1、Designation: B963 13B963 14Standard Test Methods forOil Content, Oil-Impregnation Efficiency, andInterconnectedSurface-Connected Porosity of SinteredPowder Metallurgy (PM) Products Using ArchimedesPrinciple1This standard is issued under the fixed designation B963; the number immediately following th
2、e designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for
3、use by agencies of the U.S. Department of Defense.1. Scope*1.1 This standard describes three related test methods that cover the measurement of physical properties of oil-impregnatedpowder metallurgy products.1.1.1 Determination of the volume percent of oil contained in the material.1.1.2 Determinat
4、ion of the efficiency of the oil-impregnation process.1.1.3 Determination of the percent interconnectedsurface-connected porosity by oil impregnation.1.2 With the exception of the values for density and the mass used to determine density, for which the use of the gram per cubiccentimetre (g/cm3) and
5、 gram (g) units is the long-standing industry practice, the values in inch-pound units are to be regarded asstandard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and arenot considered standard.1.3 This standard does not purport to a
6、ddress all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2B243 Terminol
7、ogy of Powder MetallurgyD1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham PycnometerD1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products byHydrometer MethodE456 Terminology Relating to Quality and S
8、tatisticsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions of powder metallurgy (PM) terms can be found in Terminology B243. Additional descriptive material isavailable in the Related Material section of Vol. 02.05 of the A
9、nnual Book of ASTM Standards.4. Summary of Test Method4.1 The part or test specimen is first weighed in air. It is then oil impregnated to fill the surface-connected porosity and thespecimen is reweighed. The test specimen is then weighed when immersed in water and its volume calculated based onArch
10、imedes principle. The oil is then removed and the specimen is reweighed.1 These test methods are under the jurisdiction ofASTM Committee B09 on Metal Powders and Metal Powder Products and are the direct responsibility of SubcommitteeB09.04 on Bearings.Current edition approved April 1, 2013Sept. 1, 2
11、014. Published June 2013September 2014. Originally approved in 2008. Last previous edition approved in 20112013 asB963 11.13. DOI: 10.1520/B0963-13.10.1520/B0963-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Boo
12、k of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be techni
13、cally possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this s
14、tandardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 The oil content of an oil-impregnated part or test specimen is then calculated as a percentage of the volume of the specimen.This may be done for the as-received and the fully
15、 oil-impregnated specimen.4.3 The oil-impregnation effciency is calculated by dividing the as-received oil content by the fully impregnated oil content andexpressing the result as a percentage.4.4 The volume percentage of interconnectedsurface-connected porosity (as measured by oil impregnation) is
16、then calculatedbased on the amount of oil in the fully oil-impregnated specimen.5. Significance and Use5.1 Oil content values are generally contained in specifications for oil-impregnated PM bearings.5.2 The oil-impregnation efficiency provides an indication of how well the as-received parts had bee
17、n impregnated.5.3 The desired self-lubricating performance of PM bearings requires a minimum amount of interconnectedsurface-connectedporosity and satisfactory oil impregnation of the interconnectedsurface-connected porosity. A minimum oil content is specified.5.4 The results from these test methods
18、 may be used for quality control or compliance purposes.6. Apparatus6.1 Analytical BalancePrecision single-pan balance that will permit readings within 0.01% of the test specimen mass. SeeTable 1.6.2 Water ContainerA glass beaker or other suitable transparent container should be used to contain the
19、water.NOTE 1A transparent container makes it easier to see air bubbles adhering to the test specimen and specimen support when immersed in water.NOTE 2For the most precise determination, the water container should be of a size that the level of the water does not rise more than0.10 in. (2.5 mm) when
20、 the test specimen is lowered into the water.6.3 WaterDistilled or deionized water to which 0.05 to 0.1 volume percent of a wetting agent has been added to reduce theeffects of surface tension.NOTE 3Degassing the water by evacuation, boiling, or ultrasonic agitation helps to prevent air bubbles from
21、 collecting on the test specimen andsupport when immersed in water.6.4 Test Specimen Support for Weighing in WaterTwo typical arrangements are shown in Fig. 1. The suspension wire may betwisted around the test specimen or the test specimen may be supported in a wire basket that is attached to the su
22、spension wire.For either arrangement, a single corrosion-resistant wirefor example, austenitic stainless steel, copper, or nichromeshall beused for the basket and suspension wire. The maximum recommended diameter of suspension wire to be used for various massranges is shown in Table 2.NOTE 4For the
