CN110887857A - Method for detecting polyacrylonitrile fiber generalized crystallinity by two-dimensional X-ray diffraction - Google Patents

Method for detecting polyacrylonitrile fiber generalized crystallinity by two-dimensional X-ray diffraction Download PDF

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CN110887857A
CN110887857A CN201811040944.6A CN201811040944A CN110887857A CN 110887857 A CN110887857 A CN 110887857A CN 201811040944 A CN201811040944 A CN 201811040944A CN 110887857 A CN110887857 A CN 110887857A
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amorphous phase
ratio
diffraction
theta
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高忠民
唐海通
高宇
李向山
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Jilin University
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention provides a method for detecting the generalized crystallinity of polyacrylonitrile fibers by applying two-dimensional X-ray diffraction, belonging to the analysis and test technology of material crystal structures. Aiming at the fact that polyacrylonitrile fibers have partial ordered and disordered structures besides three-dimensional ordered crystalline phases and disordered phases, a crystalline state X-ray characterization test method which comprehensively considers the types and values of physical phases in the PAN fibers is not established at home and abroad at present, and the ratio X of the crystalline phase is used for the inventioncOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are used as the characterization parameters of the polyacrylonitrile fiber generalized crystallinity. Selecting characteristic diffraction angles based on a two-dimensional X-ray diffraction pattern, obtaining a diffraction intensity-azimuth angle distribution curve after integration, calculating the integral intensity, and further calculating to obtain a crystal phase ratio XcOriented amorphous phase ratio XoRatio X to amorphous phaseaThree structural parameters comprehensively consider the crystalline state of the species and the numerical values of the phases in the PAN fiber, and the characterization is more accurate.

Description

Method for detecting polyacrylonitrile fiber generalized crystallinity by two-dimensional X-ray diffraction
Technical Field
The present invention belongs to the field of material crystal structure analysis and test technology.
Background
Polyacrylonitrile (PAN) fiber is a precursor for producing high-quality carbon fiber, and the quality of the performance of the Polyacrylonitrile (PAN) fiber has an important influence on the quality of the carbon fiber. PAN fibers have a long molecular chain structure, and atoms in the molecular chain are strongly bonded by covalent bonds or the like, while inter-chains are weakly bonded by hydrogen bonds or van der waals forces or the like, so that the PAN fibers have partially ordered and disordered structures such as oriented amorphous structures in addition to three-dimensional ordered crystalline and disordered phases, and the types and the numbers of various ordered structures have an important influence on the performance of the PAN fibers. However, a crystallization state X-ray characterization test technology which fully considers the species and the numerical value of the physical phase in the PAN fiber is not established at home and abroad up to now. Therefore, the object and original intention of the present invention are to solve the technical problem.
Disclosure of Invention
Aiming at the problems, the invention provides a method for detecting the generalized crystallinity of polyacrylonitrile fiber by two-dimensional X-ray diffraction, which uses the crystalline phase ratio XcOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are used as the characterization parameters of the polyacrylonitrile fiber generalized crystallinity.
The technical scheme adopted by the invention is as follows:
1) testing polyacrylonitrile fibers by using a two-dimensional X-ray diffractometer to obtain a two-dimensional diffraction pattern, and simultaneously obtaining an I (2 theta, kappa) curve, namely a diffraction intensity-diffraction angle-azimuth angle curve;
2) selecting a diffraction angle 2 theta of a (100) crystal plane for a crystal phasec16.9 deg. at diffraction angle 2 thetacSolving curve integral in the range of +/-delta 2 theta; the diffraction angle 2 theta is selected for the oriented amorphous phaseo25.2 deg. at diffraction angle 2 thetaoSolving curve integral in the range of +/-delta 2 theta; respectively obtaining I-kappa distribution curves, namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) respectively carrying out integration on the peaks of the I-kappa distribution curves to obtain the integrated intensity I of the crystalline phase in the range of azimuth angle-90 DEG for the two I-kappa distribution curvescAnd the integral intensity I of the oriented amorphous phase in the interval of azimuth angle-90 DEGoIntegral intensity I of amorphous phase in the interval of azimuth angle-90 DEGaObtaining by integrating the baseline of the diffraction arc I-kappa distribution curve of the oriented amorphous phase;
4) calculating the phase ratio X of the crystalloid according to a formulacOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are set to be in a certain range,
Figure BDA0001792080480000011
Figure BDA0001792080480000012
Figure BDA0001792080480000013
the invention has the beneficial effects that:
solving the problem that a crystallization state X-ray characterization test technology which comprehensively considers the species and the numerical value of the object phase in the PAN fiber is not established at home and abroad up to now, providing a method for detecting the generalized crystallinity of the polyacrylonitrile fiber by applying two-dimensional X-ray diffraction, and taking the ratio of the crystallization phase to the XcOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are used as the characterization parameters of the polyacrylonitrile fiber generalized crystallinity, and the structures of ordered crystalline phase, disordered phase and partial ordered and disordered phases (oriented amorphous phase) can be accurately described.
Drawings
FIG. 1 two-dimensional diffraction pattern of Polyacrylonitrile (PAN) fiber;
FIG. 2 diffraction intensity-azimuth (I-. kappa.) distribution curves.
Detailed Description
Example 1
1) Testing polyacrylonitrile fiber by using a two-dimensional X-ray diffractometer to obtain a two-dimensional diffraction pattern (shown as figure 1), and simultaneously obtaining an I (2 theta, kappa) curve, namely a diffraction intensity-diffraction angle-azimuth angle curve;
2) selecting a diffraction angle 2 theta of a (100) crystal plane for a crystal phasec16.9 deg. at diffraction angle 2 thetacSolving curve integral in the range of +/-delta 2 theta; the diffraction angle 2 theta is selected for the oriented amorphous phaseo25.2 deg. at diffraction angle 2 thetaoSolving curve integral in the range of +/-delta 2 theta; respectively obtaining I-kappa distribution curves (shown in figure 2), namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) respectively carrying out integration on the peaks of the I-kappa distribution curves to obtain the integrated intensity I of the crystalline phase in the range of azimuth angle-90 DEG for the two I-kappa distribution curvescAnd the integral intensity I of the oriented amorphous phase in the interval of azimuth angle-90 DEGoIntegral intensity I of amorphous phase in the interval of azimuth angle-90 DEGaObtained by integrating the baseline of the diffraction arc I-. kappa.distribution curve of the oriented amorphous phase:
Ic＝164522，Io＝6536，Ia＝52787；
4) calculating the phase ratio X of the crystalloid according to a formulacOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are set to be in a certain range,
Figure BDA0001792080480000021
Figure BDA0001792080480000022
Figure BDA0001792080480000023

