1、Designation: C 1300 95 (Reapproved 2007)Standard Test Method forLinear Thermal Expansion of Glaze Frits and CeramicWhiteware Materials by the Interferometric Method1This standard is issued under the fixed designation C 1300; the number immediately following the designation indicates the year oforigi
2、nal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the interferometric determina-tion of l
3、inear thermal expansion of premelted glaze frits andfired ceramic whiteware materials at temperatures lower than1000C (1830F).1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish ap
4、pro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 289 Test Method for Linear Thermal Expansion of RigidSolids with Interferometry3. Significance and Use3.1 This test method defines the thermal e
5、xpansion of glazefrits by the interferometric method. This determination iscritical in avoiding crazing (cracking) of these glass coatingsdue to mismatching of the thermal expansion between thecoating and substrate materials.4. Apparatus4.1 Sample Preparation Equipment:34.1.1 Glazed Porcelain Crucib
6、le, No. 0.4.1.2 Fireclay Crucible, 102 mm (4 in.) in diameter.4.1.3 Rotating Abrasive Grinding Wheel (a silicon carbidetype is satisfactory).4.2 Micrometer Calipers, having a sensitivity such that theindex can be read to 0.002 mm (0.0001 in.).4.3 Measuring Apparatus, consisting of fused silica inter
7、-ferometer plates, viewing apparatus, an electric furnace andcontrol, potentiometer, pyrometer, and a suitable monochro-matic light source of known wavelength.4.3.1 FurnaceThe furnace shall be a vertical electric tubefurnace controlled by rheostat or other means so that theheating rate of the furnac
8、e can be readily duplicated from roomtemperature to 1000C (1830F). The heating rate shall notexceed 3C (5.5F)/min.4.3.2 Temperature-Measuring InstrumentA calibratedplatinum versus platinum-rhodium thermocouple (or aChromel versus Alumel thermocouple if it is frequently cali-brated) in conjunction wi
9、th a potentiometer shall be used. Thepotentiometer shall be capable of being read to 2C (or 4F)and shall have automatic compensation for the temperature ofthe reference junction, or the reference junction shall be held at0C (32F) by means of an ice bath.5. Test Specimens5.1 For frit samples, three t
10、est specimens shall be preparedas follows:5.1.1 Fill a No. 0 glazed porcelain crucible with frit, placethe filled crucible inside a 102-mm (4-in.) diameter fireclaycrucible partly filled with silica, and work the small crucibledown into the silica until approximately 75 % of the smallcrucible is bel
11、ow the level of the silica.5.1.2 Place the crucible assembly into a furnace that is at atemperature high enough to just melt the mass. Hold for 15 minafter the frit has reached the furnace temperature.5.1.3 Remove the crucible, rapidly transfer it to anotherfurnace that is at the frit firing tempera
12、ture, and cool in thefurnace at a rate not to exceed 60C (110F)/h.1This test method is under the jurisdiction ofASTM Committee C21 on CeramicWhitewares and Related Products and is the direct responsibility of SubcommitteeC21.03 on Methods for Whitewares and Environmental Concerns.Current edition app
13、roved May 1, 2007. Published May 2007. Originallyapproved in 1995. Last previous edition approved in 2001 as C130095(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
14、fer to the standards Document Summary page onthe ASTM website.3An example of suitable test equipment and an inferometric method may befound in the paper by Merritt, G. E., “The Interference Method of MeasuringThermal Expansion,” Journal of Research , National Bureau of Standards, Vol 10,No. 1, Janua
15、ry 1933, p. 59 (RP 515).A description of a permissible automatic fringe recording device may be foundin the paper by Saunders, J. B., “An Apparatus for Photographing InterferencePhenomenon,” Journal of Research, National Bureau of Standards, Vol 35, No. 3,September 1945, p. 157 (RP 1668).1Copyright
16、ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1.4 Break the small crucible open and break up thevitreous mass. Select six fragments from the interior of themass (to avoid side portions diluted by the ceramic crucible)having minimum conical
17、dimensions of 3 mm (18 in.) at thebase and 6 mm (14 in.) high.5.2 For fired samples, break and select six samples havingminimum conical dimensions of 3 mm (18 in.) at the base and6mm(14 in.) in height. For all samples, grind the base of the(cones) flat and cement the flat cone base to the flat end o
