CN112284904A - Characterization method of shape memory behavior of thermoplastic vulcanized rubber in compression mode - Google Patents
Characterization method of shape memory behavior of thermoplastic vulcanized rubber in compression mode Download PDFInfo
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- 238000007906 compression Methods 0.000 title claims abstract description 59
- 230000006835 compression Effects 0.000 title claims abstract description 56
- 230000006399 behavior Effects 0.000 title claims abstract description 25
- 229920001169 thermoplastic Polymers 0.000 title claims abstract description 10
- 239000004416 thermosoftening plastic Substances 0.000 title claims abstract description 10
- 238000012512 characterization method Methods 0.000 title abstract description 12
- 239000004636 vulcanized rubber Substances 0.000 title description 9
- 229920006342 thermoplastic vulcanizate Polymers 0.000 claims abstract description 54
- 238000011084 recovery Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000005457 ice water Substances 0.000 claims abstract description 7
- 239000002861 polymer material Substances 0.000 claims description 11
- 229920000431 shape-memory polymer Polymers 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 4
- 230000009477 glass transition Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920006125 amorphous polymer Polymers 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 229920000459 Nitrile rubber Polymers 0.000 description 18
- 239000005038 ethylene vinyl acetate Substances 0.000 description 18
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 18
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 description 6
- 229920001084 poly(chloroprene) Polymers 0.000 description 6
- 238000004073 vulcanization Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000007723 die pressing method Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000002441 reversible effect Effects 0.000 description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 3
- 230000005526 G1 to G0 transition Effects 0.000 description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 3
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 3
- 238000010060 peroxide vulcanization Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000007334 memory performance Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- WJCRZORJJRCRAW-UHFFFAOYSA-N cadmium gold Chemical compound [Cd].[Au] WJCRZORJJRCRAW-UHFFFAOYSA-N 0.000 description 1
- 229920003020 cross-linked polyethylene Polymers 0.000 description 1
- 239000004703 cross-linked polyethylene Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012781 shape memory material Substances 0.000 description 1
- 239000002520 smart material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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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
- G01N2203/0019—Compressive
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Abstract
The invention provides an effective method for quantitatively evaluating the shape memory behavior of thermoplastic vulcanizate in a compression mode, which is a characterization method of the shape memory behavior of the thermoplastic vulcanizate in the compression mode. The quantitative characterization method comprises the following steps: (1) the initial height of the cylindrical thermoplastic vulcanizate sample is recorded as H0Then fixing the mixture on a simple compression clamp, and preheating for 10 min; (2) applying external force to deform the preheated thermoplastic vulcanizate sample, then quickly immersing the sample into an ice-water mixture for shaping, and recording the height of the sample as H1(ii) a (3) Removing external force, naturally standing the sample at room temperature for 24hr, and recording the height of the sample as H2(ii) a (4) Placing the thermoplastic vulcanizate sample in (3) in the temperature rising environment in (1), and recording the height of the sample as H3(ii) a (5) Calculating the shape of thermoplastic vulcanizatesFixation (SF) and Strain Recovery (SR), respectively:
Description
Technical Field
The invention belongs to the technical field of functional polymer materials, and particularly relates to a method for characterizing shape memory behavior of thermoplastic vulcanized rubber in a compression mode, in particular to a method for quantitatively characterizing shape memory performance of thermoplastic vulcanized rubber in the compression mode by examining shape fixation rate and deformation recovery rate.
Background
Shape memory materials are a new class of smart materials. Shape memory means that a solid material with a certain shape generates plastic deformation under a specific condition, the plastic deformation can be eliminated under the stimulation of different external environment changes (such as temperature, force, electromagnetism, solvent, humidity and the like), and the solid material can restore to the original shape. As early as 30 s in the 20 th century, the shape memory phenomenon was discovered by Olander in gold-cadmium alloys for the first time; charlesby accidentally heated crosslinked polyethylene which deforms under tension in one experiment in the 60 s of the 20 th century, and discovered the peculiar phenomenon of the shape memory polymer for the first time; in recent years, shape memory polymers have advantages of light weight, low cost, large deformation amount, easy deformation, easy adjustment of shape recovery temperature, and the like, and exhibit superior performance in the fields of aerospace, biomedicine, sensing braking, and the like, and industries related to the shape memory polymers are developing vigorously, thereby bringing about great economic and social benefits.