23、most precise determinations, it is important that the mass and volume of all supporting wires immersed in water be minimized.6.5 Oil for Oil-ImpregnationThe same type of oil that was used to impregnate the parts originally.6.5.1 If parts are not already impregnated, oil with a viscosity of 20 to 65
24、cSt or 100 to 300 SSU (20 10-6 to 65 10-6 m2/s)at 100 F (38 C) has been found to be suitable.6.6 Vacuum Impregnation ApparatusEquipment for impregnation of the part or test specimen with oil.6.7 ThermometerA thermometer with an accuracy of 1 F (0.5 C) to measure the temperature of the water.6.8 Soxh
25、let ApparatusGlass laboratory unit consisting of a condenser, extractor, filter, flask with a suitable solvent for the oilsuch as petroleum ether, and a heating mantle.7. Preparation of Test Specimens7.1 The mass of the test specimen shall be a minimum of1.0 g. For small parts, several parts may be
26、combined to reach the minimum mass.7.2 Thoroughly wipe clean all surfaces of the test specimen to remove any adhering foreign materials such as dirt or oxide scale.7.3 Take care with cut specimens to avoid rough surfaces to which an air bubble may adhere. A 100-grit sanding or abrasivegrinding is re
27、commended to remove all rough surfaces.TABLE 1 Balance SensitivityMass,gBalance Sensitivity,gless than 10 0.000110 to less than 100 0.001100 to less than 1000 0.011000 to less than 10 000 0.1B963 1428. Procedure8.1 It is important that the part or test specimen, the analytical balance and surroundin
28、g air be at a uniform temperature whenweighing is performed.8.2 For the most precise volume determinations, duplicate weighings should be made for all mass measurements. The analyticalbalance should be adjusted to zero prior to each weighing. Duplicate mass determinations should be averaged before p
29、erformingany calculations.8.3 For improved repeatability and reproducibility, the analytical balance should be verified periodically with a standard massthat is approximately equal to the part or test specimen mass.8.4 Determination of Oil Content, Oil-Impregnation Effciency, and InterconnectedSurfa
30、ce-Connected Porosity:8.4.1 Determine the mass of the as-received part or test specimen. This is mass J. This and all subsequent weighings shall beto the precision stated in Table 1.8.4.2 Oil impregnate the as-received part or test specimen using one of the following procedures:Vacuum Oil Impregnati
31、onPreferred Procedure8.4.3 Immerse the part or test specimen in oil at room temperature.8.4.4 Reduce the pressure over the sample to 1 psi (7 kPa) or less for 30 minutes, then increase the pressure back to atmosphericpressure and keep the sample immersed for at least 30 minutes.FIG. 1 Methods for Ho
32、lding the Test Specimen When Weighing in WaterTABLE 2 Maximum Recommended Wire DiametersMass,gWire Diameter,in. (mm)less than 50 0.005 (0.12)50 to less than 200 0.010 (0.25)200 to less than 600 0.015 (0.40)600 and greater 0.020 (0.50)B963 1438.4.5 Remove excess oil by wiping gently with an absorbent
33、, lint-free material. Take care not to extract oil absorbed within thepart or test specimen.8.4.6 Do not place or store parts on porous surfaces such as paper, cloth, or cardboard as these will absorb oil.8.4.7 Proceed to 8.4.13.Immersion Oil ImpregnationAlternative Procedure8.4.8 Immerse the part o
34、r test specimen in oil at a temperature of 180 6 10 F (82 6 5 C) for at least 4 hours.8.4.9 Cool by immersing in a bath of the same oil held at room temperature and keep in this oil for at least 30 minutes.8.4.10 Remove excess oil by wiping gently with an absorbent, lint-free material. Take care not
35、 to extract oil absorbed withinthe part or test specimen.8.4.11 Do not place or store parts on porous surfaces such as paper, cloth, or cardboard as these will absorb oil.8.4.12 Proceed to 8.4.13.8.4.13 Determine the mass of the oil-impregnated part or test specimen to the precision stated in Table
36、1. This is mass B.8.4.14 Support the container of water over the pan of the balance using a suitable bridge as shown in Fig. 2a. Take care to ensurethat the bridge does not restrict the free movement of the balance pan. The container of water may also be supported below thebalance for weighing large
37、r specimens if the balance has a lower beam hook for this purpose. See Fig. 2b. If this arrangement isused, shield the weighing system, including the wire, from the effect of air drafts.8.4.15 Suspend the test specimen support along with the part or test specimen from the beam hook of the balance. T
38、he watershould cover any wire twists and the specimen support basket by at least 14 in. (6 mm) to minimize the effect of surface tensionforces on the weighing.8.4.16 The test specimen support and test specimen shall hang freely from the balance beam hook, be free of air bubbles whenimmersed in the w
39、ater, and be at the same temperature as the water and the balance.8.4.17 The surface of the water shall be free of dust particles.8.4.18 Weigh the part/test specimen and specimen support immersed in water. This is mass C.8.4.19 Remove the part/test specimen from the support.FIG. 2 Methods for Weighi
40、ng in WaterB963 1448.4.20 Weigh the test specimen support immersed in water at the same depth as before. This is mass E. The suspension supportshall be free of air bubbles and the suspension wire shall not be immersed below its normal hanging depth, as a change in depthwill change the measured mass.
