CN110646287A - Characterization method for stress softening reversible recovery of thermoplastic vulcanized rubber in tearing mode - Google Patents
Characterization method for stress softening reversible recovery of thermoplastic vulcanized rubber in tearing mode Download PDFInfo
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- 238000011084 recovery Methods 0.000 title claims abstract description 51
- 230000002441 reversible effect Effects 0.000 title claims abstract description 34
- 229920001169 thermoplastic Polymers 0.000 title claims description 28
- 239000004416 thermosoftening plastic Substances 0.000 title claims description 28
- 239000004636 vulcanized rubber Substances 0.000 title claims description 27
- 238000012512 characterization method Methods 0.000 title abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 229920006342 thermoplastic vulcanizate Polymers 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000004154 testing of material Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 230000006399 behavior Effects 0.000 claims 8
- 239000004743 Polypropylene Substances 0.000 description 13
- 229920002943 EPDM rubber Polymers 0.000 description 12
- 238000000748 compression moulding Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
Abstract
The invention provides a characterization method of stress softening reversible recovery under a thermoplastic vulcanizate tearing mode, and provides an effective method for qualitative and quantitative characterization of the reversible recovery. The characterization method comprises the following steps: a. applying certain strain on a right-angle tearing sample, testing the first stress softening behavior, wherein the gauge length of the sample is l0(ii) a b. After the test is finished, the sample is cooled to room temperature after being subjected to heat treatment, and the distance between test marked lines is liTear permanent set is noted
c. Carrying out a second stress test on the sample, taking the center point of the sample after heat treatment as a reference, re-dividing the marked lines at equal intervals on the two sides of the sample, wherein the interval is l0Then applying the same strain; d. reading the maximum tear strength in the curve, wherein the maximum tear strength recovery rate is (the maximum tear strength of the second stress softening/the maximum tear strength of the first stress softening) multiplied by 100%; e. from the closeness of the two curves, the qualitative judgment can be madeDegree of reversion; and quantitatively judging the reversible recovery degree from the permanent tear deformation and the maximum tear strength recovery rate.
Description
Technical Field
The invention relates to a characterization method of stress softening reversible recovery of thermoplastic vulcanized rubber in a tearing mode, in particular to a qualitative and quantitative characterization method of stress softening reversible recovery of thermoplastic vulcanized rubber in the tearing mode by testing the tearing stress softening behavior before and after heat treatment and checking the closeness degree of a tearing strength-strain curve, the tearing permanent deformation and the maximum tearing strength recovery rate.
Background
The stress softening refers to the phenomenon that after the material is deformed by one or more times of loading and unloading, the required stress in the subsequent deformation process is smaller than that in the previous deformation, namely the material is softened after strain. The thermoplastic vulcanizate undergoes a stress softening phenomenon after the first tensile deformation, i.e. the Mullins effect, which is accompanied by residual deformation and induced anisotropy and is a loss factor of viscosity. The thermoplastic vulcanized rubber is a novel thermoplastic elastomer prepared by dynamic vulcanization, shows viscoelasticity, and the stress softening effect of the thermoplastic vulcanized rubber is related to the plastic deformation of matrix thermoplastic resin. The heat treatment is carried out on the thermoplastic vulcanized rubber sample after the stress softening test, the stress softening behavior has certain reversible recovery, the reversible recovery of the tearing stress softening behavior of the thermoplastic vulcanized rubber is researched, and the heat treatment method has important significance for researching the viscoelastic behavior of the thermoplastic vulcanized rubber and estimating the service life of the thermoplastic vulcanized rubber, both in theoretical research and application. However, current studies on the stress softening effect of thermoplastic vulcanizates are generally conducted only in tensile and compression modes for testing and characterization; in fact, the thermoplastic vulcanized rubber can generate a stress softening phenomenon under a tearing mode, and the characterization of the tearing stress softening has important significance in both theoretical research and application, but a quantitative characterization method for tearing stress softening generally accepted by people is not seen so far.
