1、Designation: F 19 64 (Reapproved 2005)e1Standard Test Method forTension and Vacuum Testing Metallized Ceramic Seals1This standard is issued under the fixed designation F 19; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year
2、of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEIn 6.1, cm was editorially changed to cc in January 2005.1. Scope1.1 This test method covers procedures for conductingtensio
3、n and vacuum tests on metal-ceramic seals to determinethe bond strength of brazed, metallized ceramics. This testmethod is not to be considered as an absolute tension test forthe ceramic.1.2 The values stated in inch-pound units are to be regardedas the standard. The values given in parentheses are
4、forinformation only.1.3 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 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to
5、 use.2. Referenced Documents2.1 ASTM Standards:E4 Practices for Force Verification of Testing Machines2E6 Terminology Relating to Methods of Mechanical Test-ing23. Terminology3.1 Definitions:3.1.1 The definitions of terms relating to tension testingappearing in Definitions E6, shall apply to the ter
6、ms used inthis test method.4. Apparatus4.1 Testing MachinesMachines used for tension testingshall conform to the requirements of Methods E4. Only loadsthat are within the loading range of the testing machine, asdefined in Methods E4, shall be used for determining tensilestrengths.4.2 Gripping Device
7、sVarious types of gripping devicesmay be used to apply the load to the test specimen. Thoseshown in Fig. 1 are recommended, but regardless of whichgrips are used, care shall be taken that the axis of the testspecimen is in alignment with the centerline of the test machineheads.5. Preparation of Spec
8、imens5.1 Prepare the test specimen by brazing together two piecesof ceramic, shown in Fig. 2, at their respective metalizedsurfaces, as described in 5.1.1 to 5.1.3:5.1.1 CeramicsGrind the test surface, A,(Fig. 2)ofthetwo ceramic parts flat to within 0.00025 in. (0.0064 mm)according to good grinding
9、practice using an abrasive passingor finer than a No. 100 (150-m) sieve. The ground surface, A,of each part shall be parallel to shoulder C, as shown in Fig. 2,consistent with the best commercial practice. The over-allappearance of each ceramic half of the test specimen shallindicate good commercial
10、 practice, and shall be free fromobvious defects. In the results of the test, report the method ofmanufacture of the specimen components, that is, slip cast,hotpressed, hydrostatically molded, etc. Measure and recordthe test surface area of each ceramic half on a projectioncomparator, or by other su
11、itable means. Dye check the twoceramic parts and inspect them for flaws (Note 1). Reject allparts showing flaws considered conducive to abnormal failuresof either ceramic part.NOTE 1A suggested dye check procedure is described in the Appen-dix.5.1.2 Metallized CoatingMetallize the specimen halvesund
12、er identical conditions, that is, temperature, atmosphere,etc. The type of metallizing used is optional, or as mutuallyagreed upon between producer and consumer. Apply themetallizing coating only to the test surface A, Fig. 2, on thespecimen. The method of metallizing is optional, that is, silkscree
13、n, brush, spray, roller, etc., but should be reported.NOTE 2A typical metallizing procedure is described in the Appendix.5.1.3 Assembling the Test SpecimenPlace the two matingparts in a suitable jig to achieve axial alignment of the matedceramic halves and alignment of the metallized surfaces.Accura
14、te alignment, which is essential to attain uniform test1This test method is under the jurisdiction of ASTM Committee F01 onElectronics and is the direct responsibility of Subcommittee F01.03 on MetallicMaterials.Current edition approved Jan. 1, 2005. Published January 2005. Originallyapproved in 196
15、1 as F 19 61 T. Last previous edition approved in 2000 as F 19 64(2000).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, refer to the standards Document Summary page onthe AS
16、TM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.results, may be accomplished by jigging with a rod ofrefractory material, such as ceramic or carbon (Fig. 3). Pass therod through the assembly and then braze the specimen in
17、avertical position. In the test results, report the brazing materialused; such as copper-silver eutectic, copper-gold alloy, 35 to65 %, etc. Use sufficient material to produce an even fillet atNOTE 1Tolerance on all dimensions shown, 60.016 in. (0.41 mm).FIG. 1 Self Aligning Grip for Tension TestASe
18、al surface area to be metalized.BSurface inscribed with date as to ceramic batch and firing temperature.CGripping shoulder.FIG. 2 Ceramic Half of Tension Test SpecimenF 19 64 (2005)e12the joint. Load the assembly to produce pressure on the sealduring the brazing operation and report the weight of th
19、e load.6. Procedure6.1 Leak TestThe brazed test specimen may be vacuum-leak checked on any conventional helium spectrometer-typeleak checker with a sensitivity of 5 3 109cc/s at standardtemperature and pressure. Subject the specimen continuouslyto an atmosphere of helium for12 to 5 min. The leak-che
20、ckinginstrument, set at maximum sensitivity, shall show no indica-tion of a leak during the test period.6.2 Tension Test Place the specimen in the self-aligninggrips with a polytetrafluoroethylene (TFE-fluorocarbon)washer between the ceramic and the jaws of the grip (see Fig.1). Test all specimens u
21、nder the same loading rate which,although optional, shall be reported.6.3 Other Tests Brazed assemblies prepared in accor-dance with Section 5 can also be used to:6.3.1 Test ceramic-metal seals with a metal washer insertedbetween the test pieces, and6.3.2 Perform environmental tests such as heat sho
22、ck, oxi-dation resistance, and bakeout, to determine either the point ofvacuum failure or the tensile strength at vacuum failure.7. Calculation7.1 Calculate the tensile strength by dividing the maximumload on the specimen during the tension test by the originalcross-sectional area. Consider only tho
23、se specimens that breakin or near the seal area when calculating test data. Fracture ofthe test specimen in any other area than at or adjacent to theseal may indicate either a lack of alignment of the ceramicparts or a bond strength exceeding the range of the testspecimen.8. Report8.1 Report the fol
24、lowing information:8.1.1 Method of manufacture of the specimen components,8.1.2 Test surface area of each specimen component,8.1.3 Method of metallizing specimen,8.1.4 Brazing material used,8.1.5 Load applied to specimen during brazing,8.1.6 Results of leak test,8.1.7 Loading rate of tension test,8.
