分步插层法制备高倍膨胀石墨及其微观结构

赵纪金; 李晓霞; 郭宇翔; 马德跃

doi:10.3788/OPE.20142205.1267

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分步插层法制备高倍膨胀石墨及其微观结构

微纳技术与精密机械 | 更新时间：2020-08-13

- 分步插层法制备高倍膨胀石墨及其微观结构
- Highly exfoliated graphite prepared by two-step intercalation and its microstructure
- 光学精密工程 2014年22卷第5期页码：1267-1273
- 作者机构：
  
  1. 电子工程学院脉冲功率激光技术国家重点实验室,安徽合肥,230037
  2. 电子工程学院红外与低温等离子体安徽省重点实验室,安徽合肥,230037
- 作者简介：
- 基金信息：
  
  脉冲功率激光技术国家重点实验室基金资助项目（No.SKL20132R03）()
- DOI：10.3788/OPE.20142205.1267
  中图分类号： TQ165
- 收稿日期：2013-11-20，
  
  修回日期：2014-01-05，
  
  纸质出版日期：2014-05-25
- 稿件说明：
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赵纪金, 李晓霞, 郭宇翔等. 分步插层法制备高倍膨胀石墨及其微观结构[J]. 光学精密工程, 2014,22(5): 1267-1273

ZHAO Ji-jin, Li Xiao-xia, GUO Yu-xiang etc. Highly exfoliated graphite prepared by two-step intercalation and its microstructure[J]. Editorial Office of Optics and Precision Engineering, 2014,22(5): 1267-1273
赵纪金, 李晓霞, 郭宇翔等. 分步插层法制备高倍膨胀石墨及其微观结构[J]. 光学精密工程, 2014,22(5): 1267-1273 DOI： 10.3788/OPE.20142205.1267.

ZHAO Ji-jin, Li Xiao-xia, GUO Yu-xiang etc. Highly exfoliated graphite prepared by two-step intercalation and its microstructure[J]. Editorial Office of Optics and Precision Engineering, 2014,22(5): 1267-1273 DOI： 10.3788/OPE.20142205.1267.

摘要

为获得密度小，漂浮性能好的膨胀石墨，采用分步插层法，依次以硝酸与磷酸的混酸、硝酸与乙酸的混酸为插层剂，高锰酸钾为氧化剂制备了高倍膨胀石墨。利用正交试验和平行试验确定了最佳工艺条件。在确定的工艺条件下制备出了膨胀体积为450ml/g的膨胀石墨。分析了用分步插层法制备高倍膨胀石墨的主要影响因素，提出其按影响大小依次为：第一步插层中高锰酸钾用量和第二步插层中乙酸、高锰酸钾和硝酸的用量。采用扫描电镜（SEM）分析了膨胀石墨微观结构随膨胀体积的变化。结果表明：随膨胀体积的增大，膨胀石墨片层被充分打开，几何截面增大，形成更大散射体，从而有利于红外辐射和毫米波的衰减。

Abstract

To achieve exfoliated graphite with low density and good suspensibility

the mixture of nitric acid and phosphoric acid

and the mixture of nitric acid and acetic acid were employed as intercalating agents; potassium permanganate was used as oxidant

and highly exfoliated graphite was prepared by two-step intercalation. The optimum preparation conditions affecting expanding volume of the exfoliated graphite were determined by orthogonal and parallel experiments

then the exfoliated graphite with an expansion volume of 450 ml/g was prepared with above special procedure. The effect factors on exfoliated graphite prepared by two-step intercalation was analyzed

and results point out that it is related to the amounts of potassium permanganate in the first intercalation and those of acetic acid

potassium permanganate and nitric acid in the second intercalation. Moreover

the microstructures of exfoliated graphite with different expanding volumes were also analyzed by Scanning Electron Microscopy(SEM). The results show that as the volume expends

the layers of the exfoliated graphite are fully opened and its geological section area is increased to form a larger deflection entity.Therefore

it accelerates the decay of infrared and micro wave radiations.

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Keywords

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