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ASTM C1326-13(2023)

(Test Method)

Standard Test Method for Knoop Indentation Hardness of Advanced Ceramics

Standard Test Method for Knoop Indentation Hardness of Advanced Ceramics

SIGNIFICANCE AND USE
5.1 For advanced ceramics, Knoop indenters are used to create indentations. The surface projection of the long diagonal is measured with optical microscopes.  
5.2 The Knoop indentation hardness is one of many properties that is used to characterize advanced ceramics. Attempts have been made to relate Knoop indentation hardness to other hardness scales, but no generally accepted methods are available. Such conversions are limited in scope and should be used with caution, except for special cases where a reliable basis for the conversion has been obtained by comparison tests.  
5.3 For advanced ceramics, the Knoop indentation is often preferred to the Vickers indentation since the Knoop long diagonal length is 2.8 times longer than the Vickers diagonal for the same force, and cracking is much less of a problem (1).5 On the other hand, the long slender tip of the Knoop indentation is more difficult to precisely discern, especially in materials with low contrast. The indentation forces chosen in this test method are designed to produce indentations as large as may be possible with conventional microhardness equipment, yet not so large as to cause cracking.  
5.4 The Knoop indentation is shallower than Vickers indentations made at the same force. Knoop indents may be useful in evaluating coating hardnesses.  
5.5 Knoop hardness is calculated from the ratio of the applied force divided by the projected indentation area on the specimen surface. It is assumed that the elastic springback of the narrow diagonal is negligible. (Vickers indenters are also used to measure hardness, but Vickers hardness is calculated from the ratio of applied force to the area of contact of the four faces of the undeformed indenter.)  
5.6 A full hardness characterization includes measurements over a broad range of indentation forces. Knoop hardness of ceramics usually decreases with increasing indentation size or indentation force such as that shown in Fig. 1.6 The trend is known as the in...
SCOPE
1.1 This test method covers the determination of the Knoop indentation hardness of advanced ceramics. In this test, a pointed, rhombic-based, pyramidal diamond indenter of prescribed shape is pressed into the surface of a ceramic with a predetermined force to produce a relatively small, permanent indentation. The surface projection of the long diagonal of the permanent indentation is measured using a light microscope. The length of the long diagonal and the applied force are used to calculate the Knoop hardness which represents the material’s resistance to penetration by the Knoop indenter.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Units—When Knoop and Vickers hardness tests were developed, the force levels were specified in units of grams-force (gf) and kilograms-force (kgf). This standard specifies the units of force and length in the International System of Units (SI); that is, force in newtons (N) and length in mm or μm. However, because of the historical precedent and continued common usage, force values in gf and kgf units are occasionally provided for information. This test method specifies that Knoop hardness be reported either in units of GPa or as a dimensionless Knoop hardness number.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-Dec-2022
ICS
81.060.30 - Advanced ceramics
Technical Committee
C28 - Advanced Ceramics
Drafting Committee
C28.01 - Mechanical Properties and Performance
Current Stage
Ref Project