The invention provides a new technical scheme, the tearing stress softening of the thermoplastic vulcanized rubber is tested before and after heat treatment, the reversible recovery of the tearing stress softening can be qualitatively represented by comparing the closeness degree of a tearing strength-strain curve, and the reversible recovery degree of the tearing stress softening can be quantitatively represented by tearing permanent deformation and the maximum tearing strength recovery rate.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a characterization method of stress softening reversible recovery under a thermoplastic vulcanizate tearing mode, and solves the problem that no characterization method of stress softening reversible recovery under the thermoplastic vulcanizate tearing mode is generally accepted by people at present.
The technical scheme is as follows: the invention relates to a characterization method of stress softening reversible recovery under a thermoplastic vulcanizate tearing mode, which adopts a universal material testing machine to test the first stress softening behavior of a right-angle thermoplastic vulcanizate tearing sample, then carries out heat treatment on the sample and cools the sample to room temperature, then carries out the second stress softening behavior test, obtains a tearing strength-strain curve according to test data, and calculates and obtains permanent tearing deformation and maximum tearing strength recovery rate, and comprises the following specific steps:
(1) applying a certain tearing strain on a right-angle thermoplastic vulcanized rubber tearing sample by using a universal material testing machine, and testing the first stress softening behavior of the right-angle thermoplastic vulcanized rubber tearing sample at room temperature, wherein the right-angle tearing sample can be divided into a non-cutting sample and a cutting sample, and the two samples are both suitable for the test mode, and if no special description exists, the test mode usually refers to the non-cutting sample; the initial distance between two parallel marked lines on the right-angle tearing sample is l0(two straight lines perpendicular to the sample strip are marked at equal distances on both sides of the center point of the sample, and the distance between the midpoints of the two straight lines is used as a length measurement standard), and the distance between the two parallel marked lines when the sample is stretched to a specified strain in a tearing mode is lsRecording the tear strength-strain curve;
(2) after the first stress softening behavior test is finished, taking the right-angle tearing sample out of the universal material testing machine, placing the right-angle tearing sample in a vacuum drying oven for heat treatment for a certain time, taking the right-angle tearing sample out and cooling the right-angle tearing sample to room temperature, wherein the distance between two parallel marked lines on the right-angle tearing sample is liAnd the tearing permanent deformation is recorded as K, and the calculation formula is as follows:
(3) adopting a universal material testing machine to carry out a second stress softening behavior test on the heat-treated right-angle-shaped tearing sample, taking the center point of the heat-treated right-angle-shaped tearing sample as a reference, marking two straight lines perpendicular to the sample strips at equal intervals on two sides of the center point again, and marking two parallel marked lines on the sampleIs a distance of l0Applying the same strain as the first stress softening behavior, testing the second stress softening behavior at room temperature, and recording a tearing strength-strain curve;
(4) the maximum tear strengths in the second and first stress softening curves were read from the tear strength-strain relationship curves in (3) and (1), respectively, and the maximum tear strength recovery rate for the reversible recovery of stress softening in the tear mode was ═ 100% of (second stress softening maximum tear strength/first stress softening maximum tear strength).
The closer the first stress softening curve and the second stress softening curve are, the smaller the permanent tear deformation is, the higher the maximum tear strength recovery rate is, and the higher the reversible recovery degree of the stress softening in the tear mode is.
Has the advantages that: the invention provides a characterization method of stress softening reversible recovery under a thermoplastic vulcanizate tearing mode, and provides an effective method for qualitative and quantitative evaluation of the stress softening reversible recovery under the thermoplastic vulcanizate tearing mode.
Drawings
FIG. 1 is a tear strength-strain curve (heat treatment temperature 100 ℃) of stress softening in the first and second tear modes of a PP/EPDM thermoplastic vulcanizate (mass ratio 40/60) obtained according to example 1 of the present invention.
FIG. 2 is a tear strength-strain curve (heat treatment temperature 120 ℃) of stress softening in the first and second tear modes of a PP/EPDM thermoplastic vulcanizate (mass ratio 40/60) obtained according to example 2 of the present invention.