Generally, a polymer material with shape memory behavior can be regarded as being composed of two phases, namely a stationary phase for memorizing an original shape and a reversible phase for realizing temporary shape memory and recovery by changing under external stimulus; the stationary phase of the shape memory polymer material is generally a cross-linked structure of a polymer or a physical entanglement of a molecular chain, and the reversible phase is generally a phase structure in which reversible phase transition can occur in the polymer material, and the switching temperature is generally a glass transition temperature or a melting point. However, current studies on the shape memory behavior of thermoplastic vulcanizates are generally conducted using only tensile and flexural modes for testing and characterization; in fact, the thermoplastic vulcanized rubber can generate the shape memory effect under the compression mode, and the representation of the compression shape memory behavior has important significance in both theoretical research and practical application, but a quantitative representation method of the compression shape memory behavior which is generally accepted by people is not seen so far. Compared with the shape memory behavior in a stretching mode and a bending mode, the shape memory behavior of the thermoplastic vulcanizate in the compression mode can overcome the problems of low melt strength of a stationary phase in the shape memory polymer material, small stretching strain caused by poor combination of two-phase interfaces and the like, and can provide stronger elastic recovery driving force in the reversible phase recovery process, so that the thermoplastic vulcanizate has more excellent shape fixation rate and deformation recovery rate.
The shape memory behavior of the thermoplastic vulcanizate in the compression mode is an important property of the thermoplastic vulcanizate, and the research on the shape memory behavior of the thermoplastic vulcanizate is only limited to a stretching mode and a bending mode at present, but no report is made about the shape memory behavior in the compression mode, so that a quantitative characterization method for the shape memory behavior of the thermoplastic vulcanizate in the compression mode is urgently needed.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a method for representing shape memory behavior of thermoplastic vulcanizate in a compression mode, which solves the problem that no method for representing shape memory behavior of thermoplastic vulcanizate in the compression mode is generally accepted by people at present.
The technical scheme is as follows: the characterization method of the shape memory behavior of the thermoplastic vulcanizate in the compression mode adopts the simple compression clamp to test the shape memory performance of the cylindrical thermoplastic vulcanizate sample, has the advantages of simple preparation, adjustable flexibility, easy molding, recycling, low switching temperature, excellent performance in the aspects of shape fixation rate and deformation recovery rate, important scientific significance and application prospect, and the specific steps are as follows:
(1) the initial height of the cylindrical thermoplastic vulcanizate sample is recorded as H0Then fixing the composite material on a simple compression clamp, and preheating for 10min in a specific environment; the specific temperature is typically near its melting point if the matrix thermoplastic of the thermoplastic vulcanizate is a crystalline polymer, and near its glass transition temperature if the matrix thermoplastic of the thermoplastic vulcanizate is an amorphous polymer;
(2) circle after preheatingA columnar sample, under the condition of preheating temperature, applying external force on a compression clamp to deform the sample, after reaching the specified deformation, rapidly immersing the compression clamp and the sample into an ice-water mixture under the condition of maintaining the external force, wherein the height of the sample is H1；
(3) Taking off the cylindrical sample from the simple compression fixture, and naturally standing at room temperature for 24hr to obtain a sample with height of H2；
(4) Placing the cylindrical sample in the step (3) in the specific temperature environment in the step (1), and testing after 5min, wherein the height of the sample is H3；
(5) The calculation formulas of the shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material under the thermoplastic vulcanizate compression mode are respectively as follows:
compression set of cylindrical thermoplastic vulcanizate is achieved by uniformly applying equal but opposite compressive forces to its upper and lower parallel surfaces, and during compression, the sides of the cylindrical specimen typically expand outwardly. If the side surface of the cylindrical sample is bent and deformed in the compression process to form a barrel-shaped appearance with thin upper part and thin lower part and thick middle part, the stress applied to the sample is not uniform, and the reliability of the test result is influenced; in the test process, in order to avoid the appearance of a barrel shape of the sample in the compression process, a thin layer of lubricant (methyl silicone oil) is generally coated on the upper and lower parallel surfaces of the cylindrical sample, so that the upper and lower surfaces can slide well under the compressive stress in the compression process, the cylindrical sample can be compressed uniformly without generating a remarkable appearance of the barrel shape, and the reliability of the test result is ensured.
Has the advantages that: the invention provides a characterization method of shape memory behavior of thermoplastic vulcanizate in compression mode, and provides an effective method for quantitative evaluation of shape memory behavior of thermoplastic vulcanizate in compression mode.
Drawings
FIG. 1 is a graph showing the process of testing the shape memory properties of a thermoplastic vulcanizate obtained in example 2 of the present invention in a compression mode, wherein: FIG. 1a is an initial view of a sample before compression of a thermoplastic vulcanizate, FIG. 1b is a view of a sample after compression to set, and FIG. 1c is a view of a sample after deformation recovery.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1: quantitative characterization of shape memory behavior in EVA/NBR thermoplastic vulcanizate compression mode
A cylindrical EVA (ethylene-vinyl acetate copolymer)/NBR (nitrile-butadiene rubber) (mass ratio of 50/50) vulcanized rubber sample is prepared by a die pressing method, the height of the sample is 10mm, the sample is prepared by dynamic vulcanization of a peroxide vulcanization system, the EVA brand is 3135SB, the vinyl acetate content is 12%, the NBR brand is N41, the acrylonitrile content is 29%, and the sample does not have air bubbles, impurities or damage.