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ASTM C1326-13(2023) - Standard Test Method for Knoop Indentation Hardness of Advanced CeramicsASTM C1326-13(2023) - Standard Test Method for Knoop Indentation Hardness of Advanced Ceramics
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ASTM C1326-13(2023) - Standard Test Method for Knoop Indentation Hardness of Advanced Ceramics
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1326 − 13 (Reapproved 2023)
Standard Test Method for
1
Knoop Indentation Hardness of Advanced Ceramics
This standard is issued under the fixed designation C1326; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
1.1 This test method covers the determination of the Knoop
2.1 ASTM Standards:
indentation hardness of advanced ceramics. In this test, a C730 Test Method for Knoop Indentation Hardness of Glass
pointed, rhombic-based, pyramidal diamond indenter of pre-
C849 Test Method for Knoop Indentation Hardness of Ce-
scribed shape is pressed into the surface of a ceramic with a
ramic Whitewares
predetermined force to produce a relatively small, permanent
E4 Practices for Force Calibration and Verification of Test-
indentation. The surface projection of the long diagonal of the
ing Machines
permanent indentation is measured using a light microscope.
E177 Practice for Use of the Terms Precision and Bias in
The length of the long diagonal and the applied force are used
ASTM Test Methods
to calculate the Knoop hardness which represents the material’s
E384 Test Method for Microindentation Hardness of Mate-
resistance to penetration by the Knoop indenter.
rials
E691 Practice for Conducting an Interlaboratory Study to
1.2 The values stated in SI units are to be regarded as
Determine the Precision of a Test Method
standard. No other units of measurement are included in this
IEEE/ASTM SI 10 Standard for Use of the International
standard.
System of Units (SI) (The Modern Metric System)
1.3 Units—When Knoop and Vickers hardness tests were
3
2.2 European Standard:
developed, the force levels were specified in units of grams-
CEN ENV 843-4 Advanced Technical Ceramics, Monolithic
force (gf) and kilograms-force (kgf). This standard specifies
Ceramics, Mechanical Properties at Room Temperature,
the units of force and length in the International System of
Part 4: Vickers, Knoop, and Rockwell Superficial Hard-
Units (SI); that is, force in newtons (N) and length in mm or
ness Tests
μm. However, because of the historical precedent and contin-
4
ued common usage, force values in gf and kgf units are
2.3 ISO Standard:
occasionally provided for information. This test method speci-
ISO 9385 Glass and Glass Ceramics—Knoop Hardness Test
fies that Knoop hardness be reported either in units of GPa or
as a dimensionless Knoop hardness number.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 Knoop hardness number (HK), n—an expression of
responsibility of the user of this standard to establish appro-
hardness obtained by dividing the force applied to the Knoop
priate safety, health, and environmental practices and deter-
indenter by the projected area of the permanent impression
mine the applicability of regulatory limitations prior to use.
made by the indenter.
1.5 This international standard was developed in accor-
3.1.2 Knoop indenter, n—a rhombic-based pyramidal-
dance with internationally recognized principles on standard-
shaped diamond indenter with edge angles of 172° 30' and
ization established in the Decision on Principles for the
130° 00'.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1
This test method is under the jurisdiction of ASTM Committee C28 on the ASTM website.
3
Advanced Ceramics and is the direct responsibility of Subcommittee C28.01 on Available from European Committee for Standardization (CEN), 36 rue de
Mechanical Properties and Performance. Stassart, B-1050, Brussels, Belgium, http://www.cenorm.be.
4
Current edition approved Jan. 1, 2023. Published February 2023. Originally Available from International Organization for Standardization (ISO), 1, ch. de
approved in 1996. Last previous edition approved in 2018 as C1326 – 13 (2018). la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://
DOI: 10.1520/C1326-13R23. www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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FIG. 1 Microcracks Associated with Grinding (Ref. (1))2  
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1.1 This test method covers determination of the flexural strength of advanced ceramics at elevated temperatures.2 Four-point-1/4-point and three-point loadings with prescribed spans are the standard as shown in Fig. 1. Rectangular specimens of prescribed cross-section are used with specified features in prescribed specimen-fixture combinations. Test specimens may be 3 by 4 by 45 to 50 mm in size that are tested on 40-mm outer span four-point or three-point fixtures. Alternatively, test specimens and fixture spans half or twice these sizes may be used. The test method permits testing of machined or as-fired test specimens. Several options for machining preparation are included: application matched machining, customary procedures, or a specified standard procedure. This test method describes the apparatus, specimen requirements, test procedure, calculations, and reporting requirements. The test method is applicable to monolithic or particulate- or whisker-reinforced ceramics. It may also be used for glasses. It is not applicable to continuous fiber-reinforced ceramic composites.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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SIGNIFICANCE AND USE
4.1 This test method may be used for material development, quality control, characterization, and design data generation purposes. This test method is intended to be used with ceramics whose strength is 50 MPa (~7 ksi) or greater. The test method may also be used with glass test specimens, although Test Methods C158 is specifically designed to be used for glasses. This test method may be used with machined, drawn, extruded, and as-fired round specimens. This test method may be used with specimens that have elliptical cross section geometries.  
4.2 The flexure strength is computed based on simple beam theory with assumptions that the material is isotropic and homogeneous, the moduli of elasticity in tension and compression are identical, and the material is linearly elastic. The average grain size should be no greater than one-fiftieth of the rod diameter. The homogeneity and isotropy assumptions in the standard rule out the use of this test for continuous fiber-reinforced ceramics.  
4.3 Flexural strength of a group of test specimens is influenced by several parameters associated with the test procedure. Such factors include the loading rate, test environment, specimen size, specimen preparation, and test fixtures (1-3).3 This method includes specific specimen-fixture size combinations, but permits alternative configurations within specified limits. These combinations were chosen to be practical, to minimize experimental error, and permit easy comparison of cylindrical rod strengths with data for other configurations. Equations for the Weibull effective volume and Weibull effective surface are included.  
4.4 The flexural strength of a ceramic material is dependent on both its inherent resistance to fracture and the size and severity of flaws in the material. Flaws in rods may be intrinsically volume-distributed throughout the bulk. Some of these flaws by chance may be located at or near the outer surface. Flaws may alternatively be intrinsically surface-distrib...
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1.1 This test method is for the determination of flexural strength of rod-shaped specimens of advanced ceramic materials at ambient temperature. In many instances it is preferable to test round specimens rather than rectangular bend specimens, especially if the material is fabricated in rod form. This method permits testing of machined, drawn, or as-fired rod-shaped specimens. It allows some latitude in the rod sizes and cross section shape uniformity. Rod diameters between 1.5 and 8 mm and lengths from 25 to 85 mm are recommended, but other sizes are permitted. Four-point-1/4-point as shown in Fig. 1 is the preferred testing configuration. Three-point loading is permitted. This method describes the apparatus, specimen requirements, test procedure, calculations, and reporting requirements. The method is applicable to monolithic or particulate- or whisker-reinforced ceramics. It may also be used for glasses. It is not applicable to continuous fiber-reinforced ceramic composites.
FIG. 1 Four-Point-1/4-Point Flexure Loading Configuration  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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ASTM C1323-22(Test Method)
Standard Test Method for Ultimate Strength of Advanced Ceramics with Diametrally Compressed C-Ring Specimens at Ambient Temperature

