1、Designation: F19 11 (Reapproved 2016)Standard Test Method forTension and Vacuum Testing Metallized Ceramic Seals1This standard is issued under the fixed designation F19; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of l
2、ast revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers procedures for conductingtension and vacuum tests on metal-ceramic seals to determinethe bond stren
3、gth of brazed, metallized ceramics.1.2 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.3 This standard does not purport to address all
4、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 use.2. Referenced Documents2.1 ASTM Standards:2E4 Practices for Force
5、 Verification of Testing MachinesE6 Terminology Relating to Methods of Mechanical Testing3. Terminology3.1 Definitions:3.1.1 The definitions of terms relating to tension testingappearing in Terminology E6, shall apply to the terms used inthis test method.4. Significance and Use4.1 This test method c
6、overs procedures for conductingtension and vacuum tests on metal-ceramic seals.4.2 This test method is not to be considered as an absolutetension test for the ceramic.4.3 This test method is suitable for quality control andresearch and development use.5. Apparatus5.1 Testing MachinesMachines used fo
7、r 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.5.2 Gripping DevicesVarious types of gripping devicesmay be used to apply the load to the test
8、 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.6. Preparation of Specimens6.1 Prepare the test specimen by brazing together two piecesof ceramic
9、, shown in Fig. 2, at their respective metalizedsurfaces, as described in 6.1.1 to 6.1.3:6.1.1 CeramicsGrind the test surface, A,(Fig. 2)ofthetwo ceramic parts flat to within 0.00025 in. (0.0064 mm)according to good grinding practice using an abrasive passingor finer than a No. 100 (150-m) sieve. Th
10、e 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 practice, and shall be free fromobvious defects. In the results of the tes
11、t, 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 suitable means. Dye check the twoceramic parts and inspect them for flaws (No
12、te 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.6.1.2 Metallized CoatingMetallize the specimen halvesunder identical conditions, that is, temperature, atmosphere,etc. The type of
13、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, silkscreen, brush, spray, roller, etc., but should be reported.1This test method is
14、under the jurisdiction of ASTM Committee F01 onElectronics and is the direct responsibility of Subcommittee F01.03 on MetallicMaterials, Wire Bonding, and Flip Chip.Current edition approved May 1, 2016. Published May 2016. Originallyapproved in 1961 as F19 61 T. Last previous edition approved in 201
15、1 as F19 11. DOI: 10.1520/F0019-11R16.2For 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 ASTM website.Copyright ASTM Internat
16、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1NOTE 2A typical metallizing procedure is described in the Appendix.NOTE 1Tolerance on all dimensions shown, 60.016 in. (0.41 mm).FIG. 1 Self Aligning Grip for Tension TestASeal surface area to be metalized.BSu
17、rface inscribed with date as to ceramic batch and firing temperature.CGripping shoulder.FIG. 2 Ceramic Half of Tension Test SpecimenF19 11 (2016)26.1.3 Assembling the Test SpecimenPlace the two matingparts in a suitable jig to achieve axial alignment of the matedceramic halves and alignment of the m
18、etallized surfaces.Accurate alignment, which is essential to attain uniform testresults, 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 avertical position. In the test results, repor
19、t the brazing materialused; such as copper-silver eutectic, copper-gold alloy, 35 to65 %, etc. Use sufficient material to produce an even fillet atthe joint. Load the assembly to produce pressure on the sealduring the brazing operation and report the weight of the load.7. Procedure7.1 Leak TestThe b
20、razed test specimen may be vacuum-leak checked on any conventional helium spectrometer-typeleak checker with a sensitivity of 5 109cc/s at (5 109mL/s) at standard temperature and pressure. Subject the speci-men continuously to an atmosphere of helium for12 to 5 min.The leak-checking instrument, set
21、at maximum sensitivity,shall show no indication of a leak during the test period.7.2 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 under the same loading r
22、ate which,although optional, shall be reported.7.3 Other Tests Brazed assemblies prepared in accordancewith Section 5 can also be used to:7.3.1 Test ceramic-metal seals with a metal washer insertedbetween the test pieces, and7.3.2 Perform environmental tests such as heat shock, oxi-dation resistance
23、, and bakeout, to determine either the point ofvacuum failure or the tensile strength at vacuum failure.8. Calculation8.1 Calculate the tensile strength by dividing the maximumload on the specimen during the tension test by the originalcross-sectional area. Consider only those specimens that breakin
24、 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.9. Report9.1 Report the following information:9.1.1
25、Method of manufacture of the specimen components,9.1.2 Test surface area of each specimen component,9.1.3 Method of metallizing specimen,9.1.4 Brazing material used,9.1.5 Load applied to specimen during brazing,9.1.6 Results of leak test,9.1.7 Loading rate of tension test,9.1.8 Tensile strength in p
26、ounds per square inch, and9.1.9 Results of other tests performed in addition to leak andtension tests.10. Precision and Bias10.1 PrecisionIt is not possible to specify the precision ofTest Method F19 for measuring the tensile strength or leak rateof metallized ceramic seals because and interlaborato
27、ry studyutilizing these methods has not been conducted.10.2 BiasNo information can be presented on the bias ofthe procedures in Test Method F19 for measuring tensilestrength of leak rate of metallized ceramic seals because nospecimens having an accepted reference value (traceable to anational standa
28、rds laboratory) are available.11. Keywords11.1 brazing; leak rate test; metallized ceramic seals; ten-sion testingAPPENDIX(Nonmandatory Information)X1. TYPICAL METALLIZING PROCEDUREX1.1 ScopeX1.1.1 This procedure is intended to serve as a guide forthose not familiar with ceramic metallizing techniqu
29、es. 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 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
30、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 1MaterialACX Graphite.FIG. 3 Alignment Jig for Brazing Tension Test SpecimenF19 11 (2016)3NOTE X1.1A satisfactory dye is Rhodamine B, 50 % concentratedsolution,
31、 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
32、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
33、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
34、) deionized water, and oven dry.X1.5 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 components in a 1-qt. (1-L) ball mill, andgrind with alumina balls for 100 h.X1.5.3 Mount the speci
35、men 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 coated in one operation.Keep the paint well stirred while painting. After painting airdry the specimen.
36、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 dew point to prevent reduction of the ceramic.X1.6.2 Fire the specimen for 30 min at 1500 to 1525C
37、 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 Table X1.2.X1.7 PlatingX1.7.1 To facilitate brazing with commercially availablealloys, plate the meta
38、lized specimens to a thickness of 0.013mm with nickel. A suitable plating bath (Note X1.2)isasfollows:Material QuantityNickel chloride (NiCl2) 300 g/LBoric acid (H3BO3)30g/LpHA3.0AAdjust the pH with pure hydrochloric acid (HCl).NOTE X1.2Use pure nickel anodes. Operate the bath at 60C(approximate).X1
39、.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 dry.ASTM International takes no position respecting the validity of any patent rights asserted in connection wit
40、h 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 techn
41、ical 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 or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful considerati
42、on at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Har
43、bor 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 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www
44、.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ X1.1 Typical Metallization Coating MixtureMaterial QuantityMolybdenum metal powder, fine, passing No. 200 (75-m) sieve, g
45、 200Manganese metal powder, fine, passing No. 200 (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 minF19 11 (2016)4
