CN108469388A - The prediction technique of high polymer dynamic storage modulus under wet heat condition - Google Patents
The prediction technique of high polymer dynamic storage modulus under wet heat condition Download PDFInfo
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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
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Abstract
The present invention relates to a kind of prediction techniques of high polymer dynamic storage modulus under wet heat condition.Linear correlation of this method based on glass transition temperature and relative humidity, the dynamic storage modulus of high polymer is described using hyperbolic tangent function；Pass through warm and humid coupling factor and viscoelastic function of state, obtain EVOLUTION EQUATION of the high polymer dynamic storage modulus with temperature and relative humidity, and material parameter therein is determined respectively with reference to the temperature scanning dynamic test under humidity by 2 kinds, the prediction technique of high polymer dynamic modulus under wet heat condition is obtained accordingly.The present invention can influence of the Accurate Prediction temperature and humidity to dynamic mechanical behavior, be on active service valuable help be provided for the safety of polymer and its composite material.
Description
Technical field
The present invention relates to a kind of prediction technique of high polymer dynamic storage modulus in hygrothermal environment, be mainly used for polymer and
The optimization design of its composite material and in-service performance evaluation, belong to Polymer Mechanical field.
Background technology
High molecular polymer makes it have unrivaled feature performance benefit and is widely used in life because of unique molecular structure
The numerous areas such as life science, aerospace, microelectronics Packaging and building.Involved amorphous and partially crystallizable high polymer size
It is smaller, surface area is larger, therefore extremely sensitive to the variation of Service Environment factor.The increase of wherein temperature and humidity provides not only
More free volumes, and weaken the hydrogen bond connection for even destroying polymer molecule, Key Performance Indicator-mould of material
Thus amount is remarkably decreased, partly or entirely lose use value so as to cause it.Therefore, under accurate evaluation and prediction wet heat condition
Dynamic storage modulus be the key that avoid such functional material unstability, failure.Due to time temperature equivalence principle and hot Theory of Viscoelasticity
Development, temperature is more mature to the Effect on Mechanical Properties mechanism of polymer and its composite material, establishes from glassy state
Modulus in rubbery state universe is with Temperature Evolution equation, such as polymer chain damage model, the list extended by population logical model
Parameter stiffness method, the semi analytic formula etc. based on Wei Bo distribution and Arrhenius function.In recent years, hygrothermal environment is to viscoelastic material
Though the influence research of mechanical behavior also obtains impressive progress, obtain viscous containing damp and hot coupled linear for isotropic material
Elastic constitutive relation, and corresponding heat transfer and coupling moisture diffusion equation；Polymer matrix is had studied based on homogenization theory
The wet viscoelastic property of composite material gives equivalent wet Relaxation Modulus and equivalent hygral expansion coefficient.However, the above method
Coupling influence of the temperature and humidity to high polymer dynamic storage modulus can not be described.
Invention content
It is insufficient it is an object of the invention to be directed to existing for prior art, middle high polymer dynamic under a kind of wet heat condition is provided
The prediction technique of storage modulus, it is amorphous under wet heat condition or partially crystallizable state polymer dynamic storage modulus accurate to be suitable for
Prediction.
The present invention thinking be：1. determining that glass transition temperature and relative humidity are linear according to free volume theory and experiment
Correlation；2. describing high polymer dynamic storage modulus variation with temperature rule using hyperbolic tangent function, and referred to by 2 kinds
Temperature scanning dynamic test under humidity determines the material parameter in formula respectively；4. being based on warm and humid coupling factor and viscoelastic shape
State function provides EVOLUTION EQUATION of the high polymer dynamic storage modulus with temperature and humidity respectively, thus to obtain high under wet heat condition
The prediction technique of polymers dynamic modulus.
