ASTM B963-2008 Standard Test Methods for Oil Content Oil-Impregnation Efficiency and Interconnected Porosity of Sintered Powder Metallurgy (PM) Products Using Archimedes&x2019 Prin.pdf

1、Designation: B 963 08Standard Test Methods forOil Content, Oil-Impregnation Efficiency, and InterconnectedPorosity of Sintered Powder Metallurgy (PM) ProductsUsing Archimedes Principle1This standard is issued under the fixed designation B 963; the number immediately following the designation indicat

2、es 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. Scope1.1 This standard describes three related test me

3、thods thatcover the measurement of physical properties of oil-impregnated powder metallurgy products.1.1.1 Determination of the volume percent of oil containedin the material.1.1.2 Determination of the efficiency of the oil-impregnation process.1.1.3 Determination of the percent interconnected poros

4、ityby oil impregnation.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are converted in accor-dance with IEEE/ASTM SI 10 and are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its us

5、e. 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:2B 243 Terminology of Powder MetallurgyD 1217 Test Method for Density and Re

6、lative Density(Specific Gravity) of Liquids by Bingham PycnometerD 1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer Method2.2 IEEE/ASTM Standard:SI 10 American National Standard for Use of the Interna-tiona

7、l System of Units (SI): The Modern Metric System3. Terminology3.1 Definitions of powder metallurgy (PM) terms can befound in Terminology B 243. Additional descriptive material isavailable in the Related Material section of Vol. 02.05 of theAnnual Book of ASTM Standards.4. Summary of Test Method4.1 T

8、he part or test specimen is first weighed in air. It is thenoil impregnated to fill the surface-connected porosity and thespecimen is reweighed. The test specimen is then weighedwhen immersed in water and its volume calculated based onArchimedes principle. The oil is then removed and thespecimen is

9、reweighed.4.2 The oil content of an oil-impregnated part or testspecimen is then calculated as a percentage of the volume ofthe specimen. This may be done for the as-received and thefully oil-impregnated specimen.4.3 The oil-impregnation effciency is calculated by dividingthe as-received oil content

10、 by the fully impregnated oil contentand expressing the result as a percentage.4.4 The volume percentage of interconnected porosity (asmeasured by oil impregnation) is then calculated based on theamount of oil in the fully oil-impregnated specimen.5. Significance and Use5.1 Oil content values are ge

11、nerally contained in specifica-tions for oil-impregnated PM bearings.5.2 The oil-impregnation efficiency provides an indicationof how well the as-received parts had been impregnated.5.3 The desired self-lubricating performance of PM bear-ings requires a minimum amount of interconnected porosityand s

12、atisfactory oil impregnation of the interconnected poros-ity. A minimum oil content is specified.5.4 The results from these test methods may be used forquality control or compliance purposes.6. Apparatus6.1 Analytical BalancePrecision single-pan balance thatwill permit readings within 0.01 % of the

13、test specimen mass.See Table 1.6.2 Water ContainerA glass beaker or other suitabletransparent container should be used to contain the water.NOTE 1A transparent container makes it easier to see air bubblesadhering to the test specimen and specimen support when immersed inwater.1These test methods are

14、 under the jurisdiction of ASTM Committee B09 onMetal Powders and Metal Powder Products and are the direct responsibility ofSubcommittee B09.04 on Bearings.Current edition approved Nov. 1, 2008. Published December 2008.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact A

15、STM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 2For the most precise

16、determination, the water containershould be of a size that the level of the water does not rise more than2.5 mm (0.10 in.) when the test specimen is lowered into the water.6.3 WaterDistilled or deionized water to which 0.05 to 0.1volume percent of a wetting agent has been added to reduce theeffects

17、of surface tension.NOTE 3Degassing the water by evacuation, boiling, or ultrasonicagitation helps to prevent air bubbles from collecting on the test specimenand support when immersed in water.6.4 Test Specimen Support for Weighing in WaterTwotypical arrangements are shown in Fig. 1. The suspension w

18、iremay be twisted around the test specimen or the test specimenmay be supported in a wire basket that is attached to thesuspension wire. For either arrangement, a single corrosion-resistant wirefor example, austenitic stainless steel, copper,or nichromeshall be used for the basket and suspension wir

