1、Designation: D 6601 02Standard Test Method forRubber PropertiesMeasurement of Cure and After-CureDynamic Properties Using a Rotorless Shear Rheometer1This standard is issued under the fixed designation D 6601; the number immediately following the designation indicates the year oforiginal adoption or
2、, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the use of a rotorless oscillatingshear rheometer for
3、measuring after cure dynamic properties atpredetermined temperature(s) below the cure temperature.1.2 Specified cure conditions that approximate a “staticcure” also are covered to minimize effects on cured rubbercompound dynamic properties. This test method is not in-tended to replace Test Method D
4、5289.1.3 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 standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.4 Warnin
5、gCompounds based on silicone or fluoroelas-tomers may have high levels of thermal contraction or pooradhesion to the dies when cooled after the cure portion of thistest method, causing slippage during strain sweeps. If thisoccurs, the results will not be reliable.2. Referenced Documents2.1 ASTM Stan
6、dards:D 1349 Practice for RubberStandard Temperatures forTesting2D 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black Industries2D 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure Meters2D 5992 Guide for Dynamic Testing of Vulcanized
7、Rubberand Rubber-Like Materials Using Vibratory Methods23. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 complex shear modulus, G*, nthe ratio of peakamplitude shear stress to peak amplitude shear strain; math-ematically, G* =(G82+ G92)1/2.3.1.2 complex torque, S*, nthe peak am
8、plitude torqueresponse measured by a reaction torque transducer for asinusoidally applied strain; mathematically, S* is computed byS* =(S82+ S92)1/2.3.1.3 dynamic cure, nany cure condition which oscillatesor moves the die.3.1.4 elastic torque, S8, nthe peak amplitude torque com-ponent, which is in p
9、hase with a sinusoidally applied strain.3.1.5 loss angle, d, nthe phase angle by which thecomplex torque (S*) leads a sinusoidally applied strain.3.1.6 loss factor, tan d, nthe ratio of loss modulus tostorage modulus, or the ratio of viscous torque to elastictorque; mathematically, tan d = G9/G8 =S9
10、/S8.3.1.7 loss shear modulus, G9, nthe component of appliedstress that is 90 out-of-phase with the shear strain, divided bythe strain.3.1.8 static cure, nthe cure conditions of 0.0 arc strainand 0.0 Hz in frequency, that is, no movement of the diesduring the cure test.3.1.9 storage shear modulus, G8
11、, nthe component ofapplied stress that is in phase with the shear strain, divided bythe strain.3.1.10 viscous torque, S9, nthe peak amplitude torquecomponent, which is 90 out of phase with a sinusoidallyapplied strain.4. Summary of Test Method4.1 A rubber test specimen is contained in a die cavity t
12、hatis closed and maintained at an elevated cure temperature. Thecavity is formed by two dies, one of which is oscillated througha rotary amplitude. This action produces a sinusoidal torsionalstrain in the test specimen resulting in a sinusoidal torque,which measures the viscoelastic changes of the t
13、est specimenas it cures. The test specimen must be a unvulcanized rubbercompound containing curatives. A controlled limited strain isapplied during cure to prevent effecting the aftercure proper-ties.4.2 After a predetermined cure time, the temperature isreduced and dynamic property measurements can
14、 be based ona strain sweep in which the strain amplitude is programmed tochange in steps under constant frequency and temperature, a1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.14 on Time and Temperature-Dependent Phy
15、sical Properties.Current edition approved Dec. 10, 2002. Published January 2003. Originallyapproved in 2000. Last previous edition approved in 2000 as D 6601 00.2Annual Book of ASTM Standards, Vol 09.01.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
16、59, United States.frequency sweep in which the frequency is programmed tochange in steps under constant strain amplitude and tempera-ture, or, a temperature sweep in which the temperature isprogrammed to decrease under constant strain amplitude andfrequency conditions.4.3 For an after-cure strain sw
17、eep, the instrument is typi-cally programmed to increase the strain with each subsequentstep change. This is done to minimize the influence of prior testconditions on subsequent test steps. Typically two repeat strainsweeps may be programmed consecutively to quantify thePayne Effect3, which is the r
