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Microscopy characterization and evaluation method of homogeneity of carbon fibers

An evaluation method, carbon fiber technology, applied in the preparation of test samples, material analysis using radiation diffraction, etc., can solve the problems of lack of quantifiable operability of information, too macroscopic concepts, and inability to give qualitative information on structural changes, etc.

Inactive Publication Date: 2014-06-25
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the scanning electron microscope is limited by its own resolution, it is difficult to give fine structural information
Although there are reports in the literature that FE-SEM is used to observe polyacrylonitrile carbon fibers of different systems and obtain different surface morphology features, such as granular and granular, the concept is too macroscopic to give qualitative information on structural changes.
Although it is also possible to observe cracks, inclusions and holes on the surface of carbon fibers, these are product defects and cannot be used for comparison with products from other manufacturers. In short, the information obtained by SEM lacks standard quantifiable operability

Method used

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  • Microscopy characterization and evaluation method of homogeneity of carbon fibers
  • Microscopy characterization and evaluation method of homogeneity of carbon fibers
  • Microscopy characterization and evaluation method of homogeneity of carbon fibers

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Experimental program
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Embodiment 1

[0044] 1. T700S carbon fiber material sample preparation

[0045] When embedding and preparing thin-section samples, ensure that the fiber axis is placed horizontally. Using 3~6kV argon ions in high vacuum (10 -5 Pa) directly bombard the sample to obtain a thinner sample. During thinning, the angle between the incident argon ion beam and the surface of the sample is φ. Using the LKY-AB ion thinning instrument, first select the angle φ=20°. When the central area of ​​the sample is slightly transparent during thinning , reduce the included angle φ to 13°, and then reduce it from 13° to 8°; the time of "sweeping" the sample surface is reduced from 20min to 10min to "clean" the surface of the sample to ensure that the fiber The uniformity of the thickness of the thin area in the diameter direction. In this experiment, the sample thickness at the data collection position is greater than 5nm and less than 50nm.

[0046] 2. Collect SAED spectrum

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Abstract

The invention aims to provide a microscopy characterization and evaluation method of homogeneity of carbon fibers. The method has the advantages that the homogeneity of a carbon fiber structure can be systematically evaluated, the method is not limited by the structures of the carbon fiber products of different diameters, different densities, different batches and different corporations, meanwhile, a condition that the carbon fibers are high modulus or high strength carbon fibers is not distinguished, and a simple, convenient and feasible evaluation standard is provided for evaluating the homogeneity of the carbon fiber structure in a qualitative manner. The evaluation method comprises the following specific steps of collecting an axially horizontal slice sample of carbon fibers, and collecting a series of continuous selected area electron diffraction (SAED) patterns on slices the sizes of which are same with the longitudinal sections of the carbon fibers by using a transmission electron microscope; respectively reading diffracted intensity values of the positions (0002) of the periphery along each diffraction arc to obtain a preferred orientation angle OA map, wherein the preferred orientation angle directly corresponds to the arrangement orientation degree of a (0002) carbon atom layer of the carbon fibers; accurately and quantitatively characterizing a texture degree of the carbon fibers by using the orientation angle.

Description

technical field [0001] The invention relates to a method for characterizing and evaluating the radial structural uniformity of carbon fibers, which is suitable for polyacrylonitrile (PAN)-based carbon fibers of any different precursors, and can qualitatively represent the change of structural uniformity along the radial direction of the fiber. Background technique [0002] Carbon fiber is a fibrous carbon material with a carbon content of more than 90%. It is made by pyrolysis of other organic fibers. It has low density, high strength, high modulus, fatigue resistance, high temperature resistance, corrosion resistance, and good conductivity. It is widely used in fiber-reinforced resin-based composite materials due to its small thermal expansion coefficient. PAN-based carbon fiber is the most important and absolute type of high-performance carbon fiber. It plays an irreplaceable role in aerospace, weapons, ships and other national defense fields. It is a strategic basic mater...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N23/20
Inventor 贺连龙郭新爽刘叶群周庚衡郑风珊
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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