CN108469388B - Prediction method of dynamic storage modulus of high polymer under damp and hot conditions - Google Patents

Prediction method of dynamic storage modulus of high polymer under damp and hot conditions Download PDF

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CN108469388B
CN108469388B CN201810100837.1A CN201810100837A CN108469388B CN 108469388 B CN108469388 B CN 108469388B CN 201810100837 A CN201810100837 A CN 201810100837A CN 108469388 B CN108469388 B CN 108469388B
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胡宏玖
张柯烽
张晓龙
贺耀龙
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Abstract

The invention relates to a method for predicting dynamic storage modulus of a high polymer under a damp and hot condition. The method is based on the linear correlation between the glass transition temperature and the relative humidity, and adopts a hyperbolic tangent function to describe the dynamic storage modulus of a high polymer; the evolution equation of the dynamic storage modulus of the high polymer along with the temperature and the relative humidity is obtained through the temperature-humidity coupling factor and the viscoelastic state function, and the material parameters are respectively determined through the temperature scanning dynamic mechanical test under 2 reference humidities, so that the prediction method of the dynamic modulus of the high polymer under the damp-heat condition is obtained. The method can accurately predict the influence of temperature and humidity on the dynamic mechanical behavior, and provides important help for the safe service of the polymer and the composite material thereof.