Claims (1)

1. a method for detecting the generalized crystallinity of polyacrylonitrile fiber by two-dimensional X-ray diffraction is characterized in that the method uses the crystal phase ratio XcOriented amorphous phase ratio XoRatio X to amorphous phaseaThree structural parameters are taken as characterization parameters of the polyacrylonitrile fiber generalized crystallinity, and the detection method comprises the following specific steps:
1) testing polyacrylonitrile fibers by using a two-dimensional X-ray diffractometer to obtain a two-dimensional diffraction pattern, and simultaneously obtaining an I (2 theta, kappa) curve, namely a diffraction intensity-diffraction angle-azimuth angle curve;
2) to, forCrystal phase, selective (100) plane diffraction angle 2 thetac16.9 deg. at diffraction angle 2 thetacSolving curve integral in the range of +/-delta 2 theta; the diffraction angle 2 theta is selected for the oriented amorphous phaseo25.2 deg. at diffraction angle 2 thetaoSolving curve integral in the range of +/-delta 2 theta; respectively obtaining I-kappa distribution curves, namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) respectively carrying out integration on the peaks of the I-kappa distribution curves to obtain the integrated intensity I of the crystalline phase in the range of azimuth angle-90 DEG for the two I-kappa distribution curvescAnd the integral intensity I of the oriented amorphous phase in the interval of azimuth angle-90 DEGoIntegral intensity I of amorphous phase in the interval of azimuth angle-90 DEGaObtaining by integrating the baseline of the diffraction arc I-kappa distribution curve of the oriented amorphous phase;
4) calculating the phase ratio X of the crystalloid according to a formulacOriented amorphous phase ratio XoRatio X to amorphous phaseaThe three structural parameters are set to be in a certain range,
Figure FDA0001792080470000011
Figure FDA0001792080470000012
Figure FDA0001792080470000013
CN201811040944.6A 2018-09-07 2018-09-07 Method for detecting polyacrylonitrile fiber generalized crystallinity by two-dimensional X-ray diffraction Pending CN110887857A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104264264A (en) * 2014-09-23 2015-01-07 中复神鹰碳纤维有限责任公司 Preparation method of high-orientation-degree polyacrylonitrile fibers
CN106426973A (en) * 2016-08-31 2017-02-22 苏州西脉新诚生物科技有限公司 Method for preparing orientated-state polylactic acid profile
CN107192729A (en) * 2017-05-18 2017-09-22 吉林大学 The online fast analyser of polyacrylonitrile fibre structure X-ray diffraction and method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104264264A (en) * 2014-09-23 2015-01-07 中复神鹰碳纤维有限责任公司 Preparation method of high-orientation-degree polyacrylonitrile fibers
CN106426973A (en) * 2016-08-31 2017-02-22 苏州西脉新诚生物科技有限公司 Method for preparing orientated-state polylactic acid profile
CN107192729A (en) * 2017-05-18 2017-09-22 吉林大学 The online fast analyser of polyacrylonitrile fibre structure X-ray diffraction and method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
葛陈程等: "应用二维X射线衍射法测定涤纶工业丝结晶和取向行为", 《纺织学报》 *

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