Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process

A technology of mullite whiskers and mullite, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve problems such as complex process, small size of mullite whiskers, complex process, etc., to achieve The process is simple, the inclusion of particles is less, and the effect of low preparation temperature

Inactive Publication Date: 2009-08-05
JINGDEZHEN CERAMIC INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Comparing the above five methods, it is not difficult to see that: the mineral method is used to prepare whiskers. Since the minerals contain flux impurities, after calcination, in order to obtain high-purity mullite whiskers, the product must be pickled. However, in the pickling process The mullite whiskers with small size will be dissolved to a certain extent in the medium, so the glass phase must be quickly removed by microwave corrosion technology, the process is complicated, and the aspect ratio of the prepared whiskers is not high, and the ion doping method is also Also there is above-mentioned problem; Although the raw material that Chinese patent report adopts is cheap, needs to adopt high-energy ball milling process, and cost is higher
The preparation of mullite whiskers by the molten salt method requires washing of the sintered samples. The process is quite complicated, and there will be waste liquid treatment problems during the washing process.
[0007] Al 2 o 3 -SiO 2 Because the raw materials used in the powder calcination method are alumina and silicon oxide, although the cost of the raw materi

Method used

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  • Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process
  • Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process
  • Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous AlCl 3 (analytical pure) as the precursor, anhydrous ether (chemically pure) as the oxygen donor, AlF 3 (Industrial pure) is a whisker catalyst. First, measure 0.0179mol Si(OC 2 h 5 ) 4 Place in a 100ml dry Erlenmeyer flask, add 0.0537mol anhydrous AlCl 3, stirred magnetically at room temperature to obtain a khaki precursor mixture, added 0.0448mol ether, and stirred for 15 minutes to obtain a black solution. The solution was placed in an oil bath at 110°C for reflux heating for 24 hours to obtain mullite xerogel; Grind and pass through a 250 mesh sieve to obtain xerogel powder. After granulating the xerogel powder, press it into a sheet-like sample in a powder tablet press under a pressure of 12 MPa, then place the sample in an alumina crucible for airtight calcination, and External 1wt% whisker catalyst AlF in the crucible 3 . The firing system is as follows: the heating rate is 4°C / min before 350°C, and then rais...

Embodiment 2

[0024] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous AlCl 3 (analytical pure) as the precursor, anhydrous ether (chemically pure) as the oxygen donor, AlF 3 (Industrial pure) is a whisker catalyst. The amount of raw materials used to prepare mullite whiskers, the process flow and the firing system are the same as in Example 1, except that AlF 3 The dosage is 3wt%, and the morphology of the prepared mullite whiskers is shown in the appendix image 3 .

Embodiment 3

[0026] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous AlCl 3 (analytical pure) as the precursor, anhydrous ether (chemically pure) as the oxygen donor, AlF 3 (Industrial pure) is a whisker catalyst. The amount of raw materials used to prepare mullite whiskers, the process flow and the firing system are the same as in Example 1, except that AlF 3 The consumption of is 6wt%.

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Abstract

The invention discloses a method of preparing porzite whiskers by a non-hydrolyzed sol-gel technology. The method comprises the following steps: using an anhydrous aluminum source and an anhydrous silicon source as precursors and using low-carbon alcohol or ether as an oxygen donor to prepare porzite xerogel powder; then adding a certain amount of fluoride as a whisker catalyst and calcining a closed crucible to prepare the high-purity and white porzite whiskers which have the diameter of 0.2 micron to 2 micron, a slenderness ratio up to 60 to 70 and do not comprise mingled particles. Compared with the prior art, the invention has the advantages of simple technology, convenient operation, low whisker preparation temperature and high whisker yield.

Description

technical field [0001] The invention relates to a method for preparing mullite whiskers by using a non-hydrolytic sol-gel process, and belongs to the technical field of new materials. Background technique [0002] Mullite whiskers not only have the properties of high temperature resistance, wear resistance and oxidation resistance, but also have the characteristics of high temperature strength, small high temperature creep, small thermal expansion and good thermal shock resistance. Therefore, it is an excellent It can be used as a reinforcement for metals, polymers, ceramic-based materials, etc. Not only that, but it can also be used at higher temperatures and harsher oxidation conditions than non-oxide whiskers. [0003] At present, many literatures at home and abroad have reported the preparation methods of mullite whiskers, mainly including mineral decomposition method, molten salt method, ion doping method, Al 2 o 3 -SiO 2 Powder calcination method and traditional hy...

Claims

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Application Information

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IPC IPC(8): C30B29/62C30B29/34
Inventor 江伟辉彭永烽刘健敏谭训彦包镇红苗立峰虞澎澎
Owner JINGDEZHEN CERAMIC INSTITUTE
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