25、1.8 Tensile strength in pounds per square inch, and8.1.9 Results of other tests performed in addition to leak andtension tests.9. Keywords9.1 brazing; leak rate test; metallized ceramic seals; ten-sion testingAPPENDIX(Nonmandatory Information)X1. TYPICAL METALLIZING PROCEDUREX1.1 ScopeX1.1.1 This pr
26、ocedure is intended to serve as a guide forthose not familiar with ceramic metallizing techniques. It is notintended as a recommended procedure.X1.2 Summary of MethodX1.2.1 This procedure for metallizing the ceramic speci-mens is covered in five essential steps as follows:X1.2.1.1 Dye check,X1.2.1.2
27、 Clean,X1.2.1.3 Paint,X1.2.1.4 Fire, andX1.2.1.5 Plate.X1.3 Dye CheckX1.3.1 Dye check the test specimen parts to bring out flawssuch as chips or cracks in the ceramic in the following manner:X1.3.1.1 Soak the test specimen in dye.NOTE X1.1A satisfactory dye is Rhodamine B, 50 % concentratedsolution,
28、 diluted to 30 mL/L with methyl alcohol.X1.3.1.2 Rinse the specimen in methyl alcohol until the dyeis removed, and allow it to dry.X1.3.2 Inspect the specimen for flaws.X1.3.2.1 Visible cracks on the test specimen are cause forrejection.X1.3.2.2 Chips in areas other than the seal area are permis-sib
29、le.X1.3.2.3 Excessive retention of dye, indicating high poros-ity of the ceramic is cause for rejection.X1.4 Cleaning of Ceramics to Be MetalizedX1.4.1 The specimen shall be free of all oils and greases andthe seal surface free of contamination from metallic particles orsmears when cleaned in the fo
30、llowing manner:X1.4.1.1 Soak the specimen in a hot solution of any gooddetergent for12 h, then rinse in deionized water.X1.4.1.2 Soak the specimen for 5 min in hot (approximately65C) dilute (1 + 1) solution of nitric acid (HNO3), technicalgrade, and water. Rinse the specimen in hot (approximately80C
31、) deionized water, and oven dry.NOTE 1MaterialACX Graphite.FIG. 3 Alignment Jig for Brazing Tension Test SpecimenF 19 64 (2005)e13X1.5 Application of Metalizing CoatingX1.5.1 Paint the seal surface of the ceramic, using a suitablebrush, with the (typical) mixture shown in Table X1.1.X1.5.2 Mix the c
32、omponents in a 1-qt. (1-L) ball mill, andgrind with alumina balls for 100 h.X1.5.3 Mount the specimen on a slowly rotating fixture. Dipthe brush in the well-stirred mixture and apply a smooth,continuous, uniform coat to the ceramic. Use sufficient mixtureon the brush to cover the surface to be coate
33、d in one operation.Keep the paint well stirred while painting. After painting airdry the specimen.X1.6 FiringX1.6.1 Fire the coated specimen in a furnace capable ofsustaining 1500C continuous operation. The atmosphere inwhich the part is fired should be strongly reducing but with asufficiently high
34、dew point to prevent reduction of the ceramic.X1.6.2 Fire the specimen for 30 min at 1500 to 1525C inhydrogen, bubbled through water to attain the proper humidity.Cool the specimen in hydrogen at the recommended rateprescribed in X1.6.3.X1.6.3 Recommended rates of heating and cooling areshown in Tab
35、le X1.2.X1.7 PlatingX1.7.1 To facilitate brazing with commercially availablealloys, plate the metalized specimens to a thickness of 0.0005in. (0.013 mm) with nickel.Asuitable plating bath (Note X1.2)is as follows:Material QuantityNickel chloride (NiCl2) 300 g/LBoric acid (H3BO3)30g/LpHA3.0AAdjust th
36、e pH with pure hydrochloric acid (HCl).NOTE X1.2Use pure nickel anodes. Operate the bath at 60C (ap-proximate).X1.7.2 Mount the specimen on a rack and make contactwith the seal area. Plate the part at 60 A/ft2(5.5 A/m2), for 10min. Rinse the specimen in deionized water, then rinse inacetone, and air
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40、mmittee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveadd
41、ress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE X1.1 Typical Metallization Coating MixtureMaterial QuantityMolybdenum metal powder, fine, passing No. 200 (75-m) sieve, g 200Manganese metal powder, fine, passing No. 200
42、 (75-m) sieve, g 50Ethylcellulose, g 5Methyl amyl acetate, mL 65Methyl ethyl ketone, mL 45Ethylene glycol monoethyl ether (Cellosolve), mL 85Acetone, mL 90TABLE X1.2 Typical Heating and Cooling RatesTemperature Range TimeHeating20 to 600C 15 min600 to 1200C 30 min1200 to 1500C 15 minCooling:1500 to 1000C1000 to room temperature (C)5min60 minF 19 64 (2005)e14