18、eduction in dynamic storagemodulus from strain softening of the rubber vulcanizate.5. Significance and Use5.1 This test method is used to determine the vulcanizationcharacteristics of (vulcanizable) rubber compounds under se-lected test conditions of strain and frequency which do notsignificantly af
19、fect the cured dynamic properties. In the sametest, this test method also will measure the dynamic propertiesof the vulcanizate at temperatures significantly below the curetemperature. These lower temperature measurements are nec-essary in order to more effectively relate to rubber productservice co
20、nditions.5.2 This test method may be used for quality control inrubber manufacturing processes and for research and develop-ment testing of rubber compounds containing curatives. Thistest method also may be used for evaluating cure and dynamicproperty differences resulting from the use of different
21、com-pounding ingredients.5.3 For additional information regarding the significance ofdynamic testing of vulcanized rubber, the reader may wish toreference Guide D 5992.6. Apparatus6.1 Torsion Strain Rotorless Oscillating Rheometer with aSealed CavityThis type of rheometer measures the elastictorque
22、S8 and viscous torque S9 produced by oscillating angularstrain of set amplitude and frequency in a completely closedand sealed test cavity.6.2 Sealed Die CavityThe sealed die cavity is formed bytwo conical surface dies. In the measuring position, the twodies are fixed a specified distance apart so t
23、hat the cavity isclosed and sealed (see Fig. 1).6.3 Die GapFor the sealed cavity, no gap should exist atthe edges of the dies. At the center of the dies, the die gap shallbe set at 0.45 6 0.05 mm.6.4 Die Closing MechanismFor the sealed cavity, a pneu-matic cylinder or other device shall close the di
24、es and holdthem closed during the test with a force not less than 11 kN(2500 lbf).6.5 Die Oscillating SystemThe die oscillating systemconsists of a direct drive motor, which imparts a torsionaloscillating movement to the lower die in the cavity plane.6.5.1 The oscillation amplitude can be varied, bu
25、t a selec-tion of 0.2 arc (62.8 % shear strain) is preferred for the curetest while strains from 61to6100 % are preferred for theafter-cure strain sweeps. The oscillation frequency can bevaried between 0.03 Hz and 30 Hz.6.6 Torque Measuring SystemThe torque measuring sys-tem shall measure the result
26、ant shear torque.6.6.1 The torque measuring device shall be rigidly coupledto the upper die, any deformation between the die and deviceshall be negligibly small, and the device shall generate a signal,which is proportional to the torque. The total error resultingfrom zero point error, sensitivity er
27、ror, linearity, and repeat-ability errors shall not exceed 1 % of the selected measuringrange.6.6.2 The torque recording device shall be used to record thesignal from the torque measuring device and shall have aresponse time for full scale deflection of the torque scale of 1s or less. The torque sha
28、ll be recorded with an accuracy of 60.5 % of the range. Torque recording devices may includeanalog chart recorders, printers, plotters, or computers.6.6.3 A reference torque device is required to calibrate thetorque measurement system. A torque standard may be used tocalibrate the torque measuring s
29、ystem at the selected angular3A.R. Payne, J. Polymer Sci., 6, 57 (1962).FIG. 1 Typical Sealed Torsion Shear Rotorless CuremeterD6601022displacement by clamping a steel torsion rod to the oscillatingand the torque measuring dies of the torsion shear rheometer(see Fig. 2). The reference values for ang
30、ular displacement andcorresponding torque shall be established by the manufacturerfor each torque standard.6.7 Reference Test TemperatureThe standard referencetest temperature for cure shall be either 140C, 160C, or180C while dynamic property measurements after-cure (dy-namic property measurements m
31、ade after completion of thecure test) should be made at either 100C or 60C. Tests maybe carried out at other temperatures, if required. Other tem-peratures should be selected in accordance with PracticeD 1349 when practical.6.8 Temperature Control SystemThis system shall permitthe reference temperat
32、ure to be varied between 40C and220C with an accuracy of 60.3C or better.6.8.1 The dies shall heat to the set point temperature in 1.0min or less from closure of the test cavity. Once the initialheating up time has been completed, die temperature shall notvary by more than 60.3C for the remainder of
