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Method for preparing hexagonal phase aluminum nitride nanofiber by using electrostatic spinning and ammonia nitridation

An electrospinning, phase aluminum nitride technology is applied in the field of electrospinning combined with ammonia nitridation to prepare hexagonal aluminum nitride nanofibers, which can solve the problems of complex post-processing process and high reaction temperature, and achieves low cost of raw materials, The effect of reducing the reaction temperature and simplifying the production equipment

Inactive Publication Date: 2012-07-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction temperature required by this method is still high, and the product needs to be decarbonized after the reaction, and the post-treatment process is complicated.

Method used

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  • Method for preparing hexagonal phase aluminum nitride nanofiber by using electrostatic spinning and ammonia nitridation
  • Method for preparing hexagonal phase aluminum nitride nanofiber by using electrostatic spinning and ammonia nitridation
  • Method for preparing hexagonal phase aluminum nitride nanofiber by using electrostatic spinning and ammonia nitridation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 3ml of deionized water and 7ml of absolute ethanol and mix evenly; dissolve 0.75g of aluminum nitrate in the hydroalcoholic solution; then add 1.05g of polyvinylpyrrolidone (number average molecular weight 1300000) to the above solution, and stir until the solution becomes clear transparent.

[0038] The obtained precursor solution was electrospun: at room temperature, the humidity was controlled at 25%, the spinning voltage was set to 10kv, the propulsion speed of the propulsion pump was 15 μL / min, and the receiving distance was 15cm.

[0039] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 2° C. / min and a calcination temperature of 500° C. After 6 hours of heat preservation, the temperature was naturally lowered to obtain alumina nanofibers.

[0040] The calcined fibers were transferred to a tube-type atmosphere furnace, and ammonia gas was introduced. The flow rate of ammonia gas was 400mL / min, and the heating rate of ...

Embodiment 2

[0043]Take 3ml of deionized water and 7ml of absolute ethanol and mix evenly. Dissolve 0.75g of aluminum nitrate in the hydroalcoholic solution; then add 0.95g of polyvinylpyrrolidone (number average molecular weight: 1,300,000) to the above solution, and stir until the solution becomes clear and transparent.

[0044] The obtained precursor solution was electrospun: at room temperature, the humidity was controlled at 25%, the spinning voltage was set to 10kv, the propulsion speed of the propulsion pump was 15 μL / min, and the acceptance distance was 15cm.

[0045] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 3° C. / min and a calcination temperature of 600° C. After holding for 4 hours, the temperature was naturally lowered to obtain alumina nanofibers.

[0046] The calcined fibers were transferred to a tube-type atmosphere furnace, and ammonia gas was introduced. The flow rate of ammonia gas was 400mL / min. The heating rate of the tu...

Embodiment 3

[0049] Take 3ml of deionized water and 7ml of absolute ethanol and mix evenly; dissolve 0.75g of aluminum nitrate in the hydroalcoholic solution; then add 0.95g of polyvinylpyrrolidone (number average molecular weight 1300000) to the above solution, and stir until the solution becomes clear transparent.

[0050] The obtained precursor solution was electrospun: at room temperature, the humidity was controlled at 25%, the spinning voltage was set to 10kv, the propulsion speed of the propulsion pump was 15 μL / min, and the acceptance distance was 15cm.

[0051] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 1° C. / min and a calcination temperature of 500° C. After 6 hours of heat preservation, the temperature was naturally lowered to obtain alumina nanofibers.

[0052] The calcined fibers were transferred to a tube-type atmosphere furnace, and ammonia gas was introduced. The flow rate of ammonia gas was 400mL / min. The heating rate of the...

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Abstract

The invention relates to a method for preparing a hexagonal phase aluminum nitride nanofiber by using electrostatic spinning and ammonia nitridation. The method comprises the following steps of: (1) mixing ethanol and water to obtain a water ethanol mixed solution; and then adding aluminum nitrate to the water ethanol mixed solution; adding polyvinyl pyrrolidone to the water ethanol mixed solution; and stirring the water ethanol mixed solution until obtaining a precursor solution; (2) carrying out electrostatic spinning by using the precursor solution; (3) calcining the fiber obtained in the step (2) in the air atmosphere; heating the fiber to 500-600 DEG C at a heating speed of 1-3 DEG C / min; and preserving the heat of the fiber for 4-6 h; (4) after cooling the fiber to the room temperature, heating alumina nanofiber, which is obtained after the calcining, in the atmosphere of continuously introducing the ammonia to 1200-1400 DEG C; and preserving the heat of the alumina nanofiber for 4-9 h. The preparation method provided by the invention has the advantages of simple method, low raw material cost, low reaction temperature of nitrided alumina and short reaction time; and the hexagonal phase aluminum nitride nanofiber obtained by the preparation method provided by the invention has high purity.

Description

technical field [0001] The invention belongs to the field of preparation of aluminum nitride ceramic fibers, in particular to a method for preparing hexagonal phase aluminum nitride nanofibers by electrospinning combined with ammonia nitriding. Background technique [0002] Aluminum nitride ceramics have excellent physical and chemical properties such as high thermal conductivity, low expansion coefficient, high strength, good thermal and chemical stability, high resistivity and low dielectric loss. Circuit substrates, semiconductor module circuits, luminescent materials and other fields have broad application prospects. The one-dimensional nanostructured aluminum nitride ceramics not only retains the above advantages, but also expands the application field of aluminum nitride ceramics to the future nano-devices, nano-circuits, and nano-system centers due to the influence of the nano-size effect. Aluminum nitride ceramic fiber can also be used as a mechanically reinforced c...

Claims

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Application Information

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IPC IPC(8): C04B35/581C04B35/622
Inventor 王宏志丁狄李耀刚张青红
Owner DONGHUA UNIV
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