ASTM C1350M-1996(2008) Standard Test Method for Measurement of Viscosity of Glass Between Softening Point and Annealing Range (Approximately 108 Pa&183 s to Approximately 10 13 Pa&.pdf

1、Designation: C 1350M 96 (Reapproved 2008)Standard Test Method forMeasurement of Viscosity of Glass Between Softening Pointand Annealing Range (Approximately 108Pas toApproximately 1013Pas) by Beam Bending (Metric)1This standard is issued under the fixed designation C 1350M; the number immediately fo

2、llowing the 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.1. Scope1.1 This test meth

3、od covers the determination of glassviscosity from approximately 108Pas to approximately 1013Pas by measuring the rate of viscous bending of a simplyloaded glass beam.2Due to the thermal history of the glass, theviscosity may not represent conditions of thermal equilibriumat the high end of the meas

4、ured viscosity range. Measurementscarried out over extended periods of time at any temperature orthermal preconditioning will minimize these effects by allow-ing the glass to approach equilibrium structural conditions.Conversely, the method also may be used in experimentalprograms that focus on none

5、quilibrium conditions.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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 stan

6、dard 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:3C 336 Test Method for Annealing Point and Strain Point ofGlass by Fiber ElongationC 338 Test Method for Softening Point of Gla

7、ssC 598 Test Method for Annealing Point and Strain Point ofGlass by Beam BendingC 965 Practice for Measuring Viscosity of Glass Above theSoftening PointC 1351M Test Method for Measurement of Viscosity ofGlass Between 104Pas and 108Pas by Viscous Compres-sion of a Solid Right Cylinder Metric3. Termin

8、ology3.1 Definitions:3.1.1 beam bending viscometera device used to determinethe viscosity of glass from approximately 108Pas to approxi-mately 1013Pas by measuring the deflection rate of a simplysupported beam. The equation for calculating viscosity by thismethod is:h5gL31440 Icdh/dt!FM 1rAL1.6GF1 1

9、asT!31 1agT!4G(1)where:h = viscosity, Pas,M = load (applied load + loading train), gms,dh/dt = midpoint deflection rate of test beam, cm/s,g = acceleration of gravity, 980 cm/s2,Ic= cross-sectional moment of inertia, cm4,r = density of glass, g/cm3,A = cross-sectional area of the beam, cm2,L = suppo

10、rt span, cm, andasand ag= mean coefficient of linear thermal expansionof support stand and glass, respectively, 25Cto temperature of measurement, T, m/m/C.See Note 1.NOTE 1The term (1 + asT)3/(1 + agT)4corrects for thermal expan-sion changes of room temperature dimensions. It can be ignored when asa

11、nd agare approximately equal. A fused silica support stand in combina-tion with a high expansion glass can make this term 3 % in magnitude.Only an estimate of agis required, singe the correction is small. Use 1.5times the room temperature coefficient if data are unavailable.4. Significance and Use4.

12、1 This test method is well suited for measuring theviscosity of glasses in ranges higher than those covered byparallel plate (see Test Method C 1351) and rotational viscom-etry (see Practice C 965) methods. This test method is useful1This test method is under the jurisdiction of ASTM Committee C14 o

13、n Glassand Glass Products and is the direct responsibility of Subcommittee C14.04 onPhysical and Mechanical Properties.Current edition approved April 1, 2008. Published December 2008. Originallyapproved in 1996. Last previous edition approved in 2003 as C 1350M 96 (2003).2Hagy, H. E., “Experimental

14、Evaluation of Beam Bending Method of Deter-mining Glass Viscosities in the Range 108to 1015Poises”, Journal of the AmericanCeramic Society, Vol 46, No. 2, 1963, pp. 9597.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annu

15、al 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.for providing information related to the behavior of glass afterit has been

16、formed into an object of commerce and in researchand development.5. Apparatus5.1 The apparatus shall consist of a furnace, a means ofcontrolling its temperature and heating rate, specimen holdersand loading rod, and a means of observing the rate of viscousdeflection of the glass specimen.5.2 Furnace

17、5.2.1 The furnace shall be electrically heated by resistanceelements. The dimensions and the details of the furnaceconstruction are not critical; its cross-section can be circular of75 mm (;3 in.) diameter or square with sides of 75 mm. Thefurnace should have a constant temperature zone that covers