Description

Prediction method of dynamic storage modulus of high polymer under damp and hot conditions
Technical Field
The invention relates to a prediction method of dynamic storage modulus of a high polymer in a damp and hot environment, which is mainly used for the optimization design and the in-service performance evaluation of the polymer and a composite material thereof and belongs to the field of high polymer material mechanics.
Background
Due to the unique molecular structure, the high molecular polymer has incomparable performance advantages and is widely applied to the fields of life sciences, aerospace, microelectronic packaging, buildings and the like. The related amorphous and partially crystalline high polymers have small size and large surface area, so the amorphous and partially crystalline high polymers are extremely sensitive to changes of service environment factors. Wherein the increase in temperature and humidity not only provides more free volume but also weakens or even destroys the hydrogen bonding of the polymer molecules, the key performance indicator of the material-modulus is thereby significantly reduced, resulting in its partial or total loss of value in use. Therefore, the accurate evaluation and prediction of the dynamic storage modulus under the damp and hot conditions is the key to avoid the instability and the failure of the functional materials. Due to the development of a time-temperature equivalent principle and a thermal viscoelastic theory, the mechanism of influence of temperature on the mechanical properties of polymers and composite materials thereof is mature, and equations of evolution of modulus along with temperature in a whole range from a glass state to a rubber state are established, such as a polymer chain damage model, a single-parameter rigidity method expanded by a population logic model, a semi-analytic equation based on WeiPo distribution and an Arrhenius function and the like. In recent years, although the research on the influence of a damp and hot environment on the mechanical behavior of a viscoelastic material is also greatly advanced, a damp and hot coupling-containing linear viscoelastic constitutive relation aiming at an isotropic material and a corresponding heat conduction and coupling moisture diffusion equation are obtained; the wet viscoelasticity characteristic of the polymer matrix composite material is researched based on the homogenization theory, and the equivalent wet stress relaxation modulus and the equivalent wet expansion coefficient are given. However, none of the above methods describe the coupling effect of temperature and humidity on the dynamic storage modulus of the high polymer.
Disclosure of Invention
The invention aims to provide a method for predicting the dynamic storage modulus of a high polymer under a damp and hot condition aiming at the defects in the prior art, and the method is suitable for accurately predicting the dynamic storage modulus of an amorphous or partially crystalline polymer under the damp and hot condition.
The idea of the invention is as follows: firstly, determining a linear correlation formula of glass transition temperature and relative humidity according to a free volume theory and a test; describing the change rule of the dynamic storage modulus of the high polymer along with the temperature by adopting a hyperbolic tangent function, and respectively determining the material parameters in the formula through a temperature scanning dynamic mechanical test under 2 reference humidities; and fourthly, respectively giving out an evolution equation of the dynamic storage modulus of the high polymer along with the temperature and the humidity based on the temperature-humidity coupling factor and the viscoelastic state function, thereby obtaining the prediction method of the dynamic modulus of the high polymer under the damp and hot condition.
According to the inventive concept, the invention adopts the following technical scheme:
a method for predicting the dynamic storage modulus of an amorphous or partially crystalline polymer in a damp and hot environment is characterized by comprising the following analysis steps:
a. placing an amorphous or partially crystalline polymer sample into a dynamic mechanical analyzer equipped with a humidity control accessory, and drying for 24 hours in an environment with the temperature of 25 +/-0.1 ℃ and the relative humidity of 0 +/-1%;
b. selecting 2 reference relative humidities RH within the range of 0-90%1And RH2The method comprises the following steps of performing dynamic mechanical test of a linear viscoelastic range on a thin film test piece by adopting a temperature scanning mode in the equal humidity state, and respectively recording and drawing E '(T) -T and E' (T) -T curves of a material when the storage modulus E '(T) and the loss modulus E' (T) are changed along with the environmental temperature T from the glass state to the rubber state in a global range in real time;
c. determining the glass transition temperature T at the corresponding humidity based on the peak value of the E' (T) -T curveg(RH)；
d. According to relative humidity RH1And RH2And its glass transition temperature Tg(RH1) And Tg(RH2) Data and the glass transition temperature T was determined by the following formula (1)g(RH) linear variation with relative humidity RH:
Figure BDA0001566278890000021
e. the change rule of the dynamic storage modulus E' (T, RH) of the high polymer along with the temperature T is described by adopting a hyperbolic tangent function shown in the following formula (2): wherein E'UAnd ER′RInitial and final storage moduli before and after the glass transition of the high polymer, phi (T, RH) and lambda (RH) are temperature-humidity coupling function and humidity plasticizing factor,
Figure BDA0001566278890000022
f. phi (T, RH) and lambda (RH) are determined by the following formulas (3) and (4), respectively: wherein the material parameters alpha, beta, gamma and eta are defined by relative humidity RH1And RH2Temperature sweep E' (T) -T test curve fitting,
Figure BDA0001566278890000023
λ(RH)＝γ·RH+η (4)
g. by combining the above formula (1) to formula (4), the dynamic storage modulus of the high polymer under ordinary temperature and humidity conditions can be obtained.
Compared with the prior art, the invention has the prominent substantive characteristics and remarkable advantages that: the evolution rule of the dynamic storage modulus of the high polymer along with the damp and hot conditions can be obtained only by obtaining related material parameters through 2 groups of temperature scanning dynamic mechanical tests under the constant humidity condition. Therefore, the dynamic mechanical behavior under other temperatures and relative humidity can be accurately predicted, and important help is provided for the safe service of the polymer and the composite material thereof.
Drawings
FIG. 1 is a dynamic mechanical properties-temperature curve of polyvinyl alcohol at 0% RH.
FIG. 2 is a dynamic mechanical properties-temperature curve of polyvinyl alcohol at 30% RH.
FIG. 3 is a dynamic mechanical properties-temperature curve of polyvinyl chloride at 20% RH.
FIG. 4 is a dynamic mechanical properties-temperature curve of polyvinyl chloride at 60% RH.
FIG. 5 is a comparison of predicted values of the dynamic storage modulus of polyvinyl alcohol under different temperature and humidity conditions with experimental data.
FIG. 6 is a comparison of the predicted values of the dynamic storage modulus of polyvinyl chloride under different temperature and humidity conditions with the test data.
Detailed Description
Preferred embodiments of the present invention are described in detail below with reference to the accompanying drawings:
the first embodiment is as follows:
the prediction method of the dynamic storage modulus of the high polymer under the damp and hot condition comprises the following analysis steps:
slowly adding 10 g of PVA powder into 90 ml of distilled water at 25 ℃, gradually heating to 95 ℃, stirring and dissolving for 3 hours, cooling to normal temperature, and preparing a PVA film tensile sample with the geometric dimension (length, width and thickness) of 20mm multiplied by 5mm multiplied by 0.03mm by a spin coater; placing the test piece into a constant temperature and constant humidity box with the temperature of 120 ℃, annealing for 30 minutes to eliminate the prestress of the test piece, cooling the test piece to room temperature at the speed of 5 ℃/hour, and placing the test piece into a drying dish; thirdly, applying a dynamic tensile load (frequency is 1Hz) of 3.5MPa to the film sample on a TA Q800 Dynamic Mechanical Analyzer (DMA), and carrying out temperature scanning when the relative humidity is 0 percent and 30 percent respectively through a humidity accessory of the DMA, wherein the temperature scanning speed is 1 ℃/minute. Respectively recording E '(T) -T and E' (T) -T test curves of the material under two equal wet conditions when the storage modulus and the loss modulus of the material are continuously changed along with the temperature from 10 ℃ to 100 ℃ (shown in figure 1 and figure 2); determination of the glass transition temperature T at 0% and 30% relative humidity based on the peak of the E' (T) -T curveg(RH1) And Tg(RH2) Respectively as follows: 71.7 ℃ and 45.3 ℃, and determining an evolution equation of the linear correlation of the relative temperature of the glass transition and the relative humidity by the formula (1). And describing the change rule of the dynamic storage modulus E' (T, RH) of the PVA according to the temperature-humidity coupling by adopting a formula (1) to a formula (4), wherein the obtained material parameters alpha, beta, gamma and eta are 250.0, 4.5, 0.285 and 0.075 respectively.
Example two:
the prediction method of the dynamic storage modulus of the high polymer under the damp and hot condition comprises the following analysis steps:
amorphous polyvinyl chloride (PVC) films with the thickness of 0.20mm are respectively made into the following geometric dimensions (length x width x thickness): isothermal moisture adsorption samples of 5mm × 5mm × 0.20mm and DMA tensile samples of 20mm × 5mm × 0.20 mm; placing the test piece into a constant temperature and constant humidity box with the temperature of 110 ℃, annealing for 120 minutes to eliminate the prestress of the test piece, cooling the test piece to room temperature at the speed of 5 ℃/hour, and placing the test piece into a drying dish; thirdly, applying 2MPa dynamic tensile load (frequency is 1Hz) on a TA Q800 Dynamic Mechanical Analyzer (DMA) to a PVC film sample, and passing through DMAThe humidity accessory performs temperature scans at 20% and 60% relative humidity, with a temperature scan rate of 1 ℃/min. Respectively recording E '(T) -T and E' (T) -T test curves of the material under two equal wet conditions when the storage modulus and the loss modulus of the material are continuously changed along with the temperature from 35 ℃ to 100 ℃ (such as figures 3 and 4); determination of the glass transition temperature T at 20% and 60% relative humidity based on the peak of the E' (T) -T curveg(RH1) And Tg(RH2) Respectively as follows: 79.7 ℃ and 72.2 ℃ and determining the evolution equation of the linear dependence of the glass transition relative temperature on the relative humidity from the formula (1). Describing evolution of PVC dynamic storage modulus E' (T, RH) along with temperature-humidity coupling by adopting formula (1) to formula (4), wherein material parameters alpha, beta, gamma and eta are 328.3, 6.0, 0 and 0.179 respectively.
Comparing the dynamic storage moduli of PVA and PVC predicted by the above formulas (1) to (4) with the test data under the corresponding test conditions in FIGS. 5 and 6, it can be found that the method of the present invention has higher calculation accuracy.

