 5.4 Method B—Dye Penetration Under Pressure:
Constant) of Solid Electrical Insulating Materials at Mi- 5.4.1 Apparatus—The apparatus shall consist of a suitable
crowave Frequencies and Temperatures to 1650°C pressure chamber of such dimensions as to accommodate the
E18 Test Methods for Rockwell Hardness and Rockwell testspecimenwhenimmersedinthedyesolutionwitharrange-
Superficial Hardness of Metallic Materials ments for obtaining and maintaining the required pressure for
E228 Test Method for Linear Thermal Expansion of Solid the required time.
Materials with a Vitreous Silica Dilatometer 5.4.2 Reagent—Afuchsinedyesolutionconsistingof1gof
F77 Test Method for Apparent Density of Ceramics for basic fuchsine in 1 Lof 50% reagent ethyl alcohol is suitable.
Electron Device and Semiconductor Application 5.4.3 Specimens—The specimens shall be freshly broken
F417 Test Method for Flexural Strength (Modulus of Rup- fragments of the ceramic body, having clean and apparently
ture) of Electronic-Grade Ceramics unshatteredsurfacesexposed.Atleast75%oftheareaofsuch
specimens should be free of glaze or other surface treatment.
3. Significance and Use
Fragments approximately 5 mm in the smallest dimension up
3.1 For any given ceramic composition, one or more of the to 20 mm in the largest dimensions are recommended.
properties covered herein may be of more importance for a 5.4.4 Procedure:
given insulating application than the other properties. Thus, it 5.4.4.1 Place the specimen fragments in the pressure cham-
may be appropriate that selected properties be specified for ber and immerse completely in the fuchsine solution.
testing these ceramic materials. 5.4.4.2 Apply a pressure of 28 MPa (4000 psi) 6 10% for
3.2 Pertinent statements of the significance of individual
approximately 15 h. An optional pressure of 70 MPa (10000
properties may be found in the sections pertaining to such psi) 6 10% for 6 h may be used.
properties.
5.4.4.3 At the conclusion of the application of the test
pressure, remove the specimens from the pressure chamber,
4. Specific Gravity
rinse and dry thoroughly, and break as soon as possible for
4.1 Scope—Three methods are given, providing for accu- visual examination.
racy, convenience, or testing of small specimens. 5.4.4.4 Porosity is indicated by penetration of the dye into
4.2 Significance and Use—Specific gravity measurements the ceramic body to an extent visible to the unaided eye.
provide data indicating the control of quality of the ceramic Disregardanypenetrationintosmallfissuresformedinprepar-
material.The thermal maturity of specimens may be estimated ing the test specimen.
from such data. Specific gravity data are related to electrical, 5.4.5 Report—The report shall include a statement of the
thermal, and mechanical properties of ceramics. observations recorded in accordance with the examination in
4.3 Procedure: 5.4.4.4.
4.3.1 Whenthedestructionofthespecimencanbetolerated 5.4.6 Precision and Bias—This method has been in use for
and the highest precision is required, determine the specific
many years, but no statement for precision has been made and
gravity in accordance with Test Method C329. no activity is planned to develop such a statement.Astatement
4.3.2 When it is not desirable to destroy the specimen and
ofbiasisunavailableinviewofthelackofastandardreference
less precise values are acceptable, determine the specific material for this property.
gravity in accordance with Test Methods C20.
5.5 Method C—Dye Penetration Under Atmospheric Pres-
4.3.3 When only a very small specimen is available, deter- sure:
minethespecificgravityinaccordancewithTestMethodF77.
5.5.1 Apparatus—The apparatus shall consist of a suitable
open-air chamber of such dimensions as to accommodate the
5. Porosity
test specimens when immersed in the dye solution.
5.1 Scope—Three methods are given based on the relative 5.5.2 Reagent—The fuchsine solution of 5.4.2 is suitable.
porosity of the specimens. 5.5.3 Specimens—The specimens of 5.4.3 are suitable.
5.2 Significance—Amountofporosityofaspecimenisused
5.5.4 Procedure:
as a check on structural reproducibility and integrity. 5.5.4.1 Place the test specimens in the chamber and im-
5.3 Method A:
merse completely in the fuchsine solution.
5.3.1 In the case of relatively porous ceramics (water 5.5.4.2 Permit the specimens to remain immersed for 5 min
absorptiongreaterthan0.1%),determinetheporosityaswater
or longer, remove, rinse, dry thoroughly and break as soon as
absorption in accordance with Test Method C373. possible for visual examination.
NOTE 1—Test Method C373 has been found suitable for determining
water absorption in the range of 0.1%, although that method was derived
specifically for absorptions exceeding 3.0%.
Wasburn, E. W. and Bunting, E. N., “The Determination of the Porosity of
HighlyVitrifiedBodies,” Journal of the American Ceramic Society,Vol5,1922,pp.
527–535.