18、the specimen geometry, including the deflection range. Differ-ences in temperature greater than 2C within that constanttemperature zone are unacceptable.5.3 Temperature Measuring and Indicating Instruments:5.3.1 For the measurement of temperature, there shall beprovided a calibrated Type K, R, or S

19、thermocouple. Thethermocouple shall be housed in a double-bore alumina tubewith its junction placed within 5 mm of the specimen near theaxis of the furnace. The thermocouple shall be referenced to0C by means of an ice bath, and its emf measured with acalibrated potentiometer that can be read with a

20、sensitivity of0.1C and an accuracy of 60.5C. Precautions shall be taken toensure that the ice bath is maintained at 0C throughout thetest. Alternately, the output of the thermocouple can bemeasured on a calibrated, direct reading meter (electronicthermometer) that can be read with a sensitivity of 0

21、1C andan accuracy of 60.5C. See Note 3 for temperature lag-leadcorrections.5.4 Furnace Control:5.4.1 Suitable means shall be provided for maintaining thefurnace temperature at a fixed control point and for controllingthe heating and cooling rates. Commercially available pro-gramming equipment provi

22、des excellent control. A variabletransformer with manual control is an inexpensive, but lessadequate means of accomplishing the required control.5.5 Specimen Holder and Loading Rod:5.5.1 A diagram of the apparatus can be found in TestMethod C 598.5.5.2 A ceramic support stand and a ceramic loading r

23、odshall be provided for supporting the specimen and applying theload to it. The thermal expansion characteristics of bothmembers must be very similar so as to minimize motion of theloading rod due to expansion differences. A rectangular alu-mina muffle or circular tube that can be notched to defines

24、pecimen position is a suitable support stand (see Note 2). Thesupporting surfaces of these notches shall be flat and lie in aplane perpendicular to the axis of the furnace. The inside edgesof these notches define the support span once the specimenbeam starts to deflect. A support span of about 5 cm

25、62 in.)is recommended. A suitable loading rod can be provided by asingle-crystal sapphire rod flame bent at one end in the form ofa shepherds crook.4This crook will contribute to the load onthe specimen, so its weight should be kept to a minimum.NOTE 2Vitreous silica is a suitable material for both

26、 support standand loading rod. It is not recommended for temperatures above 900C.5.6 Extensometer for Measuring Midpoint Deflection:5.6.1 The means for observing the rate of deflection of thespecimen shall allow reliable reading of total deflection of atleast 10 mm. The extensometer shall permit dir

27、ect reading of0.010 mm and estimates of 0.0010 mm. Its accuracy shall besuch that the error of indication will not exceed 62 % for anymeasured deflection. This will limit the minimum deflectionthat may be used in calculation. A linearly variable differentialtransformer (LVDT) is suitable for this pu

28、rpose, as is any otherdevice (for example, optical or capacitive), provided thatdeflection is reliably measured as specified.5.7 Weights:5.7.1 A set of weights spanning the range from 1 to 500 gand accurate to 0.1 % relative is required.5.8 Micrometre Calipers:5.8.1 Micrometre calipers which can be

29、read to an accuracyof at least 0.01 mm are required for measuring specimendimensions.5.9 Analytical Balance:5.9.1 An analytical balance capable of weighing the shep-herds crook and loading train to an accuracy of 0.1 % relative.6. Preparation of Test Specimen6.1 Specimens may either be flame drawn o

30、r centerlessground into cylindrical form or diamond-saw cut and millground into rectangular form. Nonuniformity of any dimensionalong the length of the specimen shall not exceed 2 %. Whennonuniformity of any dimension exists, an average value shallbe used.6.2 The numerical ratio of beam span to mome

31、nt of inertiashall not be less than 60. The thickness or diameter to spanratio shall be less than 0.1.7. Calibration7.1 Direct calibration of the apparatus is accomplished byusing standard glasses, such as those supplied and certified bythe National Institute of Standards and Technology (NIST),havin

32、g known temperature values over the viscosity rangecovered by this practice.5Bias should be corrected by overallinstrument calibration:7.1.1 Determine the viscosity using test beams of an SRMglass which cover a range of cross-sectional moments ofinertia. Determine the viscosity over the viscosity ra

33、nge of 108Pas to 1011Pas by following the standard procedure de-scribed in Sections 8 and 9. Carry out tests keeping span andtime-temperature function constant.4The sole source of supply of flamebent hooks known to the committee at thistime is Insaco Inc., P.O. Box 422, Quakertown, PA 18951. If you

34、are aware ofalternative suppliers, please provide this information to ASTM Headquarters. Yourcomments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend.5Table 2, Annual Book of ASTM Standards, Vol 15.02 NIST Special PublicationNo. 260.C 1350M

35、 96 (2008)27.1.2 Mathematically fit resulting data to a convenient form(for example, polynomial or Fulcher6equation). Fit the datasupplied for the glass SRM to a Fulcher equation.7.1.3 Calculate the viscosities from both equations deter-mined in 7.1.2 at 20C minimum intervals over the measuredrange.