19、e.The maximum recommended diameter of suspension wire tobe used for various mass ranges is shown in Table 2.NOTE 4For the most precise determinations, it is important that themass and volume of all supporting wires immersed in water be minimized.6.5 Oil for Oil-ImpregnationThe same type of oil that

20、wasused to impregnate the parts originally.6.5.1 If parts are not already impregnated, oil with aviscosity of 20 3 10-6to 65 3 10-6m2/s (20 to 65 cSt or 100to 300 SSU) at 38 C (100 F) has been found to be suitable.6.6 Vacuum Impregnation ApparatusEquipment for im-pregnation of the part or test speci

21、men with oil.6.7 ThermometerA thermometer with an accuracy of0.5 C (1 F) to measure the temperature of the water.6.8 Soxhlet ApparatusGlass laboratory unit consisting ofa condenser, extractor, filter, flask with a suitable solvent forthe oil such as petroleum ether, and a heating mantle.7. Preparati

22、on 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 reachthe minimum mass.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 0

23、00 0.1FIG. 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)B9630827.2 Thoroughly wipe clean all su

24、rfaces of the test specimento remove any adhering foreign materials such as dirt or oxidescale.7.3 Take care with cut specimens to avoid rough surfaces towhich an air bubble may adhere.A100-grit sanding or abrasivegrinding is recommended to remove all rough surfaces.8. Procedure8.1 It is important t

25、hat the part or test specimen, theanalytical balance and surrounding air be at a uniform tem-perature when weighing is performed.8.2 For the most precise volume determinations, duplicateweighings should be made for all mass measurements. Theanalytical balance should be adjusted to zero prior to each

26、weighing. Duplicate mass determinations should be averagedbefore performing any calculations.8.3 For improved repeatability and reproducibility, the ana-lytical balance should be verified periodically with a standardmass that is approximately equal to the part or test specimenmass.8.4 Determination

27、of Oil Content, Oil-Impregnation Eff-ciency, and Interconnected Porosity:8.4.1 Determine the mass of the as-received part or testspecimen. This is mass J. This and all subsequent weighingsshall be to the precision stated in Table 1.8.4.2 Oil impregnate the as-received part or test specimenusing one

28、of the following procedures:Vacuum Oil ImpregnationPreferred Procedure8.4.3 Immerse the part or test specimen in oil at roomtemperature.8.4.4 Reduce the pressure over the sample to 7 kPa (1 psi)or less for 30 minutes, then increase the pressure back toatmospheric pressure and keep the sample immerse

29、d for atleast 30 minutes.8.4.5 Remove excess oil by wiping gently with an absor-bent, lint-free material. Take care not to extract oil absorbedwithin the part or test specimen.8.4.6 Do not place or store parts on porous surfaces such aspaper, cloth, or cardboard as these will absorb oil.8.4.7 Procee

30、d to 8.4.13.Immersion Oil ImpregnationAlternative Procedure8.4.8 Immerse the part or test specimen in oil at a tempera-ture of 82 6 5 C (180 6 10 F) for at least 4 hours.8.4.9 Cool by immersing in a bath of the same oil held atroom temperature and keep in this oil for at least 30 minutes.8.4.10 Remo

31、ve excess oil by wiping gently with an absor-bent, lint-free material. Take care not to extract oil absorbedwithin the part or test specimen.8.4.11 Do not place or store parts on porous surfaces such aspaper, cloth, or cardboard as these will absorb oil.8.4.12 Proceed to 8.4.13.8.4.13 Determine the

32、mass of the oil-impregnated part ortest specimen to the precision stated in Table 1. This is mass B.8.4.14 Support the container of water over the pan of thebalance using a suitable bridge as shown in Fig. 2a. Take careto ensure that the bridge does not restrict the free movement ofthe balance pan.

33、The container of water may also be supportedbelow the balance for weighing larger specimens if the balancehas a lower beam hook for this purpose. See Fig. 2b. If thisarrangement is used, shield the weighing system, including thewire, from the effect of air drafts.8.4.15 Suspend the test specimen sup

34、port along with thepart or test specimen from the beam hook of the balance. Thewater should cover any wire twists and the specimen supportbasket by at least 6 mm (14 in.) to minimize the effect ofsurface tension forces on the weighing.8.4.16 The test specimen support and test specimen shallhang free