(1) The initial height of the cylindrical ethylene vinyl acetate/nitrile rubber thermoplastic vulcanizate sample is recorded as H0Fixing the powder on a simple compression clamp for 10.00mm, and preheating for 10min at the temperature of 95 ℃;
(2) applying external force to a compression clamp at 95 ℃ to deform the preheated cylindrical thermoplastic vulcanizate sample, rapidly immersing the compression clamp and the sample into an ice-water mixture to cool and shape under the condition of maintaining the external force after the sample is deformed by 50 percent, wherein the height of the sample is H at the moment1＝5.00mm；
(3) Taking off cylindrical thermoplastic vulcanizate sample from simple compression fixture, and naturally standing at room temperature for 24hr to obtain sample with height of H2＝5.11mm；
(4) Putting the cylindrical thermoplastic vulcanizate sample in the step (3) into an environment at 95 ℃ again, and after 5min, the height of the sample is H3＝9.91mm；
(5) The shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material of the ethylene-vinyl acetate copolymer/nitrile rubber thermoplastic vulcanizate are respectively 97.89% and 98.16%.
Example 2: quantitative characterization of shape memory behavior in EVA/NBR thermoplastic vulcanizate compression mode
A cylindrical EVA (ethylene-vinyl acetate copolymer)/NBR (nitrile-butadiene rubber) (mass ratio of 60/40) vulcanized rubber sample is prepared by a die pressing method, the height of the sample is 10mm, the sample is prepared by dynamic vulcanization of a peroxide vulcanization system, the EVA brand is 3135SB, the vinyl acetate content is 12%, the NBR brand is N41, the acrylonitrile content is 29%, and the sample does not have air bubbles, impurities or damage.
(1) The initial height of the cylindrical ethylene vinyl acetate/nitrile rubber thermoplastic vulcanizate sample is recorded as H0Fixing the powder on a simple compression clamp at 10.00mm, and preheating at 95 ℃ for 10 min;
(2) applying external force to a compression clamp at 95 ℃ to deform the preheated cylindrical thermoplastic vulcanizate sample, rapidly immersing the compression clamp and the sample into an ice-water mixture to cool and shape under the condition of maintaining the external force after the sample is deformed by 50 percent, wherein the height of the sample is H at the moment1＝5.00mm；
(3) Taking off cylindrical thermoplastic vulcanizate sample from simple compression fixture, and naturally standing at room temperature for 24hr to obtain sample with height of H2＝5.07mm；
(4) Putting the cylindrical thermoplastic vulcanizate sample in the step (3) into an environment at 95 ℃ again, and after 5min, the height of the sample is H3＝9.88mm；
(5) The shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material of the ethylene-vinyl acetate copolymer/nitrile rubber thermoplastic vulcanizate are calculated to be 98.60 percent and 97.57 percent respectively.
Example 3: quantitative characterization of shape memory behavior under compression of EVA/NBR thermoplastic vulcanizate
A cylindrical EVA (ethylene-vinyl acetate copolymer)/NBR (nitrile-butadiene rubber) (mass ratio of 70/30) vulcanized rubber sample is prepared by a die pressing method, the height of the sample is 10mm, the sample is prepared by dynamic vulcanization of a peroxide vulcanization system, the EVA brand is 3135SB, the vinyl acetate content is 12%, the NBR brand is N41, the acrylonitrile content is 29%, and the sample does not have air bubbles, impurities or damage.
(1) The initial height of the cylindrical ethylene vinyl acetate/nitrile rubber thermoplastic vulcanizate sample is recorded as H0Fixing the powder on a simple compression clamp at 10.00mm, and preheating at 95 ℃ for 10 min;
(2) applying external force to a compression clamp at 95 ℃ to deform the preheated cylindrical thermoplastic vulcanizate sample, rapidly immersing the compression clamp and the sample into an ice-water mixture to cool and shape under the condition of maintaining the external force after the sample is deformed by 50 percent, wherein the height of the sample is H at the moment1＝5.00mm；
(3) Taking off cylindrical thermoplastic vulcanizate sample from simple compression fixture, and naturally standing at room temperature for 24hr to obtain sample with height of H2＝5.02mm；
(4) Putting the cylindrical thermoplastic vulcanizate sample in the step (3) into an environment at 95 ℃ again, and after 5min, the height of the sample is H3＝9.79mm；
(5) The shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material of the ethylene-vinyl acetate copolymer/nitrile rubber thermoplastic vulcanizate are respectively 99.55 percent and 95.78 percent.