FIG. 3 is a tear strength-strain curve (heat treatment temperature 140 ℃) for stress softening in the first and second tear modes of a PP/EPDM thermoplastic vulcanizate (mass ratio 40/60) obtained according to example 3 of the present invention.
FIG. 4 is a schematic view of a right angle tear specimen and a marked line.
The specific implementation mode is as follows: the following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1: characterization of stress softening reversible recovery under PP/EPDM thermoplastic vulcanizate tearing mode
Rectangular PP (polypropylene)/EPDM (ethylene propylene diene monomer) (mass ratio: 40/60) thermoplastic vulcanized tear test specimens are prepared by a compression molding method, and the test specimens should not have air bubbles, impurities and damage.
(1) A GT-TCS-2000 type universal material testing machine is adopted to apply 40% strain on a right-angle thermoplastic vulcanized rubber tearing sample, the first stress softening behavior of the thermoplastic vulcanized rubber tearing sample is tested under the room temperature condition, and the initial distance between two parallel marked lines on the right-angle tearing sample is l050.00mm, distance between two parallel markings when stretched to a specified strain in tear mode, is lsRecording the tearing strength-strain relation curve of the product which is 70.00 mm;
(2) after the first stress softening behavior test is finished, taking out the right-angle tearing sample from the universal material testing machine, placing the right-angle tearing sample in a vacuum drying oven at 100 ℃ for heat treatment for 30min, then taking out the right-angle tearing sample and cooling the right-angle tearing sample to room temperature, wherein the distance between two parallel marked lines on the right-angle tearing sample is liThe tear set is recorded as K, 51.50mm, and the formula is:
(3) adopting a GT-TCS-2000 type universal material testing machine to carry out a second stress softening behavior test on the right-angle-shaped thermoplastic vulcanized rubber tearing sample after heat treatment, taking the center point of the right-angle-shaped tearing sample after heat treatment as a reference, marking two straight lines perpendicular to the sample strips at equal intervals on two sides of the center point again, and setting the distance between two parallel marked lines of the sample as l0Applying 40% strain, testing the second stress softening behavior at room temperature, and recording the tearing strength-strain relation curve;
(4) maximum tear strengths in the second and first stress softening curves were read from the tear strength-strain relationship curves in (3) and (1), respectively, and were 60.95kN/m and 57.07kN/m, respectively; for the reversible recovery of the thermoplastic vulcanizate from stress softening in tear mode, the maximum tear recovery is 106.80% (second time stress softening maximum tear/first time stress softening maximum tear) x 100%.
FIG. 1 is a tear strength-strain curve of the stress softening test in the first and second tear modes for the PP/EPDM thermoplastic vulcanizate obtained in example 1. It can be qualitatively seen from the relationship curve of the tearing strength and the strain of the stress softening in the first tearing mode and the second tearing mode that the stress softening of the sample obtains a certain reversible recovery in the tearing mode, but a certain obvious distance exists between the tearing strength and the strain relationship curves of the two times, and the stress after softening only obtains a certain recovery after heat treatment; the maximum tear strength in the second stress-softening curve is significantly higher than the first because the specimen still has a partially oriented state after heat treatment, and the second test requires more resistance to overcome and thus higher maximum tear strength when the same strain is applied; quantitatively showing that after the stress softening test in the first tearing mode, the sample is subjected to heat treatment, the tearing permanent deformation of the sample is 3.00 percent, and the deformation of the sample is recovered to a certain degree; the recovery of maximum tear strength during the second stress softening test was 106.80%, quantitatively indicating some stress softening reversible recovery.
Example 2: characterization of stress softening reversible recovery under PP/EPDM thermoplastic vulcanizate tearing mode
Rectangular PP/EPDM (40/60 mass ratio) thermoplastic vulcanizate tear specimens were prepared by compression molding, and the specimens should be free of air bubbles, impurities and damage.