SIGNIFICANCE AND USE
4.1 This test method may be used for material development, material comparison, quality assurance, and characterization. Extreme care should be exercised when generating design data.  
4.2 For a C-ring under diametral compression, the maximum tensile stress occurs at the outer surface. Hence, the C-ring specimen loaded in compression will predominately evaluate the strength distribution and flaw population(s) on the external surface of a tubular component in the hoop direction. Accordingly, the condition of the inner surface may be of lesser consequence in specimen preparation and testing.
Note 1: A C-ring in tension or an O-ring in compression may be used to evaluate the internal surface.  
4.2.1 The flexure stress is computed based on simple curved beam theory (1-5).3 It is assumed that the material is isotropic and homogeneous, the moduli of elasticity are identical in compression or tension, and the material is linearly elastic. These homogeneity and isotropy assumptions preclude the use of this standard for continuous fiber reinforced composites. Average grain size(s) should be no greater than one fiftieth (1/50 ) of the C-ring thickness. The curved beam stress solution from engineering mechanics is in good agreement (within 2 %) with an elasticity solution as discussed in (6) for the test specimen geometries recommended for this standard. The curved beam stress equations are simple and straightforward, and therefore it is relatively easy to integrate the equations for calculations for effective area or effective volume for Weibull analyses as discussed in Appendix X1.  
4.2.2 The simple curved beam and theory of elasticity stress solutions both are two-dimensional plane stress solutions. They do not account for stresses in the axial (parallel to b) direction, or variations in the circumferential (hoop, σθ) stresses through the width (b) of the test piece. The variations in the circumferential stresses increase with increases in width (b) and ring thicknes...
SCOPE
1.1 This test method covers the determination of ultimate strength under monotonic loading of advanced ceramics in tubular form at ambient temperatures. The ultimate strength as used in this test method refers to the strength obtained under monotonic compressive loading of C-ring specimens such as shown in Fig. 1, where monotonic refers to a continuous nonstop test rate with no reversals from test initiation to final fracture. This method permits a range of sizes and shapes since test specimens may be prepared from a variety of tubular structures. The method may be used with microminiature test specimens.
FIG. 1 C-Ring Test Geometry with Defining Geometry and Reference Angle (θ) for the Point of Fracture Initiation on the Circumference  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Values expressed in this test method are in accordance with the International System of Units (SI) and IEEE/ASTM SI 10.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1292-22(Test Method)
Standard Test Method for Shear Strength of Continuous Fiber-Reinforced Advanced Ceramics at Ambient Temperatures