36、 Determine the viscosity ratio, hSRM fit/hmeasuredfit = fractional correction, and construct a calibration curve offractional correction versus log viscosity (measured fit). This isused to correct experimental viscosity data. (See Note 3.)Corrections greater than 20 % are cause for concern and shoul

37、dinitiate apparatus troubleshooting.NOTE 3If analyses are performed under some heating or cooling ratetime-temperature function, the thermocouple temperature may lag or leadthe actual sample temperature. If thermocouple lag or lead does occur, thecalibration curve described in 7.1.3 would incorporat

38、e this temperaturebias as well as any viscosity bias. To assess whether thermocouple lag orlead exists, viscosities for a glass SRM may be measured under isothermalconditions at several temperatures. Compare temperatures at equivalentviscosity levels from the analysis of the same glass SRM measured

39、underthe heating or cooling rate condition. Temperature differences indicatethermocouple lag or lead. The difference should be applied as a tempera-ture correction to measured temperatures prior to generating the calibra-tion curve (7.1.3) or applying the calibration correction to test data(Section

40、9).8. Procedure8.1 Deflection data may be taken under isothermal condi-tions or heating or cooling at controlled rates not to exceed5C/min.8.2 Identify the time-temperature function (for example,5C/min heating rate) to be used in the test. Use a sapphire oralumina specimen to generate a curve of bac

41、kground deflectionagainst temperature, using the chosen time-temperature func-tion intended for specimen measurement. The deflection of thetest specimen is then determined by algebraic subtraction ofthis background curve from the measured curve.8.3 Measure the dimensions of the test beam to the near

42、est0.01 mm. Use this data to calculate the cross-sectional momentof inertia. (Formulae for common cross-sections are presentedin Appendix X1 of Test Method C 598.)8.4 To protect the support from reaction with the specimenand reduce friction between specimen and support, place a thinplatinum foil in

43、each notch, then place the specimen beamacross the support stand at the notch points. Place a thinplatinum foil between the loading rod and the specimen. Allplatinum foil must be the same thickness, and suitably thin(preferably 25 m thick) so as to allow seating of thecomponents in their required po

44、sition.8.5 Carefully engage the loading rod to the specimen andcenter it. Apply a weight to the hook on the end of theextensometer, adjusting the total, applied load (consisting ofthe specimen, loading rod, hooks, fixtures, and weight) so thata usable deflection rate is obtained. Adjust the position

45、 of theextensometer to the lower end of its measuring range. Startheating the furnace, using the time-temperature function cho-sen for measurements.8.6 When a usable deflection rate is attained, begin record-ing extensometer, time, and temperature data to be used in datareduction. The collection int

46、erval should not exceed 1 min.Suitable means of accumulating data include computer-controlled data acquisition or plotting the deflection andtemperature of the specimen with a two pen recorder operatingon a convenient time base. (If such a recording device is notavailable and data must be taken manu

47、ally, the deflection andtemperature may be recorded by taking readings of both theextensometer and temperature alternately at 30-s intervals sothat each will be read at 1-min. intervals. Because it is lessaccurate than the other methods, the user is discouraged fromusing this method to acquire data.

48、) If the extensometer goes offrange during the test, reset it. Total beam deflections greaterthan 10 mm are excessive.9. Calculation9.1 Use the corrected change in extensometer readings, dh,during a given time interval, dt, as the rate of midpointdeflection, dh/dt, at the temperature corresponding t

49、o themiddle of that interval. Substitute those data into Eq 1 tocalculate the viscosity, h. Correct viscosity using the calibra-tion curve (see Section 7) by multiplying the viscosity by thefractional correction factor corresponding to that viscosity.10. Report10.1 At a minimum, report the following information:10.1.1 Identification of the glass tested,10.1.2 Manufacturing source and date,10.1.3 Calibration reference,10.1.4 Temperature and viscosity points,10.1.5 Date of test and name of operator, and10.1.6 Other observations (for example, sample