33、 a cure test ata set temperature. When the set temperature is changed in aprogrammed temperature sweep or strain sweep, dynamicproperty measurements should not be recorded until the dietemperatures are within 60.3C of the new set temperature forat least 30 s.6.8.2 Temperature distribution within the
34、 test piece shall beas uniform as possible. Within the deformation zone, a toler-ance of 61C of the average test piece temperature shall not beexceeded.6.8.3 Die temperature is determined by a temperature sensorused for control. The difference between the die temperatureand the average test piece te
35、mperature shall not be more than2C. Temperature measurement accuracy shall be 60.3C forthe die temperature sensor.6.8.4 The upper and lower dies shall each be jacketed withforced air cooling devices in order to rapidly decrease thetemperature of the upper and lower dies after the cure test iscomplet
36、ed.7. Test Specimen7.1 A test specimen taken from a sample shall be between 5and6cm3for the sealed cavity oscillating rheometer. Thespecimen volume should exceed the test cavity volume by asmall amount, to be determined by preliminary tests. Typically,specimen volume should be 130 to 150 % of the te
37、st cavityvolume. Once a target mass for a desired volume has beenestablished, specimen masses should be controlled to within60.5 g for best repeatability. The initial test specimen shapeshould fit well within the perimeter of the test cavity.7.2 Compounded Rubber SpecimensTest specimens shallbe take
38、n from a rubber compound as required by the mixingmethod or other sampling instructions. Only rubber com-pounds with curatives may be tested.7.2.1 The rubber compound shall be in the form of a sheet,at room temperature, and as free of air as possible.8. Procedure8.1 Select from one of six different
39、cure conditions shown inTable 1.8.2 Select from one of eight different after-cure dynamictesting conditions shown in Table 2.8.3 Program a test configuration which incorporates theseconditions and store on the instrument computer operatingsystem.8.4 Load the test configuration to run the test.8.5 En
40、ter specimen identification.8.6 Wait until both dies are at the initial test temperature.Open the test cavity and visually check both upper and lowerdies for cleanliness. Clean the dies, if necessary. Place the testspecimen on the center of the lower die and close the dieswithin 20 s.FIG. 2 Typical
41、Torque Standard Calibration Device for TorsionShear CuremetersTABLE 1 Test Conditions for Cure TestANOTE 1Cure properties should be measured in accordance with TestMethod D 5289.Cure Condition No. Temperature, C Frequency, Hz Strain, 6 Arc.1 140 1.67 0.22 160 1.67 0.23 180 1.67 0.24 140 0 05 160 0 0
42、6 180 0 0APlease note that cure conditions of 0.2 arc strain and 1.67 Hz frequency mayinfluence post cure propertiesD66010239. Report9.1 Report the following information.9.1.1 A full description of the sample, or test specimen(s), orboth, including their origin.9.1.2 Type and model of oscillating rh
43、eometer.9.1.3 The frequency, strain, temperature and time for thecure test (if no strain, indicate “static cure”).9.1.4 Minimum torque (ML) as dNm, maximum torque (MH)as dNm, time to scorch as indicated by time to one unit rise (indNm units) from minimum torque (tS1) in minutes and decimalfraction o
44、f a minute, and time to 10 %, 50 %, and 90 % state ofcure in minutes and decimal fraction of a minute.NOTE 1For static cure, no cure properties are reported since nomeasurements are possible.9.1.5 The temperature, frequency and different strains ap-plied in an after-cure strain sweep.9.1.6 The stora
45、ge shear modulus G8 in kPa and the percentstrain for each step in the programmed strain sweep.9.1.7 The loss shear modulus G9 in kPa and the percentstrain for each step in the programmed strain sweep.9.1.8 The tangent delta (tan d) and the percent strain foreach step in the programmed strain sweep.9
46、.1.9 If two consecutive strain sweeps are programmed, theresults from both of these strain sweeps should be recorded(reference the Payne Effect discussed in 4.3).10. Precision and Bias10.1 A precision and bias estimate has not been completedfor this test method at this time. This will be completed i
47、naccordance with Practice D 4483.11. Keywords11.1 dynamic properties; loss modulus; rotorless oscillatingshear rheometer; storage modulusASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this sta
48、ndard 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 technical committee and must be reviewed every five years an
49、dif 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 consideration 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 Harb
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