Conceived according to foregoing invention, the present invention uses following technical proposals：
Amorphous or partially crystallizable state polymer dynamic storage modulus prediction technique under a kind of hygrothermal environment, feature exist
It is as follows in analytical procedure：
A., amorphous or partially crystallizable state polymer samples are placed in the dynamic mechanical analysis of configuration humid control attachment
It is 24 hours dry in the environment that temperature is 25 ± 0.1 DEG C, relative humidity is 0 ± 1% in instrument；
B. 2 are chosen within the scope of 0-90% with reference to relative humidity RH1And RH2, using etc. it is wet when temperature scanning pattern,
To film test piece implement linear-viscoelastic range dynamic mechanical test, respectively in real time record drafting material storage modulus E ' (T) and
Loss modulus E " (T) with environment temperature T by glassy state to rubbery state universe range when E ' (T)-T and E " (T)-T curve；
C. based on E, " peak value of (T)-T curve determines the glass transition temperature T under corresponding humidityg(RH)；
D. according to relative humidity RH1And RH2And its glass transition temperature Tg(RH1) and Tg(RH2) data, and by following formula
(1) glass transition temperature T is determinedg(RH) with the linear change of relative humidity RH：
E. hyperbolic tangent function shown in following formula (2) is used to describe high polymer dynamic storage modulus E ' (T, RH) with temperature
The changing rule of T：Wherein E 'UAnd ER′RRespectively the initial and final storage modulus before and after glass transition, φ occur for high polymer
(T, RH) and λ (RH) are then that warm and humid coupling function and humidity are plasticized the factor,
F. φ (T, RH) and λ (RH) are determined by following formula (3) and formula (4) respectively：Wherein material parameter α, β, γ and η is by phase
To humidity RH1And RH2Under temperature scanning E ' (T)-T trial curves fitting determine,
λ (RH)=γ RH+ η (4)
G. in summary formula (1)-formula (4), you can the dynamic energy storage mould of high polymer under the conditions of general temperature and humidity
Amount.
The present invention compared with prior art, protrudes substantive distinguishing features and remarkable advantage is：Only it need to pass through 2 groups of constant humidity items
Temperature scanning dynamic mechanical test under part obtains relevant material parameters, you can obtains high polymer dynamic storage modulus with wet heat condition
Evolution.Hereby it is possible to the dynamic mechanical behavior under the other temperature of Accurate Prediction and relative humidity, for polymer and its again
The safety of condensation material, which is on active service, provides valuable help.
Description of the drawings
Polyvinyl alcohol dynamic mechanical-temperature curve when Fig. 1 is 0%RH.
Polyvinyl alcohol dynamic mechanical-temperature curve when Fig. 2 is 30%RH.
Polyvinyl chloride dynamic mechanical-temperature curve when Fig. 3 is 20%RH.
Polyvinyl chloride dynamic mechanical-temperature curve when Fig. 4 is 60%RH.
Fig. 5 is the comparison of polyvinyl alcohol dynamic storage modulus predicted value and test data under different temperature and humidity conditions.
Fig. 6 is the comparison of polyvinyl chloride dynamic storage modulus predicted value and test data under different temperature and humidity conditions.
Specific implementation mode
Details are as follows for the preferred embodiment combination attached drawing of the present invention：
Embodiment one：
Steps are as follows for the Analysis of Prediction of high polymer dynamic storage modulus under this wet heat condition：
1. 10 grams of PVA powder are slowly added in 90 milliliters 25 DEG C of distilled water, 95 DEG C are gradually heated to, stirring and dissolving 3
The PVA film that geometric dimension (long x wide x are thick) is 20mm × 5mm × 0.03mm is made to room temperature, and by sol evenning machine in hour postcooling
Tensile sample；2. test specimen is put into constant temperature, the constant humidity cabinet that temperature is 120 DEG C, 30 minutes are annealed to eliminate its prestressing force, then with 5
DEG C/h speed be cooled to room temperature at a slow speed, be placed in drying basin；3. on TA Q800 dynamic mechanical analyzers (DMA),
Apply the dynamic tensile load (frequency 1Hz) of 3.5MPa to film sample, and relative humidity is carried out by the humidity attachment of DMA
Temperature scanning when respectively 0% and 30%, wherein temperature scan rate are 1 DEG C/min.Under the conditions of two kinds of record etc. is wet respectively
Material storage modulus and loss modulus with temperature by 10-100 DEG C of consecutive variations when E ' (T)-T and E " (T)-T trial curves
(such as Fig. 1 and Fig. 2)；4. " peak value of (T)-T curve determines the glass transition temperature temperature under 0% and 30% relative humidity based on E
Spend Tg(RH1) and Tg(RH2) be respectively：71.7 DEG C and 45.3 DEG C, and by formula (1) determine glass transition relative temperature with it is opposite
The evolution equation of humidity linear correlation.5. using formula (1)-formula (4) description PVA dynamic storage modulus E ' (T, RH) with warm and humid
The changing rule of coupling, wherein obtained material parameter α, β, γ and η are respectively 250.0,4.5,0.285 and 0.075.
