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Method for preparing one-dimensional aluminum oxide fibre by hydrothermal-flux technique

A technology of alumina fiber and flux, which is applied in the field of preparation of inorganic chemical materials, can solve the problems of many holes, poor shape, uneven thickness, etc.

Inactive Publication Date: 2008-05-21
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the predecessors used methods such as inducing crystallization and reducing the phase transition temperature (Murase Yoshio, IGA Takeo, Method for production of needlelike crystalline particles, US patent 5286687; Hu Peng, Yuan Fangli, Li Shaohua, Li Jinlin, Huang Shulan, a needle-like α-Al 2 o 3 The preparation method of nano-powder, CN1800023A) slows down the shape damage, and the obtained product has more pores and poor shape (or length / thickness or agglomeration / particle coexistence), which limits the one-dimensional Al 2 o 3 Large-scale industrial applications of fibers

Method used

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  • Method for preparing one-dimensional aluminum oxide fibre by hydrothermal-flux technique
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  • Method for preparing one-dimensional aluminum oxide fibre by hydrothermal-flux technique

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preparation example Construction

[0021] The invention provides a simple and feasible new method for preparing one-dimensional alumina fiber. The basic idea: first prepare the amorphous aluminum hydroxide precursor at room temperature, and then use the inorganic morphology control agent to selectively adsorb under hydrothermal conditions to achieve directional growth of γ-AlOOH to obtain one-dimensional γ-AlOOH with high aspect ratio; use multi-stage Slow heating and flux roasting methods realize low-temperature and slow dehydration and structural reformation of one-dimensional γ-AlOOH, and obtain one-dimensional γ-AlOOH with a diameter of 10-100nm, a length of 0.5-10μm, an aspect ratio of 50-200, regular morphology, and good crystallization. Al 2 o 3 fiber. The method has the advantages of simple process, low cost and easy popularization. The resulting alumina fiber has superior performance and high added value, and can be used as a reinforcing material in aluminum alloy, ceramics, plastics, rubber and oth...

Embodiment 1

[0031] Prepare 100 milliliters of 0.5 mol / liter aluminum chloride solution, 100 milliliters of 1.5 mol / liter ammonia solution, and 50 milliliters of 1% (w / v) sodium sulfate solution. Add ammonia solution (2 ml / min) to aluminum chloride solution at 25°C under stirring (300 rpm) to obtain amorphous aluminum hydroxide suspension. Filter and wash the suspension, then add the precipitate and sodium sulfate solution into the autoclave, conduct a hydrothermal reaction at 250°C with stirring (100 rpm) for 8 hours, cool, filter, and wash to obtain γ-AlOOH hydrothermal intermediate Product; mix the γ-AlOOH hydrothermal intermediate product with sodium chloride, control the weight ratio of the two to 100:5, place the mixture in a muffle furnace, raise the temperature (2°C / min) to 250°C and keep it for 1 hour, then Raise the temperature (1°C / min) to 600°C and keep it warm for 0.1 hour, then continue to raise the temperature (5°C / min) to 800°C and keep it warm for 1 hour. The calcined pro...

Embodiment 2

[0033] Prepare 100 ml of 1 mol / liter aluminum sulfate solution, 100 ml of 4 mol / liter sodium hydroxide solution, and 50 ml of 10% (w / v) potassium sulfate solution. Add sodium hydroxide solution (5 ml / min) to aluminum sulfate solution at 30°C under stirring (50 rpm) to obtain amorphous aluminum hydroxide suspension. Filter and wash the suspension, then add the precipitate and potassium sulfate solution into the autoclave, conduct a hydrothermal reaction at 300°C with stirring (50 rpm) for 30 hours, cool, filter, and wash to obtain γ-AlOOH hydrothermal intermediate Product; mix the γ-AlOOH hydrothermal intermediate product with potassium chloride, control the weight ratio of the two to 100:10, place the mixture in a muffle furnace, raise the temperature (0.5°C / min) to 200°C and keep it for 0.5 hours, then Raise the temperature (0.5°C / min) to 650°C and keep it warm for 1 hour, then continue to raise the temperature (1°C / min) to 900°C and keep it warm for 2 hours. The calcined pr...

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Abstract

The invention discloses a method for preparing one-dimensional alumina fiber by a hydrothermal-flux process, which belongs to the technical field of preparation of inorganic chemical materials. In the present invention, inorganic water-soluble aluminum salt is used as raw material, and inorganic alkali or inorganic acid is used as precipitating agent. Firstly, amorphous aluminum hydroxide precipitate is prepared by a normal temperature synthesis method, and then added to an aqueous solution containing an inorganic morphology control agent for hydrothermal reaction. , to obtain a one-dimensional boehmite (γ-AlOOH) intermediate product; then mix γ-AlOOH with flux, and after multi-stage roasting, it can be obtained with a diameter of 10-100nm, a length of 0.5-10μm, and an aspect ratio of 50-200. A one-dimensional alumina fiber with regular appearance and good crystallization. The invention has the advantages of simple process, low cost, high added value and easy industrial popularization. The one-dimensional alumina fiber prepared by the invention has superior performance and high added value, and can be used as a reinforcing material in industries such as aluminum alloy, ceramics, plastics, and rubber.

Description

technical field [0001] The invention relates to a method for preparing one-dimensional alumina fiber by a hydrothermal-flux process, which belongs to the field of preparation of inorganic chemical materials. Background technique [0002] One-dimensional alumina fiber has the characteristics of high melting point (2040°C), high strength (modulus 21GPa), one-dimensional orientation and good compatibility with metal aluminum. It is a reinforcing and toughening agent with excellent mechanical properties. It can be used In the preparation of high-performance aluminum matrix, ceramic matrix and polymer matrix composite materials. [0003] The preparation methods of one-dimensional alumina fibers mainly include gas phase method and liquid phase method. The gas-phase method is to vaporize aluminum-containing substances at a high temperature of 1250-1800 ° C, and then form one-dimensional alumina fibers through gas-phase reaction or vapor-phase deposition. According to different re...

Claims

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Application Information

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IPC IPC(8): C01F7/30B82B3/00
Inventor 向兰何涛波高立东朱万诚朱慎林
Owner TSINGHUA UNIV
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