Example 4: quantitative characterization of shape memory behavior in EAA/CR thermoplastic vulcanizate compression mode
A cylindrical EAA (ethylene-acrylic acid copolymer)/CR (chloroprene rubber) (mass ratio is 60/40) vulcanized rubber sample is prepared by a die pressing method, the height of the sample is 10mm, the sample is prepared by dynamic vulcanization of a metal oxide vulcanization system, the EAA is N300, the acrylic acid content is 9.7%, the CR is SN244X, and the sample has no bubbles, impurities and damage.
(1) The initial height of the cylindrical ethylene-acrylic acid copolymer/chloroprene rubber thermoplastic vulcanizate sample is recorded as H0Fixing the powder on a simple compression clamp at 10.00mm, and preheating at 95 ℃ for 10 min;
(2) preheating cylindrical thermoplastic vulcanizate samples inApplying external force on the compression clamp at 95 ℃ to deform the sample to 50%, rapidly immersing the compression clamp and the sample into an ice-water mixture to cool and shape under the condition of maintaining the external force, wherein the height of the sample is H1＝5.00mm；
(3) Taking off cylindrical thermoplastic vulcanizate sample from simple compression fixture, and naturally standing at room temperature for 24hr to obtain sample with height of H2＝5.41mm；
(4) Putting the cylindrical thermoplastic vulcanizate sample in the step (3) into an environment at 95 ℃ again, and after 5min, the height of the sample is H3＝9.55mm；
(5) The shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material of the ethylene-acrylic acid copolymer/chloroprene rubber thermoplastic vulcanizate are calculated to be 91.81 percent and 90.20 percent respectively.
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 shape memory behavior of thermoplastic vulcanizate in compression mode, said method comprising the steps of:
(1) the initial height of the cylindrical thermoplastic vulcanizate sample is recorded as H0Then fixing the composite material on a simple compression clamp, and preheating for 10min at a specific temperature; the specific temperature is typically near its melting point if the matrix thermoplastic of the thermoplastic vulcanizate is a crystalline polymer, and near its glass transition temperature if the matrix thermoplastic of the thermoplastic vulcanizate is an amorphous polymer;
(2) the preheated cylindrical sample is subjected to preheating temperature conditionThen, an external force is applied to the compression jig to deform the sample to a predetermined deformation, and then the compression jig and the sample are quickly immersed in an ice-water mixture while maintaining the external force, wherein the height of the sample is H1；
(3) Taking off the cylindrical sample from the simple compression fixture, and naturally standing at room temperature for 24hr to obtain a sample with height of H2；
(4) Placing the cylindrical sample in (3) at the temperature in (1), and testing after 5min, wherein the height of the sample is H3；
(5) The calculation formulas of the shape fixing rate (SF) and the deformation recovery rate (SR) of the shape memory polymer material under the thermoplastic vulcanizate compression mode are respectively as follows:
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| US20020157478A1 (en) * | 2001-04-26 | 2002-10-31 | Seale Joseph B. | System and method for quantifying material properties |
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| CN110308053A (en) * | 2019-07-18 | 2019-10-08 | 青岛科技大学 | A kind of preparation method of the shape-memory material based on thermoplastic sulfurized rubber |
| CN110346549A (en) * | 2019-08-14 | 2019-10-18 | 南京林业大学 | A kind of evaluation method of modified gutta-percha shape-memory properties |
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- 2020-11-06 CN CN202011231025.4A patent/CN112284904A/en active Pending
Patent Citations (7)
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|---|---|---|---|---|
| US20020157478A1 (en) * | 2001-04-26 | 2002-10-31 | Seale Joseph B. | System and method for quantifying material properties |
| CN107400344A (en) * | 2017-06-29 | 2017-11-28 | 华南理工大学 | Ultra-toughness PLA/NBR bio-based thermoplastic sulfurized rubbers with shape memory function and preparation method thereof |
| CN107561253A (en) * | 2017-08-23 | 2018-01-09 | 南京林业大学 | A kind of sealing material shape-memory properties evaluation method of mist containing sand |
| CN108503941A (en) * | 2018-04-12 | 2018-09-07 | 青岛科技大学 | A kind of preparation method of the shape memory high molecule material based on thermoplastic sulfurized rubber |
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| CN110308053A (en) * | 2019-07-18 | 2019-10-08 | 青岛科技大学 | A kind of preparation method of the shape-memory material based on thermoplastic sulfurized rubber |
| CN110346549A (en) * | 2019-08-14 | 2019-10-18 | 南京林业大学 | A kind of evaluation method of modified gutta-percha shape-memory properties |
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