CN110887854A - Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction - Google Patents

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

Info

Publication number
CN110887854A
CN110887854A CN201811041121.5A CN201811041121A CN110887854A CN 110887854 A CN110887854 A CN 110887854A CN 201811041121 A CN201811041121 A CN 201811041121A CN 110887854 A CN110887854 A CN 110887854A
Authority
CN
China
Prior art keywords
orientation
degree
theta
diffraction
amorphous phase
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811041121.5A
Other languages
Chinese (zh)
Inventor
高忠民
唐海通
高宇
李向山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jilin University
Original Assignee
Jilin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jilin University filed Critical Jilin University
Priority to CN201811041121.5A priority Critical patent/CN110887854A/en
Publication of CN110887854A publication Critical patent/CN110887854A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention provides a method for detecting the generalized orientation degree of polyacrylonitrile fibers by applying two-dimensional X-ray diffraction, and belongs to the technical field of analysis and detection of material crystalline structures. The PAN fiber X-ray method for measuring the orientation degree applied at home and abroad is carried out aiming at the diffraction line of the crystalline phase (100), but has obvious incompleteness and inaccuracy. Therefore, the invention provides a method which is based on a two-dimensional diffraction pattern, selects a characteristic diffraction angle, integrates to obtain a diffraction intensity-azimuth angle curve, and calculates to obtain a crystal phase orientation degree A by utilizing the half-height peak width of the curvecDegree of orientation of oriented amorphous phase AoAnd degree of orientation A of amorphous phaseaThe orientation states of the crystalline phase, the oriented amorphous phase and the amorphous phase in the PAN fiber are completely characterized, and compared with the prior art, the result is more accurate.

Description

Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction
Technical Field
The invention belongs to the technical field of analysis and detection of material crystal structures.
Background
Polyacrylonitrile fiber is a precursor for manufacturing high-quality carbon fiber, and the structural characteristics of the polyacrylonitrile fiber have important influence on the quality of the carbon fiber. PAN fiber belongs to macromolecular chain conformation, atoms in a molecular chain are connected by covalent strong bonds, and molecular chains have the functions of hydrogen bonds and van der Waals weak bonds. Therefore, the orientation state of molecular chains has an important influence on the axial strength and modulus of Polyacrylonitrile (PAN) fiber precursors, and therefore, the orientation behaviors of crystalline phases, oriented amorphous phases and amorphous phases along the fiber axis are key structural parameters of PAN fibers. The PAN fiber X-ray method used at home and abroad up to now measures the degree of orientation by aiming at the diffraction line of the crystalline phase (100), but has obvious incompleteness and inaccuracy.
Disclosure of Invention
The invention aims to create a brand-new PAN fiber generalized orientation degree characterization technology on the premise of comprehensively considering the contribution of multiple types of crystal types in PAN fibers to PAN fiber orientation parameters. Therefore, the invention provides a method for detecting the generalized orientation degree of polyacrylonitrile fibers by using two-dimensional X-ray diffraction, which adopts the following technical scheme:
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) the (100) plane diffraction angle 2 theta is selected for the crystalline 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 curves, namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) calculating the half-height peak width of two I-kappa curves respectively, and the half-height width of the crystalline phase curve is HcThe half height width of the oriented amorphous phase curve is HoThe width of the base line of the oriented amorphous phase curve is Ha＝180°；
4) The crystal phase orientation degree A was calculated according to the following formulacDegree of orientation of oriented amorphous phase AoAnd degree of orientation A of amorphous phasea；
Figure BDA0001792110530000011
Figure BDA0001792110530000012
Figure BDA0001792110530000013
The invention has the beneficial effects that:
the invention comprehensively considers the orientation parameters of the PAN fiber by various types of crystals in the PAN fiber, and solves the problem that the PAN fiber is not accurately and comprehensively described by the structural parameters caused by detecting the orientation degree of the crystal phase only in the prior art.
Drawings
FIG. 1 example 1 two-dimensional diffraction pattern of polyacrylonitrile fibers;
FIG. 2I-kappa curves of the crystalline phase and the oriented amorphous phase of example 1.
Detailed Description
The technical solution of the present invention is further explained and illustrated below by way of specific examples.
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) the (100) plane diffraction angle 2 theta is selected for the crystalline 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 curves, namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) calculating the half-height peak width of two I-kappa curves respectively, and the half-height width of the crystalline phase curve is Hc50.74 DEG, and the half width of the oriented amorphous phase curve is Ho143.26 DEG, the baseline width of the oriented amorphous phase curve is Ha＝180°；
4) The crystal phase orientation degree A was calculated according to the following formulacDegree of orientation of oriented amorphous phase AoAnd degree of orientation A of amorphous phasea；
Figure BDA0001792110530000021
Figure BDA0001792110530000022
Figure BDA0001792110530000023

Claims (1)