SIGNIFICANCE AND USE
5.1 Continuous fiber-reinforced ceramic composites can be candidate materials for structural applications requiring high degrees of wear and corrosion resistance, and damage tolerance at high temperatures.  
5.2 Shear tests provide information on the strength and deformation of materials under shear stresses.  
5.3 This test method may be used for material development, material comparison, quality assurance, characterization, and design data generation.  
5.4 For quality control purposes, results derived from standardized shear test specimens may be considered indicative of the response of the material from which they were taken for given primary processing conditions and post-processing heat treatments.
SCOPE
1.1 This test method covers the determination of shear strength of continuous fiber-reinforced ceramic composites (CFCCs) at ambient temperature. The test methods addressed are (1) the compression of a double-notched test specimen to determine interlaminar shear strength, and (2) the Iosipescu test method to determine the shear strength in any one of the material planes of laminated composites. Test specimen fabrication methods, testing modes (load or displacement control), testing rates (load rate or displacement rate), data collection, and reporting procedures are addressed.  
1.2 This test method is used for testing advanced ceramic or glass matrix composites with continuous fiber reinforcement having unidirectional (1D) or bidirectional (2D) fiber architecture. This test method does not address composites with 3D fiber architecture or discontinuous fiber-reinforced, whisker-reinforced, or particulate-reinforced ceramics.  
1.3 The values stated in SI units are to be regarded as the standard and are in accordance with IEEE/ASTM SI 10.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in 8.1 and 8.2.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1469-22(Test Method)
Standard Test Method for Shear Strength of Joints of Advanced Ceramics at Ambient Temperature

SIGNIFICANCE AND USE
5.1 Advanced ceramics can be candidate materials for structural applications requiring high degrees of wear and corrosion resistance, often at elevated temperatures.  
5.2 Joints are produced to enhance the performance and applicability of materials. While the joints between similar materials are generally made for manufacturing complex parts and repairing components, those involving dissimilar materials usually are produced to exploit the unique properties of each constituent in the new component. Depending on the joining process, the joint region may be the weakest part of the component. Since under mixed-mode and shear loading the load transfer across the joint requires reasonable shear strength, it is important that the quality and integrity of joint under in-plane shear forces be quantified. Shear strength data are also needed to monitor the development of new and improved joining techniques.  
5.3 Shear tests provide information on the strength and deformation of materials under shear stresses.  
5.4 This test method may be used for material development, material comparison, quality assurance, characterization, and design data generation.  
5.5 For quality control purposes, results derived from standardized shear test specimens may be considered indicative of the response of the material from which they were taken for given primary processing conditions and post-processing heat treatments.
SCOPE
1.1 This test method covers the determination of shear strength of joints in advanced ceramics at ambient temperature using asymmetrical four-point flexure. Test specimen geometries, test specimen fabrication methods, testing modes (that is, force or displacement control), testing rates (that is, force or displacement rate), data collection, and reporting procedures are addressed.  
1.2 This test method is used to measure shear strength of ceramic joints in test specimens extracted from larger joined pieces by machining. Test specimens fabricated in this way are not expected to warp due to the relaxation of residual stresses but are expected to be much straighter and more uniform dimensionally than butt-jointed test specimens prepared by joining two halves, which is not recommended. In addition, this test method is intended for joints, which have either low or intermediate strengths with respect to the substrate material to be joined. Joints with high strengths should not be tested by this test method because of the high probability of invalid tests resulting from fractures initiating at the reaction points rather than in the joint. Determination of the shear strength of joints using this test method is appropriate particularly for advanced ceramic matrix composite materials but also may be useful for monolithic advanced ceramic materials.  
1.3 Values expressed in this test method are in accordance with the International System of Units (SI) and IEEE/ASTM SI 10.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are noted in 8.1.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1730-17(2022)(Test Method)
Standard Test Method for Particle Size Distribution of Advanced Ceramics by X-Ray Monitoring of Gravity Sedimentation