Embodiment two：
Steps are as follows for the Analysis of Prediction of high polymer dynamic storage modulus under this wet heat condition：
1. geometric dimension (long x wide x are thick), which is respectively prepared, in amorphous polyvinyl chloride (PVC) film that thickness is 0.20mm is：
The DMA tensile samples of isothermal water adsorption sample and 20mm × 5mm × 0.20mm of 5mm × 5mm × 0.20mm；2. test specimen is put
Enter constant temperature, the constant humidity cabinet that temperature is 110 DEG C, anneals 120 minutes to eliminate its prestressing force, then cold at a slow speed with 5 DEG C/h of speed
But it to room temperature, is placed in drying basin；3. on TA Q800 dynamic mechanical analyzers (DMA), PVC film sample is applied
The dynamic tensile load (frequency 1Hz) of 2MPa, and carried out when relative humidity is 20% and 60% by the humidity attachment of DMA
Temperature scanning, wherein temperature scan rate are 1 DEG C/min.Material storage modulus and damage under the conditions of two kinds of record etc. is wet respectively
Consume modulus with temperature by 35-100 DEG C of consecutive variations when E ' (T)-T and E " (T)-T trial curves (such as Fig. 3 and Fig. 4)；4. being based on
The peak value of E " (T)-T curve determines the glass transition temperature temperature T under 20% and 60% relative humidityg(RH1) and Tg(RH2)
Respectively：79.7 DEG C and 72.2 DEG C, and evolution of the glass transition relative temperature with relative humidity linear correlation is determined by formula (1)
Equation.5. using formula (1)-formula (4) description PVC dynamic storage modulus E ' (T, RH) with the evolution of warm and humid coupling, wherein material
Parameter alpha, β, γ and η are respectively 328.3,6.0,0 and 0.179.
The PVA that above formula (1)-formula (4) is predicted and the experiment number under PVC dynamic storage modulus and corresponding experimental condition
According to being compared in Fig. 5 and Fig. 6, it can be found that the method for the present invention has higher computational accuracy.
Claims (1)
1. the prediction technique of polymer dynamic storage modulus under a kind of hygrothermal environment, it is characterised in that analytical procedure is as follows：
A. amorphous or partially crystallizable state polymer samples are placed in the dynamic mechanical analyzer of configuration humid control attachment,
It is 24 hours dry in the environment that temperature is 25 ± 0.1 DEG C, relative humidity is 0 ± 1%；
B. 2 are chosen within the scope of 0-90% with reference to relative humidity RH1And RH2, using etc. it is wet when temperature scanning pattern, to thin
Film test specimen implements the dynamic mechanical test of linear-viscoelastic range, respectively record drafting material storage modulus E ' (T) and loss in real time
Modulus E " (T) with environment temperature T by glassy state to rubbery state universe range when E ' (T)-T and E " (T)-T curve；
C. based on E, " peak value of (T)-T curve determines the glass transition temperature T under corresponding humidityg(RH)；
D. according to relative humidity RH1And RH2And its glass transition temperature Tg(RH1) and Tg(RH2) data, and by following formula (1)
Determine glass transition temperature Tg(RH) with the linear change of relative humidity RH：
E. hyperbolic tangent function shown in following formula (2) is used to describe high polymer dynamic storage modulus E ' (T, RH) with temperature T's
Changing rule, wherein E 'UAnd ER′RInitial and final storage modulus respectively before and after high polymer generation glass transition, φ (T,
RH) and λ (RH) is then that warm and humid coupling function and humidity are plasticized the factor,
F. φ (T, RH) and λ (RH) are determined by following formula (3) and formula (4) respectively：Wherein material parameter α, β, γ and η is by relatively wet
Spend RH1And RH2Under temperature scanning E ' (T)-T trial curves fitting determine,
λ (RH)=γ RH+ η (4)
G. in summary formula (1)-formula (4), you can the dynamic storage modulus of high polymer under the conditions of general temperature and humidity.
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| CN112525948A (en) * | 2020-11-19 | 2021-03-19 | 西安交通大学 | Method for realizing three glass transition temperature tests by using nano-mechanical tester |
| CN113064459A (en) * | 2021-03-11 | 2021-07-02 | 中国科学技术大学 | Method for regulating and controlling strength and toughness of cellulose film through humidity |
| CN113720872A (en) * | 2021-08-09 | 2021-11-30 | 浙江省林业科学研究院 | Method for testing curing characteristics of water-soluble low-molecular-weight resin based on dynamic thermo-mechanical method |
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| CN113064459A (en) * | 2021-03-11 | 2021-07-02 | 中国科学技术大学 | Method for regulating and controlling strength and toughness of cellulose film through humidity |
| CN113720872A (en) * | 2021-08-09 | 2021-11-30 | 浙江省林业科学研究院 | Method for testing curing characteristics of water-soluble low-molecular-weight resin based on dynamic thermo-mechanical method |
| CN113720872B (en) * | 2021-08-09 | 2023-08-11 | 浙江省林业科学研究院 | Method for testing curing characteristics of water-soluble low molecular weight resin based on dynamic thermo-mechanical method |
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