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Preparation method and application of ultrathin fiber slice

A technology of ultra-thin slices and fibers, which is applied in the preparation of test samples, material analysis using radiation, material analysis using wave/particle radiation, etc. It can solve the problems of flexible fiber sample preparation difficulties and easily damaged fiber structures, etc. Achieve the effect of not easy to peel off or pores, improve the contact interface, and increase the interface bonding force

Inactive Publication Date: 2021-06-18
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of flexible fiber sample preparation and easy damage to the fiber structure in the background technology, the present invention proposes a method for preparing fiber ultrathin slices, which can effectively separate nano-scale microfibril structures and smaller-scale lamellar structure

Method used

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  • Preparation method and application of ultrathin fiber slice
  • Preparation method and application of ultrathin fiber slice
  • Preparation method and application of ultrathin fiber slice

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preparation example Construction

[0025] The first aspect of the present invention provides a method for preparing fiber ultra-thin slices, comprising the following steps: freeze-drying, embedding, trimming, slicing, solution etching, and drying.

[0026] In one or more embodiments of the present invention, the polyacrylonitrile fibers are preferably as-spun fibers, washed fibers, densified fibers, precursors, and pre-oxidized fibers.

[0027] There are various types of fibers. Taking polyacrylonitrile fiber as an example, the internal organization of polyacrylonitrile primary fiber is a sheet structure, and the sheets are arranged perpendicular to the fiber axis, and there are many pores between the sheets; during the pre-drawing stage of the coagulation bath, The microfibril structure began to appear, and the microfibrils were arranged parallel to the fiber axis. After multi-stage drafting and densification, the microfibrils were arranged more closely, and the microfibrils were not arranged in parallel. Ther...

Embodiment 1

[0066] Such as figure 1 Shown, a kind of preparation method of fiber ultrathin section comprises the following steps:

[0067] (1) Pretreatment of fibers: some polyacrylonitrile fibers (as-spun fibers, washed fibers) contain dimethyl sulfoxide and water, which need to be freeze-dried. Drying fibers: put the fibers in liquid nitrogen for 10 minutes to make the fibers Quickly freeze, and then put the fiber into a special freeze dryer, and dry it under vacuum for 24 hours at -70°C to obtain a dry sample.

[0068] (2) Sample embedding: Cut the clean fibers into micro-segments of 2-4mm, add 3-4 drops of Epon812 epoxy resin to the embedding hole of the latex embedding plate, and use tweezers to vertically or Parallel to the long axis of the embedding hole, put it into the embedding hole, and then drop the resin until the embedding hole is full. The embedding plate was cured in a vacuum oven for 12 hours at 37°C, 12 hours at 45°C, and 48 hours at 60°C.

[0069] (3) Trimming: rough...

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Abstract

The invention relates to the technical field of characterization of fiber structures and performance, and in particular relates to a preparation method and application of an ultrathin fiber slice. The preparation method of the ultrathin fiber slice comprises the steps of freeze drying, embedding, block trimming treatment, slicing, solution etching and drying. Freeze drying and embedding can enable fibers to be in good contact with resin, block trimming treatment is beneficial to blade cutting, and solution etching of ultrathin slices can separate out nanoscale microfibril structures and lamellar structures with smaller sizes. The invention adopts a solution etching technology for ultrathin slices, and provides a method capable of more deeply researching polyacrylonitrile fiber microfibril structure transformation.

Description

technical field [0001] The invention relates to the technical field of characterization of fiber structure and performance, in particular to a preparation method and application of fiber ultrathin slices. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Polyacrylonitrile precursor is an important precursor for the preparation of high-performance carbon fibers. Polyacrylonitrile is spun, pre-oxidized, and carbonized to obtain polyacrylonitrile-based carbon fibers. Polyacrylonitrile fibers are mainly prepared by wet spinning and dry-jet wet spinning processes. During the spinning process and pre-oxidation process, the structural transformation of polyacrylonitrile fibers ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/36G01N1/42G01N1/44G01N23/04G01N23/20008
CPCG01N1/286G01N1/36G01N1/42G01N1/44G01N23/04G01N23/20008G01N2001/2873G01N2001/364
Inventor 高权王成国王玉霞
Owner SHANDONG UNIV
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