18、f aglass rod with heated sealing wax. Grind the piece to a finishedcone by rotating the rod while the piece is held against arotating abrasive wheel (a silicon carbide type is satisfactory).5.2.1 When a reasonably symmetrical cone with a roundedtip is obtained, remove it from the rod by heating the
19、wax or bypressure with the fingertips. Remove all sealing wax with aknife blade or abrasive paper.5.2.2 The test cone height may be of the order of 4.8 mm(316 in.). These bases must be smooth and flat. Use No. 0metallurgical paper to approach the desired figure and then usesuccessively finer papers
20、until the final reduction is made witha No. 3/0 paper.6. Calibration of Furnace46.1 Using the following procedure, calibrate the furnacecontrols to obtain a heating rate of 3C (5.5F)/min:6.1.1 Prepare three conical spacers closely approximatingthe dimensions of the final test pieces described in Sec
21、tion 5.These spacers shall be ground from fragments of refractoryceramic known to have a softening temperature in excess of1000C (1830F).6.1.2 Assemble the upper and lower interferometer plateswith three refractory spacers as described in Section 7, exceptfringe development is not necessary. Place t
22、his assembly in thefurnace test location. Center the hot junction of an 18 or20-gage thermocouple within the triangle formed by thespacers. It will usually be necessary to extend the thermo-couple out through the top of the furnace tube. This thermo-couple temperature measurement equipment shall mee
23、t therequirements in 4.3.2.6.1.3 The output of this thermocouple shall be used toestablish corrections required in calibrating the furnace tem-perature measuring system. Both temperature values and heat-ing rates shall be so corrected if differences exist.7. Procedure7.1 Assemble (outside the furnac
24、e) the three test piecesprepared as described in Section 5 between the two interfer-ometer plates as follows:7.1.1 Place the plate with the one frosted side down withinthe refractory specimen crucible.7.1.2 Place the three test pieces on this plate in an equilat-eral triangle.7.1.3 Lower the clear p
25、late onto the test pieces keeping themark or notch identifying the “wedge side” in the “up”position.7.1.4 Set this assembly at a height comparable to that to beused inside the furnace.7.2 Rotate the telescope and center it over the test specimenassembly. Direct the monochromatic light source down th
26、etube. If four to eight fringes are present, the setup is correct. Iffewer or more fringes are present, adjust the cone heights. Insome cases, mere tapping of the specimen assembly willproduce the correct number of fringes. Carefully measure andrecord the height of each cone. Upon achieving the prop
27、ernumber of fringes, place the refractory ring cover on thecrucible and recheck for fringes.7.3 Without rotating the crucible, gently lower it into thefurnace and onto the bottom support so that the thermocouplerests at the bottom of the crucible. Cover the top of the furnacewith a quartz plate.7.4
28、Rotate the telescope and check the fringe pattern. Ifexcessive glare or poor contrast are present, adjust by movingthe quartz cover, moving the light source, or releveling thetelescope.NOTE 1Removal of the telescope eyepiece should reveal a bright dot,which is the true image. This must be in the fie
29、ld or no fringes will beseen. If this bright dot of the true image is not seen when the eyepiece isremoved, a great deal of trial and error adjustment of the telescope tripodmust be made. A number of false images may also be present. These mustbe sorted out by inserting the eyepiece and checking to
30、see if fringes arepresent. If no fringes are seen, the bright dot is a false image.7.5 Standardize the potentiometer if necessary and set thepotentiometer or other temperature-measuring instrument to38C (100F).7.6 Slowly heat the furnace to 38C (100F). Center thecross hair of the telescope upon any
31、convenient fringe andrecord the temperature corresponding to each fifth fringe.7.7 Continue heating the furnace to maintain a 3C (5.5F)/min temperature rise or less. Below 100C a heating rate notexceeding 1.5C/min is preferred. For frit samples, when thesoftening temperature has been reached, as sho
32、wn by thefringes retreating for at least one fringe, immediately turn offthe furnace to avoid reaction with the quartz plates.8. Calculations8.1 Calculate the percentage of linear thermal expansion foreach reading as follows:L 5 nl/200h! 1 Ac(1)where:L = linear thermal expansion, % from starting tem
33、pera-ture, t0C, to temperature of observation, tC,n = number of fringes passing the reference point duringthe change from temperature t0to temperature t,l = wavelength of the light source, m,h = height of the specimen at temperature t0, cm, andAc= air correction from temperature t0to temperature t,%
