1、Designation: D8059 16Standard Test Method forRubber CompoundsMeasurement of UnvulcanizedDynamic Strain Softening (Payne Effect) Using SealedCavity Rotorless Shear Rheometers1This standard is issued under the fixed designation D8059; the number immediately following the designation indicates the year
2、 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 method covers the use of a sealed cavityrotorl
3、ess oscillating shear rheometer for the measurement ofthe softening effects of rising sinusoidal strain when applied toan unvulcanized rubber compound containing significantamounts of colloidal fillers (such as silica or carbon black, orboth) from a rubber mixing procedure. These strain softeningpro
4、perties relate to mixing conditions, the composition of therubber compound, colloidal particle (Payne Effect) character-istics of the fillers, and in some cases the degree of reactionbetween an organosilane and precipitated, hydrated silicaduring mixing. This procedure is being commonly applied toru
5、bber reactive mixing procedures.1.2 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 limitati
6、ons prior to use.2. Referenced Documents2.1 ASTM Standards:2D1566 Terminology Relating to Rubber3. Terminology3.1 Definitions:3.1.1 elastic torque, S, nthe peak amplitude torque com-ponent which is in phase with a sinusoidally applied strain.3.1.2 viscous torque, S”, nthe peak amplitude torquecompon
7、ent which is 90 out of phase with a sinusoidallyapplied strain.3.1.3 complex torque, S*, nthe peak amplitude torqueresponse measured by a reaction torque transducer for asinusoidally applied strain; mathematically, S* is computed byS* = (S2+S”2)1/2.3.1.4 loss angle, ,nthe phase angle by which thecom
8、plex torque (S*) leads a sinusoidally applied strain.3.1.5 storage shear modulus, G, nthe ratio of (elastic)peak amplitude shear stress to peak amplitude shear strain forthe torque component in phase with a sinusoidally appliedstrain; mathematically, G = (S/Area)/Peak Strain.3.1.6 loss shear modulus
9、, G”, nthe ratio of (viscous) peakamplitude shear stress to peak amplitude shear strain for thetorque component 90 out of phase with a sinusoidally appliedstrain; mathematically, G” = (S”/Area)/Peak Strain.3.1.7 complex shear modulus, G*, nthe ratio of peakamplitude shear stress to peak amplitude sh
10、ear strain;mathematically, G* = (S*/Area)/Strain = (G2+G”2)1/2.3.1.8 loss factor, tan ,nthe ratio of loss modulus tostorage modulus, or the ratio of viscous torque to elastictorque; mathematically, tan = G”/G = S”/S.3.1.9 Payne Effect, nin the low amplitude dynamic testingof filled rubbers, the decr
11、ease in modulus (G or E) as theamplitude of deformation is increased.3.1.9.1 DiscussionThe effect is caused by a decrease inthe additive contributions of polymer-polymer interactions,hydrodynamic effects, the polymer-filler and filler-fillerinteractions. D15664. Summary of Test Method4.1 An uncured
12、rubber compound specimen is contained ina sealed die cavity which is closed and maintained at anelevated temperature. The cavity is formed by two dies, one ofwhich is oscillated through a rotary amplitude. This actionproduces a sinusoidal torsional strain in the test specimenresulting in a sinusoida
13、l torque, which measures a viscoelasticquality of the test specimen. The test specimen can be anuncured rubber compound containing carbon black, precipi-tated hydrated silica, or both of these reinforcing fillers. Thesilica loaded compounds may also contain an organosilane1This test method is under
14、the jurisdiction of ASTM Committee D11 on Rubberand Rubber-like Materials and is the direct responsibility of Subcommittee D11.12on Processability Tests.Current edition approved July 1, 2016. Published October 2016. DOI: 10.1520/D8059-16.2For referenced ASTM standards, visit the ASTM website, www.as
15、tm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1with diff
16、ering degrees of reaction (silanization) from differingprior combinations of mixing time and temperature.4.2 The Payne effect is a phenomenon in the low amplitudedynamic testing of strain dependent filled rubbers where themodulus (Gand E) decreases as the amplitude of deformationis increased. This d
17、ynamic modulus of filled elastomers andrubbers at low amplitude deformations consists of additivecontributions of the polymer-polymer interaction, the hydro-dynamic effect, the polymer-filler interaction, and the filler-filler network caused by the filler-filler interaction. Manyfactors, including t
18、he type and surface area of colloidal fillerssuch as carbon black and precipitated hydrated silica, the fillerconcentration, silanization and other treatments, can directlyeffect this filler-filler interaction as measured by the PayneEffect. Fig. 1 illustrates this Payne Effect.4.3 Typically the unc
19、ured rubber specimen is sealed underpressure in the closed cavity for exactly 10 min with a very lowsinusoidal oscillation frequency of 0.07 % (conditioning),followed by a broad strain sweep at the programmed process-ability temperature.4.4 These viscoelastic measurements can be made from thebroad s
20、train sweep based on a strain amplitude sweep in whichthe applied strain is preprogrammed to start at 0.07 % strainand to increase in steps under constant frequency and tempera-ture conditions till reaching 300 % strain at 1 Hz.5. Significance and Use5.1 This test method is used to measure viscoelas
21、tic prop-erties through the strain softening effects of a strain amplitudesweep (the Payne Effect).5.2 For the uncured state, the time conditioning and strainamplitude strain sweeps can relate to colloidal silica particle orcarbon black deagglomeration from the mixing process. Theprofile of this Pay
22、ne Effect from G storage modulus can alsobe a function of loading levels and particle size of these fillersin the rubber hydrocarbon medium. In addition, with silica andan organosilane additive, this G strain softening effect candetermine if a given silanization reaction between a subjectsilica and