(1) A GT-TCS-2000 type universal material testing machine is adopted to apply 40% strain on a right-angle thermoplastic vulcanized rubber tearing sample, the first stress softening behavior of the thermoplastic vulcanized rubber tearing sample is tested under the room temperature condition, and the initial distance between two parallel marked lines on the right-angle tearing sample is l050.00mm, distance between two parallel markings when stretched to a specified strain in tear mode, is lsRecording the tearing strength-strain relation curve of the product which is 70.00 mm;
(2) after the first stress softening behavior test is finished, taking the right-angle tearing sample from the universal material testing machineTaking out, placing in a vacuum drying oven at 120 deg.C, heat treating for 30min, taking out, cooling to room temperature, at which time the length l of the right-angle tear specimeniThe tear set is recorded as K, 50.70mm, and the formula is:
(3) adopting a GT-TCS-2000 type universal material testing machine to carry out a second stress softening behavior test on the right-angle-shaped thermoplastic vulcanized rubber tearing sample after heat treatment, taking the center point of the right-angle-shaped tearing sample after heat treatment as a reference, marking two straight lines perpendicular to the sample strips at equal intervals on two sides of the center point again, and setting the distance between two parallel marked lines of the sample as l0Applying 40% strain, testing the second stress softening behavior at room temperature, and recording the tearing strength-strain relation curve;
(4) the maximum tear strengths in the second and first stress softening curves were 60.54kN/m and 60.10kN/m, respectively, from the tear strength-strain relationship curves in (3) and (1), respectively; for the reversible recovery of the thermoplastic vulcanizate from tear stress softening, the maximum tear strength recovery is 100.73% (second time stress softening maximum tear strength/first time stress softening tear strength) x 100%.
FIG. 2 is a tear strength-strain curve of the stress softening test in the first and second tear modes for the PP/EPDM thermoplastic vulcanizate obtained in example 2. Qualitatively, the reversible recovery rate of the stress softening of the sample in the tearing mode is higher from the tearing strength-strain relation curves of the stress softening in the first tearing mode and the second tearing mode, which is particularly shown in that the tearing strength-strain relation curves of the two tests are closer, and the softened stress can be recovered to a certain degree after the heat treatment; after the stress softening test in the first tearing mode, carrying out heat treatment on the sample, wherein the tearing permanent deformation of the sample is 1.40%, and the deformation of the sample can be recovered to a greater extent; the recovery of maximum tear strength during the second stress softening test was 100.73%, quantitatively indicating the reversible recovery from stress softening.
Example 3: characterization of stress softening reversible recovery under PP/EPDM thermoplastic vulcanizate tearing mode
Rectangular PP/DPDM (mass ratio: 40/60) thermoplastic vulcanizate tear specimens were prepared by compression molding, which should be free of bubbles, impurities and damage.
(1) A GT-TCS-2000 type universal material testing machine is adopted to apply 40% strain on a right-angle thermoplastic vulcanized rubber tearing sample, the first stress softening behavior of the thermoplastic vulcanized rubber tearing sample is tested under the room temperature condition, and the initial distance between two parallel marked lines on the right-angle tearing sample is l050.00mm, distance between two parallel markings when stretched to a specified strain in tear mode, is lsRecording the tearing strength-strain relation curve of the product which is 70.00 mm;
(2) after the first stress softening behavior test is finished, taking out the right-angle tearing sample from the universal material testing machine, placing the right-angle tearing sample in a vacuum drying oven at 140 ℃ for heat treatment for 30min, taking out the right-angle tearing sample, and cooling to room temperature, wherein the length l of the right-angle tearing sample is equal to the length l of the right-angle tearing sampleiThe tear set is recorded as K, 50.40mm, and the formula is:
(3) adopting a GT-TCS-2000 type universal material testing machine to carry out a second stress softening behavior test on the right-angle-shaped thermoplastic vulcanized rubber tearing sample after heat treatment, taking the center point of the right-angle-shaped tearing sample after heat treatment as a reference, marking two straight lines perpendicular to the sample strips at equal intervals on two sides of the center point again, and setting the distance between two parallel marked lines of the sample as l0Applying 40% strain, testing the second stress softening behavior at room temperature, and recording the tearing strength-strain relation curve;
(4) the maximum tear strengths in the second and first stress-softening curves were 57.88kN/m and 58.00kN/m, respectively, from the tear strength-strain relationship curves in (3) and (1), respectively; for the reversible recovery of the thermoplastic vulcanizate from tear stress softening, the maximum tear strength recovery (second time stress softening maximum tear strength/first time stress softening maximum tear strength) × 100% is 99.38%.