8 12
Annual Book of ASTM Standards, Vol 10.02. Navias,Louis,“MetalPorosimeterforDeterminingthePoreVolumeofHighly
Annual Book of ASTM Standards, Vol 03.01. Vitrified Ware,” Journal of the American Ceramic Society, Vol 8, 1925, pp.
Annual Book of ASTM Standards, Vol 14.02. 816–821.
D116
5.5.4.3 Porosity is indicated by penetration into the ceramic 9. Hardness
body to an extent visible with the unaided eye. Disregard any
9.1 Scope—Two methods are given. Method A requires
penetration into small fissure formed in the preparation of the
little in the way of specimen preparation and has a limited
specimens.
capability of differentiating between samples. Method B re-
5.5.5 Report—The report shall include a statement of the
quires preparation of a polished section of the specimen and
observations recorded in accordance with the examination in
has an extended limit of differentiation between samples.
5.5.4.3.
9.2 Significance and Use—Hardness can be used as an
5.5.6 Precision and Bias—This method has been in use for
easilyobtainedindicatorofthethermalmaturityofaspecimen,
many years, but no statement for precision has been made and
particularly when used in conjunction with the specimen
no activity is planned to develop such a statement.Astatement
specific gravity.
ofbiasisunavailableinviewofthelackofastandardreference
9.3 Procedure:
material for this property.
9.3.1 Method A—Determine the Rockwell superficial hard-
ness in accordance with Test Methods E18. Use the Type N
6. Compressive Strength
Scale and a 45-kg major load.
6.1 Scope—Thesemethodsprovideforthedeterminationof
9.3.2 Method B—Determine the Knoop hardness in accor-
the compressive (crushing) strengths of the full range of
dance with Test Method C730. Use a polished surface and a
ceramics from relatively weak to the very strongest.
1-kg load.
6.2 Significance and Use—Since many ceramic insulators
are subjected to compressive stresses, knowledge of this
10. Thermal Conductivity
property is important. The test yields data that are useful for
10.1 Scope—Therecommendedproceduresallowthedeter-
purposesofdesign,specification,qualitycontrol,research,and
minationofthethermalconductivityofceramicmaterialsfrom
in the comparison of ceramic materials.
40 to 150°C (100 to 300°F).
6.3 Procedure—Determine compressive strength in accor-
10.2 Significance—A ceramic insulator may be subjected
dance with Test Method C773.
frequentlytothermalshockorrequiredtodissipateheatenergy
from electrically energized devices. Thermal conductivity
7. Flexural Strength
characteristics are useful in designing ceramic insulators for
7.1 Scope:
service, research, quality control, and comparison of ceramic
compositions.
7.1.1 This test method includes two procedures: for testing
a material for characterization purposes and for testing the
10.3 Procedure—Determine the thermal conductivity in
material constituting the finished ware. accordance with Test Method C408.
7.1.2 For the characterization of ceramic compositions,
NOTE 2—If thermal conductivity values over a broader temperature
when relatively large specimens may be easily produced,
range of a lower order of magnitude than those obtainable using Test
Method A is recommended. Method B is acceptable.
Method C408 are required, Test Method C177 may be used.
7.1.3 When specimens must be cut from a fired sample
Method B is recommended. 11. Thermal Shock Resistance
7.2 Significance and Use—Flexural strength correlates with
11.1 Scope—These thermal shock tests may be used for the
other mechanical strength properties and is generally the
determination of the resistance of a given ceramic material to
easiest and most economical test procedure available. The
simulated environmental heat service conditions.
values are useful for purposes of design, quality control,
11.2 Significance and Use—These tests serve as an evalu-
research, and the comparison of different ceramic composi-
ation of the resistance of a particular ceramic composition,
tions.
shape, and dimension to temperature stress relative to another
7.3 Procedure:
composition of the same shape and dimensions.
7.3.1 Method A—Determine the flexural strength in accor-
11.3 Hazards—(Warning—Acetone vapors are flammable
dance with Test Methods C674.
and poisonous and should not be breathed. The bath in 11.4.2
7.3.2 Method B—Microbar MOR Test—Determine the flex-
shall be operated in a vented hood with no open flames or
ural strength in accordance with Test Method F417.
sparks nearby.)
(Warning—Under certain conditions some ceramic speci-
8. Elastic Properties
mens can disintegrate explosively, sending out fragments at
damage-producing velocities and causing splashing of bath
8.1 Scope—This method obtains, as a function of tempera-
mediums.)
ture,Young’s modulus of elasticity, the shear modulus (modu-
(Warning—Face shields, long-sleeve coat, and insulating
lus of rigidity), and Poisson’s ratio for vitrified ceramic
materials. gloves shall be worn by test personnel to prevent injury.)
8.2 Significance and Use—The elastic properties of a ce- 11.4 Apparatus:
ramic are important design parameters for load-bearing appli- 11.4.1 Liquid Cold Bath, maintained at <1°C (1.8°F) and
cations and give indications of relative rigidity of a material. consisting of chopped ice and water.
8.3 Pr
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