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Thermal analysis method for determining content of each phase state ingredient of half crystallization high molecular material

A technology of polymer material and component content, which is applied in the direction of material thermal analysis, analysis material, measuring device, etc., can solve the problem of no further phase state component content and other problems

Inactive Publication Date: 2017-05-31
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research and testing of semi-crystalline polymer materials, SSDSC technology is used to study the reversible and irreversible changes of materials, and there is no further research on the phase component content (crystalline state and amorphous state, etc.) of materials.

Method used

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  • Thermal analysis method for determining content of each phase state ingredient of half crystallization high molecular material
  • Thermal analysis method for determining content of each phase state ingredient of half crystallization high molecular material
  • Thermal analysis method for determining content of each phase state ingredient of half crystallization high molecular material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1: A kind of thermal analysis method of measuring the content of each phase state component of semi-crystalline polymer material, concrete operation is as follows:

[0034] (1) Weigh 40 mg of the standard substance sapphire, put it in an aluminum crucible, cover it with an empty plate and compact it, and carry out StepScan heating at 25-175°C under 15ml / min nitrogen gas, with a heating rate of 5°C / min, every Increase the temperature by 1 °C for 1 min to obtain the SSDSC curve.

[0035] (2) Through the data analysis of the SSDSC curve, a reversible specific heat capacity curve in the range of 25-175 °C was obtained, and the specific heat capacity value on the experimental curve was compared with the standard specific heat capacity value of sapphire.

[0036] (3) Carry out a SSDSC repeated experiment again according to the method of step (1) and (2), draw a reversible specific heat capacity curve; Standard curve and these two reversible specific heat capacity c...

Embodiment 2

[0048] Example 2: roughly the same as Example 1, the difference is that step (1) when carrying out the StepScan experiment, start to carry out isothermal at 25°C for 15min, and finally at 175°C for another 15min, the standard curve and the obtained two reversible specific heat capacities The curve is plotted at figure 2 middle. Such as figure 2 As shown, the reversible specific heat capacity of sapphire measured by adding isothermal steps before and after the temperature rise in the experiment also has good repeatability and accuracy. The maximum error between the specific heat capacity of sapphire and its standard specific heat capacity during the two repeated tests is 0.8 %, which is less than 2% of the conventional DSC method reported in the literature. And from the experimental results, although the maximum error of embodiment 1 and embodiment 2 is consistent, but in figure 1 When the start and end positions are not isothermal, the specific heat capacity values ​​at l...

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Abstract

The invention provides a thermal analysis method for determining the content of each phase state ingredient of a half crystallization high molecular material. According to the method, conventional and step type temperature rise modes are respectively used for heating a sample; a StepScan DSC curve is resolved into a reversible specific heat capacity curve and an irreversible specific heat capacity curve; the glass transition position is determined through the discontinuous mutation of the specific heat capacity on the reversible specific heat capacity curve; then, the content of different phase state ingredients of half crystallization molecules is determined according to the specific heat capacity increase and the melting enthalpy on the DSC curve. Through an SSDSC technology, the glass transition is separated out from a dynamic process to obtain the parameters such as the reversible specific heat capacity, the glass transition temperature and the melting enthalpy in the test sample temperature rise process; the glass transition temperature of the half crystallization high molecular material can be obtained; the reversible specific heat capacity corresponding to different temperatures can be accurately obtained; meanwhile, the content of different phase states such as the crystallization state, the flowing amorphous state and the hard amorphous state in the half crystallization high molecular test sample can be calculated according to the specific heat capacity and the melting enthalpy.

Description

technical field [0001] The invention relates to a semi-crystalline polymer material, in particular to a method for measuring the content of each phase component of the semi-crystalline polymer material. Background technique [0002] According to the regularity of molecular spatial arrangement, polymer materials can be divided into crystalline polymers and amorphous polymers. Generally speaking, when most crystalline polymer materials are stacked into crystals, the ends of the chains and entanglement points will be excluded from the crystal region, so the entire molecular chains can only be partially crystallized, and the formed crystals are not perfect. , which forms a semi-crystalline polymer. Glass transition is a common phenomenon of semi-crystalline polymers. It is the transition of amorphous molecules between the glass state and the high elastic state in the temperature field. It can reflect the motion state of polymer material segments and other structures. [0003] ...

Claims

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Application Information

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IPC IPC(8): G01N25/04G01N25/12G01N25/00
CPCG01N25/005G01N25/04G01N25/12
Inventor 王昉于海洋顾正桂
Owner NANJING NORMAL UNIVERSITY
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