34、(see Table 1).8.2 Prepare a curve by plotting each temperature reading, t,on the horizontal axis against the corresponding percentageexpansion along the vertical axis. Table 18.3 Calculate the mean coefficient of thermal expansion, E,for any temperature range, t2to t3C, within the limits of thetest,
35、 as follows:4Saunders, J. B., “Improved Interferometric Procedure with Application toExpansion Measurements,” Journal of Research, National Bureau of Standards, Vol23, No. 1, July 1939, p. 179 ( RP 1227).C 1300 95 (2007)2E 5 L8/ 100t32 t2!# (2)where:L8 = linear thermal expansion, from temperature t2
36、C totemperature t3C as determined from the curve pre-pared in accordance with 8.2,%,t2= lower temperature in range t2to t3, andt3= higher temperature in range t2to t3.9. Report9.1 The report shall include the following:9.1.1 Designation of material tested,9.1.2 Method of preparation of test specimen
37、, cooling rate,etc.,9.1.3 Identification of type of apparatus used,9.1.4 Data sheet showing:9.1.4.1 Form and height of test specimens,9.1.4.2 Wavelength of light source,9.1.4.3 Starting temperature,9.1.4.4 Corrected temperature at each reading,9.1.4.5 Number of fringes, n, at each reading,9.1.4.6 Ca
38、lculation, nl/200h, for each reading,9.1.4.7 Air correction, Ac, for each reading,9.1.4.8 Percentage of expansion, L, computed for eachreading,9.1.5 The curve (see 8.2) showing temperature plottedagainst percentage of expansion, and9.1.6 Mean coefficient of linear thermal expansion perdegree Celsius
39、 over the desired temperature ranges.10. Precision and Bias10.1 The precision and bias of this test method of measuringthe linear thermal expansion of glaze frits are as specified inTest Method E 289.TABLE 1 Air Corrections From 20C To Temperatures IndicatedAAtmospheric pressure, 760 mm Hg.Temperatu
40、re,CAirCorrection, %Temperature,CAirCorrection, %Temperature,CAirCorrection, %Temperature,CAirCorrection, %20 0.0000 84 0.0049 175 0.0094 320 0.013821 0.0001 86 0.0050 178 0.0095 326 0.013922 0.0002 88 0.0051 331 0.014023 0.0003 89 0.0052 180 0.0096 335 0.014124 0.0004 183 0.009725 0.0005 90 0.0053
41、185 0.0098 340 0.014226 0.0006 92 0.0054 188 0.0099 343 0.014327 0.0007 94 0.0055 350 0.014428 0.0008 96 0.0056 190 0.0100 354 0.014529 0.0009 97 0.0057 194 0.0101 359 0.014698 0.0058 197 0.010230 0.0010 364 0.014732 0.0011 102 0.0059 200 0.0103 369 0.014833 0.0012 103 0.0060 202 0.0104 374 0.014935
42、 0.0013 104 0.0061 205 0.0105 378 0.015036 0.0014 106 0.0062 208 0.010637 0.0015 108 0.0063 386 0.015138 0.0016 210 0.0107 392 0.0152214 0.0108 397 0.015340 0.0017 110 0.0064 217 0.010941 0.0018 112 0.0065 403 0.015442 0.0019 114 0.0066 220 0.0110 409 0.015543 0.0020 116 0.0067 223 0.0111 415 0.0156
43、45 0.0021 118 0.0068 226 0.011246 0.0022 119 0.0069 229 0.0114 421 0.015747 0.0023 427 0.015848 0.0024 122 0.0070 235 0.0115 433 0.0159124 0.0071 238 0.0116 439 0.016050 0.0025 126 0.007251 0.0026 128 0.0073 241 0.0117 446 0.016152 0.0027 245 0.0118 453 0.016254 0.0028 130 0.0074 249 0.0119 459 0.01
44、6355 0.0029 132 0.007556 0.0030 134 0.0076 252 0.0120 466 0.016458 0.0031 136 0.0077 255 0.0121 470 0.016559 0.0032 138 0.0078 258 0.0122263 0.012361 0.0033 140 0.0079 266 0.0124 480 0.016663 0.0034 142 0.0080 269 0.0125 487 0.016764 0.0035 144 0.0081 493 0.016865 0.0036 146 0.0082 273 0.012666 0.00
45、37 148 0.0083 277 0.0127 502 0.016968 0.0038 510 0.017069 0.0039 150 0.0084 280 0.0128 517 0.0171154 0.0085 285 0.012970 0.0040 156 0.0086 289 0.0130 521 0.0172C 1300 95 (2007)3TABLE 1 ContinuedTemperature,CAirCorrection, %Temperature,CAirCorrection, %Temperature,CAirCorrection, %Temperature,CAirCor
46、rection, %72 0.0041 158 0.0087 534 0.017374 0.0042 292 0.013175 0.0043 160 0.0088 296 0.0132 542 0.017476 0.0044 163 0.0089 551 0.017578 0.0045 165 0.0090 300 0.0133 559 0.0176168 0.0091 305 0.013480 0.0046 309 0.013582 0.0047 170 0.0092 313 0.0136 568 0.017783 0.0048 173 0.0093 317 0.0137 578 0.017
47、8587 0.0179 700 0.0190 840 0.0200 1000 0.0209596 0.0180 712 0.0191 850 0.0201606 0.0181 726 0.0192 870 0.0202 1020 0.0210615 0.0182740 0.0193 880 0.0203 1040 0.0211620 0.0183 752 0.0194635 0.0184 900 0.0204 1060 0.0212766 0.0195646 0.0185 920 0.0205 1080 0.0213657 0.0186 780 0.0196790 0.0197 940 0.0
48、206 1100 0.0214668 0.0187679 0.0188 810 0.0198 960 0.0207690 0.0189 820 0.0199 980 0.0208AIf the starting temperature, t0, is above 20C, the entry in the table opposite that of the starting temperature should be subtracted from each of the succeedingcorrections.ASTM International takes no position r
49、especting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard o