35、ly from the balance beam hook, be free of air bubbleswhen immersed in the water, and be at the same temperature asthe water and the balance.8.4.17 The surface of the water shall be free of dustparticles.8.4.18 Weigh the part/test specimen and specimen supportimmersed in water. This is mass C.8.4.19

36、Remove the part/test specimen from the support.8.4.20 Weigh the test specimen support immersed in waterat the same depth as before. This is mass E. The suspensionsupport shall be free of air bubbles and the suspension wireshall not be immersed below its normal hanging depth, as achange in depth will

37、 change the measured mass.NOTE 5Some balances are capable of being tared. This automaticallyremoves the necessity of reweighing the specimen support every time. Inthis case, tare the specimen support alone, immersed in water to the samedepth as with the specimen, before weighing the specimen support

38、 andpart/test specimen immersed in water. The mass of the specimen supportand specimen immersed in water is mass F, which replaces mass C minusmass E.8.4.21 Measure the temperature of the water to the nearest1 C (2 F) and record its density rw, at that temperature, fromTable 3.8.4.22 Remove the oil

39、from the part or test specimen in aSoxhlet apparatus using a solvent such as toluene or petroleumether in order to determine the dry mass of the part or testspecimen.8.4.23 After extraction of the oil, remove residual solventby heating the part or test specimen to 20 C (36 F) above theboiling point

40、of the selected solvent.8.4.24 Continue to alternate extraction and drying until themass of the part or test specimen is constant to within 0.05 %.Weigh the part to the precision stated in Table 1 to determinethe dry mass. This is mass A.8.4.25 A practical and fast method of oil removal for mostmate

41、rials consists of heating the part or test specimen in aprotective atmosphere to a temperature in the range of 430 to870 C (800 to 1600 F). The method is applicable only ifmetallurgical properties are not a point of concern and allconcerned parties agree upon its use.NOTE 6The selection of the appro

42、priate temperature is very importantand care should be taken not to exceed the melting point of any materialthat is tested. For example, 815 to 870 C (1500 to 160 F) for bronze,depending on the sintering temperature that was used; and 540 C(1000 F) should not be exceeded for aluminum alloys.8.4.26 I

43、f the oil density is not already known, determine thedensity of the oil that was used to impregnate the part or testB963083specimen in accordance with Test Method D 1217 or TestMethod D 1298. This density is ro.NOTE 7The typical density of petroleum-type lubricants is0.880 g/cm3and for synthetic lub

44、ricants it ranges from 0.910 to 1.000g/cm3.9. CalculationAs-Received Oil Content9.1 Calculate the as-received oil content (volume %) fromthe following formula:As2received oil content P1volume %!5 (1)SJ AB C E! ro3 100DrworSJ AB F! ro3 100Drw(2)where:P1= as-received oil content by volume, %,J = the m

45、ass of as-received part/test specimen, g,B = the mass of oil-impregnated part/test specimen, g,C = mass of the oil-impregnated part/test specimen andspecimen support immersed in water, g,E = the mass of the oil-impregnated part/test specimensupport immersed in water, g,F = the mass of the oil-impreg

46、nated part/test specimen inwater with the mass of the specimen support tared, g,A = the mass of the oil-free part/test specimen, g,FIG. 2 Methods for Weighing in WaterTABLE 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

47、) 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 (78.8) 0.996827 (80.6) 0.996528 (82.4) 0.996229 (84.2) 0.995930 (86.0) 0.9956AMetrological Handbook 145, “Quality Assurance for Measurements,” NationalInstitute

48、of Standards and Technology, 1990, pp. 9-10.B963084ro= the density of the oil used to impregnate the part/testspecimen, g/cm3, andrw= the density of the water, g/cm3.Fully Impregnated Oil Content9.2 Calculate the fully impregnated oil content (volume %)from the following formula:Fully impregnated oi

49、l content P1volume %!5 (3)SB AB C E! ro3 100DrworSB AB F! ro3 100Drw(4)Oil-Impregnation Efficiency9.3 Calculate the oil impregnation efficiency (%) from thefollowing formula:Oil impregnation efficiency, %!5P1/P! 3 100 (5)Interconnected Porosity9.4 Calculate the interconnected porosity (based on theextent of oil impregnation) as follows:Interconnected Porosity, P volume %!5 (6)SB AB C E! ro3 100DrworSB AB F! ro3 100Drw(7)10. Report10.1 Report the method used for oil impregnation and thefollowing to the