Claims (1)

1. A prediction method of polymer dynamic storage modulus under a damp and hot environment is characterized by comprising the following analysis steps:
a. placing the amorphous or partially crystalline polymer test piece into a dynamic mechanical analyzer equipped with a humidity control accessory, and drying for 24 hours in an environment with the temperature of 25 +/-0.1 ℃ and the relative humidity of 0 +/-1%;
b. selecting 2 reference relative humidities RH within the range of 0-90%1And RH2The method comprises the following steps of performing dynamic mechanical test of a linear viscoelastic range on a thin film test piece by adopting a temperature scanning mode in the equal humidity state, and respectively recording and drawing E '(T) -T and E' (T) -T curves of a material when the storage modulus E '(T) and the loss modulus E' (T) are changed along with the environmental temperature T from the glass state to the rubber state in a global range in real time;
c. determining the glass transition temperature T at the corresponding humidity based on the peak value of the E' (T) -T curveg(RH)；
d. According to relative humidity RH1And RH2And its glass transition temperature Tg(RH1) And Tg(RH2) Data and fromDetermination of the glass transition temperature T by the formula (1)g(RH) linear variation with relative humidity RH:
Figure FDA0002620662520000011
e. the change rule of the dynamic storage modulus E '(T, RH) of the high polymer along with the temperature T is described by a hyperbolic tangent function shown as a following formula (2), wherein E'UAnd E'RInitial and final storage moduli before and after the glass transition of the high polymer, phi (T, RH) and lambda (RH) are temperature-humidity coupling function and humidity plasticizing factor,
Figure FDA0002620662520000012
f. phi (T, RH) and lambda (RH) are determined by the following formulas (3) and (4), respectively: wherein the material parameters alpha, beta, gamma and eta are defined by relative humidity RH1And RH2Temperature sweep E' (T) -T test curve fitting,
Figure FDA0002620662520000013
λ(RH)＝γ·RH+η (4)
g. by combining the above formula (1) to formula (4), the dynamic storage modulus of the high polymer under ordinary temperature and humidity conditions can be obtained.
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