ASTM B963-2013 Standard Test Methods for Oil Content Oil-Impregnation Efficiency and Interconnected Porosity of Sintered Powder Metallurgy (PM) Products Using Archimedes&rsquo Prin.pdf

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1、Designation: B963 11B963 13Standard Test Methods forOil Content, Oil-Impregnation Efficiency, and InterconnectedPorosity of Sintered Powder Metallurgy (PM) ProductsUsing Archimedes Principle1This standard is issued under the fixed designation B963; the number immediately following the designation in

2、dicates 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.1. Scope Scope*1.1 This standard describes three rel

3、ated 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 Determination of the efficiency of the oil-impregnation process.1.1.3 Determination of the percent interco

4、nnected porosity by oil impregnation.1.2 The values stated With the exception of the values for density and the mass used to determine density, for which the useof the gram per cubic centimetre (g/cm3in SI) and gram (g) units is the long-standing industry practice, the values in inch-poundunits are

5、to be regarded as the standard. The values given in parentheses are converted in accordance with IEEE/ASTM SI 10 andare for information only.mathematical conversions to SI units that are provided for information only and are not consideredstandard.1.3 This standard does not purport to address all of

6、 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 Terminology of Powder

7、 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 StatisticsE691

8、 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 IEEE/ASTM Standard:SI 10 American National Standard for Use of the International System of Units (SI): The Modern Metric System3. Terminology3.1 Definitions of powder metallurgy (PM) terms can be found i

9、n Terminology B243. Additional descriptive material isavailable in the Related Material section of Vol. 02.05 of the Annual 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 the

10、specimen is reweighed. The test specimen is then weighed when immersed in water and its volume calculated based onArchimedes 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 Product

11、s and are the direct responsibility of SubcommitteeB09.04 on Bearings.Current edition approved May 1, 2011April 1, 2013. Published May 2011June 2013. Last prefiousOriginally approved in 2008. Last previous edition approved in 20082011as B96308. DOI: 10.1520/B0963-11. 11. DOI: 10.1520/B0963-13.2 For

12、referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book 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 provi

13、de the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the s

14、tandard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright 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

15、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 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 r

16、esult as a percentage.4.4 The volume percentage of interconnected porosity (as measured by oil impregnation) is then calculated based on the amountof oil in the fully oil-impregnated specimen.5. Significance and Use5.1 Oil content values are generally contained in specifications for oil-impregnated

17、PM bearings.5.2 The oil-impregnation efficiency provides an indication of how well the as-received parts had been impregnated.5.3 The desired self-lubricating performance of PM bearings requires a minimum amount of interconnected porosity andsatisfactory oil impregnation of the interconnected porosi

18、ty. A minimum oil content is specified.5.4 The results from these test methods may be used for quality control or compliance purposes.6. Apparatus6.1 Analytical BalancePrecision single-pan balance that will permit readings within 0.01 %0.01% of the test specimen mass.See Table 1.6.2 Water ContainerA

19、 glass beaker or other suitable transparent container should be used to contain the 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

20、 of a size that the level of the water does not rise more than2.5 mm (0.10 in.)0.10 in. (2.5 mm) when 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 3

21、Degassing the water by evacuation, boiling, or ultrasonic agitation helps to prevent air bubbles from 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 aroun

22、d the test specimen or the test specimen may be supported in a wire basket that is attached to the suspension 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 recomme

23、nded diameter of suspension wire to be used for various massranges is shown in Table 2.NOTE 4For the 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 impregna

24、te the parts originally.6.5.1 If parts are not already impregnated, oil with a viscosity of 20 to 65 cSt or 100 to 300 SSU (20 10-6 to 65 10-6 m2/s(20 to 65 cSt or 100 to 300 SSU) at 38 C (100 F) /s) at 100 F (38 C) has been found to be suitable.6.6 Vacuum Impregnation ApparatusEquipment for impregn

25、ation of the part or test specimen with oil.6.7 ThermometerA thermometer with an accuracy of 0.5 C (1 F) 1 F (0.5 C) to measure the temperature of the water.6.8 Soxhlet ApparatusGlass laboratory unit consisting of a condenser, extractor, filter, flask with a suitable solvent for the oilsuch as petro

26、leum 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 combined to reach the minimum mass.7.2 Thoroughly wipe clean all surfaces of the test specimen to remove any adhering foreign materials

27、 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 recommended to remove all rough surfaces.TABLE 1 Balance SensitivityMass,gBalance Sensitivity,gless than 10 0.000110 to less than 100 0.0