FIG. 3 is a tear strength-strain curve of the stress softening test in the first and second tear modes for the PP/EPDM thermoplastic vulcanizate obtained in example 3. Qualitatively, the tearing strength-strain relation curve of the stress softening in the first tearing mode and the second tearing mode shows that the stress softening of the sample obtains ideal reversible recovery in the tearing mode, the distance between the two tearing strength-strain relation curves is very close, and the stress after softening obtains good recovery after heat treatment; after the stress softening test in the first tearing mode, carrying out heat treatment on the sample, wherein the tearing permanent deformation of the sample is 0.80%, and the deformation of the sample is recovered to a great extent; the recovery of the maximum tear strength during the second stress softening test was 99.79%, quantitatively indicating a good reversible recovery from stress softening.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.
Claims (1)
1. A method for characterizing stress softening reversible recovery of a thermoplastic vulcanizate in a tear mode, comprising the steps of:
(1) applying a certain tearing strain on a right-angle thermoplastic vulcanized rubber tearing sample by adopting a universal material testing machine, testing the first stress softening behavior of the right-angle thermoplastic vulcanized rubber tearing sample at room temperature, wherein the initial distance between two parallel marked lines on the right-angle tearing sample is l0Recording a tearing strength-strain relation curve;
(2) after the first stress softening behavior test is finished, taking out the right-angle tearing sample from the universal material testing machine, placing the right-angle tearing sample in a vacuum drying oven for heat treatment for a certain time, taking out the right-angle tearing sample, cooling to room temperature, and then cooling to room temperatureThe distance between two parallel marked lines on the angular tearing sample is liAnd the tearing permanent deformation is recorded as K, and the calculation formula is as follows:
(3) adopting a universal material testing machine to carry out secondary stress softening behavior test on the right-angle-shaped thermoplastic vulcanized rubber tearing sample after heat treatment, taking the center point of the right-angle-shaped tearing sample after heat treatment as a reference, re-marking two straight lines perpendicular to the sample strips at equal intervals on two sides of the center point, and setting the distance between two parallel marked lines of the sample to be l0Applying the same strain as the first stress softening behavior test, testing the second stress softening behavior of the test piece at room temperature, and recording a tearing strength-strain relation curve;
(4) the maximum tear strengths in the second and first stress softening curves were read from the tear strength-strain relationship curves in (3) and (1), respectively, and the maximum tear strength recovery rate for the reversible recovery of stress softening in the tear mode was ═ 100% of (second stress softening maximum tear strength/first stress softening maximum tear strength);
(5) qualitatively judging the reversible recovery degree of the stress softening behavior in the tearing mode according to the closeness degree of the test curves of the first and second stress softening behaviors of the thermoplastic vulcanized rubber; and quantitatively judging the reversible recovery degree of the stress softening behavior in the tearing mode from the tearing permanent deformation and the maximum tearing strength recovery rate of the sample after heat treatment.
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| CN107024383A (en) * | 2017-04-10 | 2017-08-08 | 青岛科技大学 | A kind of thermoplastic sulfurized rubber compression stress relaxation can reverse recovery behavior characterizing method |
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- 2019-10-11 CN CN201910963734.2A patent/CN110646287A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| US5526823A (en) * | 1988-11-15 | 1996-06-18 | Family Health International | "Stress-softened elastometeric films, articles, and method and apparatus for making such films and articles |
| CN103776709A (en) * | 2014-01-17 | 2014-05-07 | 青岛科技大学 | Characterization method for compression stress softening and transient-persistent deformation of elastic body |
| CN105968466A (en) * | 2016-05-13 | 2016-09-28 | 吉林师范大学 | Low-temperature-resistant and aging-resistant chloroprene rubber composite material |
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Application publication date: 20200103 |