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

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

Inactive Publication Date: 2010-04-14
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 fibers. The basic idea: firstly prepare amorphous aluminum hydroxide precursor at room temperature, and then use inorganic morphology control agent to selectively adsorb γ-AlOOH under hydrothermal conditions to achieve directional growth of γ-AlOOH to obtain one-dimensional γ-AlOOH with high aspect ratio; Slow heating and flux roasting methods realize the low-temperature slow dehydration and structural reforming of one-dimensional γ-AlOOH to obtain a one-dimensional one-dimensional 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 simple process, low cost and easy promotion. The alumina fiber thus obtained 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.

[0022] The pr...

Embodiment 1

[0031] Prepare 100 ml of 0.5 mol / liter aluminum chloride solution, 100 ml of 1.5 mol / liter ammonia solution, and 50 ml of 1% (w / v) sodium sulfate solution. Add the aqueous ammonia solution (2 ml / min) to the aluminum chloride solution at 25° C. and stirring (300 rpm) to obtain an amorphous aluminum hydroxide suspension. The suspension was filtered and washed, and then the precipitate and sodium sulfate solution were added to the autoclave. The reaction was hydrothermally reacted at 250°C and stirring (100 rpm) for 8 hours, cooled, filtered, and washed 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, put the mixture in a muffle furnace, raise the temperature (2°C / min) to 250°C and keep it for 1 hour, then Increase the temperature (1°C / min) to 600°C and keep it for 0.1 hour, then continue to increase the temperature (5°C / min) to 800°C and keep it for 1 hour. T...

Embodiment 2

[0033] Prepare 100 mL of 1 mol / L aluminum sulfate solution, 100 mL of 4 mol / L sodium hydroxide solution, and 50 mL of 10% (w / v) potassium sulfate solution. Add the sodium hydroxide solution to the aluminum sulfate solution (5 ml / min) under stirring (50 rpm) at 30°C to obtain an amorphous aluminum hydroxide suspension. The suspension was filtered and washed, and then the precipitate and potassium sulfate solution were added to the autoclave. The reaction was hydrothermally reacted at 300°C and stirring (50 rpm) for 30 hours, cooled, filtered and washed 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 Increase the temperature (0.5°C / min) to 650°C and keep it for 1 hour, continue to increase the temperature (1°C / min) to 900°C and keep it for 2 h...

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Abstract

The invention relates to a preparation method of one-dimensional alumina fibers through a hydrothermal-flux technology and pertains to the technical field of inorganic chemical material preparation. The invention adopts water soluble inorganic aluminum salt as raw material and inorganic base or inorganic acid as precipitator; amorphous aluminium hydroxide deposit is first prepared by a normal temperature synthesis method and then added into water solution of inorganic morphology control agent for hydrothermal reaction to obtain an intermediate product of one-dimensional boehmite (gamma-AlOOH)which is then mixed with the flux so as to obtain the one-dimensional alumina fibers with the diameter of 10-100 nm, the length of 0.5-10 Mum, the length-diameter ratio of 50-200, regular morphology and good crystallization. The invention has simple technology, low cost and high additional value, and is easy to be popularized industrially. The one-dimensional alumina fibers prepared by the invention have excellent performance, high additional value and are capable of being applied to the industries of aluminium alloy, ceramic, plastic, rubber, etc., as reinforcing materials.

Description

Technical field [0001] The invention relates to a method for preparing one-dimensional alumina fibers by a hydrothermal-flux process, and 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℃), high strength (modulus 21GPa), one-dimensional orientation and good compatibility with metal aluminum. It is a reinforcing and toughening agent with excellent mechanical properties. Used to prepare high-performance aluminum-based, ceramic-based and polymer-based composite materials. [0003] One-dimensional alumina fiber preparation methods mainly include gas phase method and liquid phase method. The gas phase method is to vaporize the aluminum-containing material at a high temperature of 1250-1800°C, and then form one-dimensional alumina fibers through gas phase reaction or vapor deposition. According to the different reactants, the gas phase method can be divide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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