28、01100 to less than 1000 0.011000 to less than 10 000 0.1B963 1328. Procedure8.1 It is important that the part or test specimen, the analytical balance and surrounding air be at a uniform temperature whenweighing is performed.8.2 For the most precise volume determinations, duplicate weighings should

29、be made for all mass measurements. The analyticalbalance should be adjusted to zero prior to each weighing. Duplicate mass determinations should be averaged before performingany calculations.8.3 For improved repeatability and reproducibility, the analytical balance should be verified periodically wi

30、th a standard massthat is approximately equal to the part or test specimen mass.8.4 Determination of Oil Content, Oil-Impregnation Effciency, and Interconnected 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 th

31、e precision stated in Table 1.FIG. 1 Methods for Holding the Test Specimen When Weighing in WaterTABLE 2 Maximum Recommended Wire DiametersMass,gWire Diameter,mm (in.)less than 50 0.12 (0.005)50 to less than 200 0.25 (0.010)200 to less than 600 0.40 (0.015)600 and greater 0.50 (0.020)TABLE 2 Maximum

32、 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 1338.4.2 Oil impregnate the as-received part or test specimen using one of the following procedures:Vacuum Oil Impregnatio

33、nPreferred Procedure8.4.3 Immerse the part or test specimen in oil at room temperature.8.4.4 Reduce the pressure over the sample to 7 kPa (1 psi)1 psi (7 kPa) or less for 30 minutes, then increase the pressure backto atmospheric pressure and keep the sample immersed for at least 30 minutes.8.4.5 Rem

34、ove excess oil by wiping gently with an absorbent, 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 Impregna

35、tionAlternative Procedure8.4.8 Immerse the part or test specimen in oil at a temperature of 82 6 5 C (180 6 10 F) 180 6 10 F (82 6 5 C) for atleast 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

36、 by wiping gently with an absorbent, lint-free material. Take care not 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 o

37、il-impregnated part or test specimen to the precision stated in Table 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 contai

38、ner of water may also be supported below thebalance for weighing larger 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.FIG. 2 Methods for Weighing in WaterB963 134

39、8.4.15 Suspend the test specimen support along with the part or test specimen from the beam hook of the balance. The watershould cover any wire twists and the specimen support basket by at least 6 mm (14 in.)in. (6 mm) to minimize the effect of surfacetension forces on the weighing.8.4.16 The test s

40、pecimen support and test specimen shall hang freely from the balance beam hook, be free of air bubbles whenimmersed in the water, 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 specim

41、en support immersed in water. This is mass C.8.4.19 Remove the part/test specimen from the support.8.4.20 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 be

42、low its normal hanging depth, as a change in depthwill change the measured mass.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

43、 with the specimen, before weighing the specimen support and part/testspecimen immersed 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 nearest1 C (2 F) 2 F (1 C) and record its

44、 density w, at that temperature, from Table 3.8.4.22 Remove the oil from the part or test 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 h

45、eating the part or test specimen to 20 C (36 F) 36 F (20 C)above the boiling point of the selected solvent.8.4.24 Continue to alternate extraction and drying until the mass of the part or test specimen is constant to within 0.05 %.0.05%.Weigh the part to the precision stated in Table 1 to determine

46、the dry mass. This is mass A.TABLE 3 Effect of Temperature on the Density of Air-Free WaterATemperature DensityC (F) g/cm315 (59.0) 0.999116 (60.8) 0.998917 (62.6) 0.998818 (64.4) 0.998619 (66.2) 0.998420 (68.0) 0.998221 (69.8) 0.998022 (71.6) 0.997823 (73.4) 0.997524 (75.2) 0.997325 (77.0) 0.997026

47、 (78.8) 0.996827 (80.6) 0.996528 (82.4) 0.996229 (84.2) 0.995930 (86.0) 0.9956TABLE 3 Effect of Temperature 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) 0.99787

48、3.4 (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 1358.4.25 Apractical and fast method of

49、 oil removal for most materials consists of heating the part or test specimen in a protectiveatmosphere to a temperature in the range of 430 to 870 C (800 to 1600 F). 800 to 1600 F (430 to 870 C). The method isapplicable only if metallurgical properties are not a point of concern and all concerned parties agree upon its use.NOTE 6The selection of the appropriate temperature is very important and care should be taken not to exceed the melting point of any material thatis tested. For example, 815 to 870 C (1500 to 160