23、an organosilane was achieved through reactivemixing. If the silanization reaction during the mixing was notachieved, the maximum G storage modulus from the strainsweep will not be lowered and the silica particle attraction toother silica particles will still be high resulting in a more densefiller n
24、etwork that remains.6. Apparatus6.1 Torsion Strain Rotorless Oscillating Rheometer with aSealed CavityThis type of rheometer measures the elastictorque S and viscous torque S” produced by oscillatingangular strain of set amplitude and frequency in a completelyclosed and sealed test cavity.6.2 Sealed
25、 Die CavityThe sealed die cavity is formed bytwo biconical dies. In the measuring position, the two dies arefixed a specified distance apart so that the cavity is closed andsealed (see Fig. 2).6.3 Die GapFor the sealed cavity, no gap should exist atthe edges of the dies. At the center of the dies, t
26、he 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 dies 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
27、drive motor which imparts a torsionaloscillating movement to the lower die in the cavity plane.6.6 Torque Measuring SystemThe torque measuring sys-tem shall measure the resultant shear torque.6.6.1 The torque measuring device shall be rigidly coupledto one of the dies, any deformation between the di
28、e and deviceshall be negligibly small, and the device shall generate a signalwhich is proportional to the torque. The total error resultingfrom zero point error, sensitivity error, linearity, and %repeat-ability errors shall not exceed1%oftheselected measuringrange.6.6.2 The torque recording device
29、shall be used to record thesignal from the torque measuring device and shall have aFIG. 1 Effect of Filler Loading on Measured Payne EffectD8059 162response time for full scale deflection of the torque scale of 1s or less. The torque shall be recorded with an accuracy of60.5 % of the range. Torque r
30、ecording 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 system at the selected angulardisplacement by clamping a steel to
31、rsion rod to the oscillatingand the torque measuring dies of the torsion shear rheometer(see Fig. 3). The reference values for angular displacement andcorresponding torque shall be established by the manufacturerfor each torque standard.6.7 Reference Test TemperatureThe standard referencetest temper
32、ature for uncured rubber compounds for measuringthe Payne effect is 70C.6.8 Temperature Control SystemThis system shall permitthe reference temperature to be set to 70C.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 u
33、p time has been completed, die temperature shall notvary by more than 60.3C for the remainder of a test at a settemperature.6.8.2 Temperature distribution within the test piece shall beas uniform as possible. Within the deformation zone, a toler-ance of 61C of the average test piece temperature shal
34、l 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 temperature shall not be more than2C. Temperature measurement accuracy shall be 60.3C forthe die temperature sensor.7. Test Specimen7.1 A
35、 test specimen taken from a sample shall be between 5and 6 cm3for 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 110 to 130 % of the test cavityvolume. Once
36、a target mass for a desired volume has beenestablished, specimen masses should be controlled to within60.1 g for best repeatability. The initial test specimen shapeshould fit well within the perimeter of the test cavity.7.2 Uncured Rubber SpecimensCondition the mixed stockspecimen until it has reach
37、ed room temperature (23 6 3C (736 5F) throughout. The uncured rubber test specimen shouldbe tested as received, that is unmassed (not milled).FIG. 2 Typical Sealed Torsion Shear Rotorless Rheometer withBiconical DiesFIG. 3 Typical Torque Standard Calibration Device for TorsionShear CuremetersD8059 1
38、637.2.1 The rubber compound shall be in the form of a sheet,at room temperature, and as free of air as possible.7.2.2 Rubber test specimens in a sealed cavity oscillatingrheometer must be preconditioned in the instrument beforerheological measurements are made to improve test repeatabil-ity. A progr
39、ammed pre-conditioning step shall consist ofoscillating the specimen at 0.1 Hz, 60.07 % strain, 70C for 10min, as specified in Table 1. Any deviations from thesestandard frequency, strain and time duration can have signifi-cant effect on the Payne Plateau.8. Procedure8.1 Select the strain, frequency
40、, temperature and time for theconditioning step as listed for rubber compounds in Table 1.8.2 Select the strain steps and the frequency and tempera-ture conditions for the amplitude strain sweep for the uncuredrubber compounds as given in Table 1.8.3 Quantitatively weigh and cut a specimen from theu
41、ncured subject rubber compound sample to within 60.1gofthe target mass for the subject compound, which is based on themass of the subject material at 120 % cavity fill factor(reference 7.1).8.4 Program the test configuration to run the test.8.5 Enter specimen identification.8.6 Wait until both dies
42、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 a sheetof 23-micron thick Nylon 6,6 film over the lower die. Place thetest specimen on the film on the center of the lower die, lay asecond sheet o
43、f Nylon 6,6 film on top of the specimen, andclose the dies within 20 s.9. 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 rheometer.9.1.3 The frequency, strain, temperature and t
44、ime for theconditioning step.9.1.4 The frequency in Hertz and temperature in degreesCelsius for all strain sweeps.9.1.5 Report maximum G in kPa units and note % strain atmaximum G.9.1.6 Report Gin kPa units at 0.1 %, 1.0 % and 10 % strainamplitude.10. Precision and Bias10.1 A precision and bias esti
45、mate has not been completedfor this test method at this time.11. Keywords11.1 loss modulus; loss tangent; Mullins Effect; PayneEffect; processability test; rheological properties; rotorlessoscillating shear rheometer; storage modulus; strain softeningeffect; tan delta; tangent delta; VE ratio; visco
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