1. The method for detecting the generalized orientation degree of the polyacrylonitrile fiber by using two-dimensional X-ray diffraction is characterized in that the generalized orientation degree comprises three parameters, namely, a crystal phase orientation degree AcDegree of orientation of oriented amorphous phase AoAnd degree of orientation A of amorphous phasea；
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) the (100) plane diffraction angle 2 theta is selected for the crystalline 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 curves, namely diffraction intensity-azimuth angle curves; delta 2 theta is 1-5 degrees;
3) calculating the half-height peak width of two I-kappa curves respectively, and the half-height width of the crystalline phase curve is HcThe half height width of the oriented amorphous phase curve is HoThe width of the base line of the oriented amorphous phase curve is Ha＝180°；
4) The crystal phase orientation degree A was calculated according to the following formulacDegree of orientation of oriented amorphous phase AoAnd degree of orientation A of amorphous phasea；
Figure FDA0001792110520000011
Figure FDA0001792110520000012
Figure FDA0001792110520000013
CN201811041121.5A 2018-09-07 2018-09-07 Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction Pending CN110887854A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811041121.5A CN110887854A (en) 2018-09-07 2018-09-07 Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811041121.5A CN110887854A (en) 2018-09-07 2018-09-07 Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction

Publications (1)

Publication Number Publication Date
CN110887854A true CN110887854A (en) 2020-03-17

Family

ID=69744417

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811041121.5A Pending CN110887854A (en) 2018-09-07 2018-09-07 Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction

Country Status (1)

Country Link
CN (1) CN110887854A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122495A (en) * 2011-11-18 2013-05-29 东丽纤维研究所（中国）有限公司 Modified copolyester fiber, method for manufacturing same and fabric comprising modified copolyester fiber
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 (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122495A (en) * 2011-11-18 2013-05-29 东丽纤维研究所（中国）有限公司 Modified copolyester fiber, method for manufacturing same and fabric comprising modified copolyester fiber
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 (2)

* Cited by examiner, † Cited by third party
Title
唐春红等: "湿法纺各阶段聚丙烯腈基原丝微结构的Ｘ射线衍射分析", 《化工新型材料》 *
徐翔等: "一种用X衍射测定PET纤维非晶取向度的简易方法", 《纺织学报》 *

Similar Documents

Publication Publication Date Title
Schuepfer et al. Assessing the structural properties of graphitic and non-graphitic carbons by Raman spectroscopy
Tumanov et al. Pressure-induced phase transitions in L-alanine, revisited
Filip et al. NMR crystallography methods to probe complex hydrogen bonding networks: application to structure elucidation of anhydrous quercetin
CN102445173B (en) Clamping device for linear displacement sensor
Sarau et al. Efficient nitrogen doping of single-layer graphene accompanied by negligible defect generation for integration into hybrid semiconductor heterostructures
Wegner et al. The impact of the amide connectivity on the assembly and dynamics of benzene-1, 3, 5-tricarboxamides in the solid state
Latham et al. Molecular structures driving pseudo-capacitance in hydrothermal nanostructured carbons
CN110887854A (en) Method for detecting polyacrylonitrile fiber generalized orientation degree by two-dimensional X-ray diffraction
CN104034744A (en) Method for measuring residual stress of pyrolytic carbon coating by virtue of X ray diffraction
CN103424066A (en) Method for using circularly polarized antenna far field phase difference for calculating rotation offset of electric field probe
Baei et al. The influence of NH3-attaching on the NMR and NQR parameters in the (6, 0) zigzag single-walled BPNTs: a density functional study
CN203082472U (en) Universal mounting bracket for supporting, fixing, mounting and adjusting device
Hawkins et al. Conformational analysis of coordination compounds. VII. Barrier to inversion of five-membered diamine chelate rings by NMR
Li et al. High Young's modulus carbon fibers are fouling resistant with fast-scan cyclic voltammetry
CN110887857A (en) Method for detecting polyacrylonitrile fiber generalized crystallinity by two-dimensional X-ray diffraction
Facchine et al. Torsional angles in vinylarenes determined by high-field NMR spectroscopy
CN207456719U (en) A kind of arrangements for automotive doors vertical stiffness tests Universal clamp
CN207300461U (en) A kind of membrane stress test substrate clamp
CN204279980U (en) A kind of suspended beam type wing movable part center position clamp structure
CN108572277A (en) Multiple-frequency signal measurement method and system
CN204286797U (en) A kind of locating support and analyzing flat instrument
Ennis et al. Vibrational mode analysis of hydrogen-bonded organic frameworks (HOFs): synchrotron infrared studies
CN219714415U (en) Mechanical hygrothermograph convenient to installation
CN104482841A (en) Measuring device for mesh clearance value of gear rack of steering engine
Asakuma et al. Surface topography of dyed potassium dihydrogen phosphate (KDP) crystals

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20200317

WD01 Invention patent application deemed withdrawn after publication