41、NOTE 5Some balances are capable of being tared. This automatically removes the necessity of reweighing the specimen support every time. In thiscase, tare the specimen support alone, immersed in water to the same depth as with the specimen, before weighing the specimen support and part/testspecimen i
42、mmersed in water. The mass of the specimen support and specimen immersed in water is mass F, which replaces mass C minus mass E.8.4.21 Measure the temperature of the water to the nearest2 F (1 C) and record its density w, at that temperature, from Table 3.8.4.22 Remove the oil from the part or test
43、specimen in a Soxhlet apparatus using a solvent such as toluene or petroleum etherin order to determine the dry mass of the part or test specimen.8.4.23 After extraction of the oil, remove residual solvent by heating the part or test specimen to 36 F (20 C) above the boilingpoint of the selected sol
44、vent.8.4.24 Continue to alternate extraction and drying until the mass of the part or test specimen is constant to within 0.05%. Weighthe part to the precision stated in Table 1 to determine the dry mass. This is mass A.8.4.25 Apractical and fast method of oil removal for most materials consists of
45、heating the part or test specimen in a protectiveatmosphere to a temperature in the range of 800 to 1600 F (430(425 to 870 C). The method is applicable only if metallurgicalproperties are not a point of concern and all concerned parties agree upon its use.NOTE 6The selection of the appropriate tempe
46、rature is very important and care should be taken not to exceed the melting point of any material thatis tested. For example, 1500 to 1600 F (815 to 870 C) for bronze, depending on the sintering temperature that was used; and 1000 F(540 C) should not be exceeded for aluminum alloys.8.4.26 If the oil
47、 density is not already known, determine the density of the oil that was used to impregnate the part or testspecimen in accordance with Test Method D1217 or Test Method D1298. This density is o.NOTE 7The typical density of petroleum-type lubricants is0.880 g/cm3 and for synthetic lubricants it range
48、s from 0.910 to 1.000 g/cm3.9. CalculationAs-Received Oil Content9.1 Calculate the as-received oil content (volume %) from the following formula:As2received oil content P1 volume %!5 (1)S J 2AB2C 2E! o3100DworS J 2AB2F! o3100Dw (2)where:P1 = as-received oil content by volume, %,TABLE 3 Effect of Tem
49、perature on the Density of Air-Free WaterATemperature DensityF (C) g/cm359.0 (15) 0.999160.8 (16) 0.998962.6 (17) 0.998864.4 (18) 0.998666.2 (19) 0.998468.0 (20) 0.998269.8 (21) 0.998071.6 (22) 0.997873.4 (23) 0.997575.2 (24) 0.997377.0 (25) 0.997078.8 (26) 0.996880.6 (27) 0.996582.4 (28) 0.996284.2 (29) 0.995986.0 (30) 0.9956A Metrological Handbook 145, “Quality Assurance for Measurements,” NationalInstitute of Standards and Technology, 1990, pp. 9-10.B963 145J = the mass of as-received part/test specimen, g,B = the m