SIGNIFICANCE AND USE
5.1 This test method is useful to both suppliers and users of powders, as outlined in 1.1 and 1.2, in determining particle size distribution for product specifications, manufacturing control, development, and research.  
5.2 Users should be aware that sample concentrations used in this test method may not be what is considered ideal by some authorities, and that the range of this test method extends into the region where Brownian movement could be a factor in conventional sedimentation. Within the range of this test method, neither the sample concentration nor Brownian movement is believed to be significant. Standard reference materials traceable to national standards, of chemical composition specifically covered by this test method, are available from NIST,3 and perhaps other suppliers.  
5.3 Reported particle size measurement is a function of the actual particle dimension and shape factor as well as the particular physical or chemical properties being measured. Caution is required when comparing data from instruments operating on different physical or chemical parameters or with different particle size measurement ranges. Sample acquisition, handling, and preparation can also affect reported particle size results.  
5.4 Suppliers and users of data obtained using this test method need to agree upon the suitability of these data to provide specification for and allow performance prediction of the materials analyzed.
SCOPE
1.1 This test method covers the determination of particle size distribution of advanced ceramic powders. Experience has shown that this test method is satisfactory for the analysis of silicon carbide, silicon nitride, and zirconium oxide in the size range of 0.1 up to 50 µm.  
1.1.1 However, the relationship between size and sedimentation velocity used in this test method assumes that particles sediment within the laminar flow regime. It is generally accepted that particles sedimenting with a Reynolds number of 0.3 or less will do so under conditions of laminar flow with negligible error. Particle size distribution analysis for particles settling with a larger Reynolds number may be incorrect due to turbulent flow. Some materials covered by this test method may settle in water with a Reynolds number greater than 0.3 if large particles are present. The user of this test method should calculate the Reynolds number of the largest particle expected to be present in order to judge the quality of obtained results. Reynolds number (Re) can be calculated using the following equation:
   where:  
  D  =  the diameter of the largest particle expected to be present, in cm,   ρ  =  the particle density, in g/cm3,   ρ0  =  the suspending liquid density, in g/cm3,   g  =  the acceleration due to gravity, 981 cm/sec2, and   η  =  the suspending liquid viscosity, in poise.    
1.1.2 A table of the largest particles that can be analyzed with a suggested maximum Reynolds number of 0.3 or less in water at 35 °C is given for a number of materials in Table 1. A column of the Reynolds number calculated for a 50-µm particle sedimenting in the same liquid system is also given for each material. Larger particles can be analyzed in dispersing media with viscosities greater than that for water. Aqueous solutions of glycerine or sucrose have such higher viscosities.  
1.2 The procedure described in this test method may be applied successfully to other ceramic powders in this general size range, provided that appropriate dispersion procedures are developed. It is the responsibility of the user to determine the applicability of this test method to other materials. Note however that some ceramics, such as boron carbide and boron nitride, may not absorb X-rays sufficiently to be characterized by this analysis method.  
1.3 The values stated in cgs units are to be regarded as the standard, which is the long-standing industry practice. The values given in parentheses are for information onl...

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