Preparation method for micron zirconium carbide whisker

A zirconium carbide and whisker technology, which is applied in the field of ultra-high temperature ceramic matrix composite material reinforcement preparation, can solve the problems of limited output of zirconium carbide whiskers, large experimental errors, and high equipment requirements, and achieve good shape, simple steps, and equipment undemanding effects

Inactive Publication Date: 2019-07-23
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In general, the preparation of zirconium carbide whiskers by chemical vapor deposition has problems such as limited output, long cycle time, many control parameters, high equipment requirements, and relatively large experimental errors. It is urgent to develop new processes to make up for the shortcomings of existing processes.

Method used

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  • Preparation method for micron zirconium carbide whisker
  • Preparation method for micron zirconium carbide whisker
  • Preparation method for micron zirconium carbide whisker

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: Prepare raw materials for ball milling:

[0033] According to molar ratio ZrO 2 :C:Ni:NaF=1:3:0.2:0.1 Prepare 30g of raw materials, perform ball milling according to the mass ratio of ball to material=3:1, and the speed of rotation is 70r / min, and the ball milling time is 5h. A uniform precursor powder is obtained.

[0034] Step 2: Sifting:

[0035] The precursor powder obtained in step 1 is sieved with 100 meshes to obtain a powder with uniform particle size.

[0036] Step 3: Carbothermal Reduction

[0037] Weigh 2 g of the powder obtained in step 2, put it into a graphite crucible, and carry out carbothermal reduction reaction in a tube furnace. Reaction temperature: 1500°C, holding time: 4h, heating rate: 5K / min, atmosphere: Ar, Ar flow rate: 20cc / min, zirconium carbide whiskers were prepared by carbothermal reduction reaction.

[0038] Step 4: pickling to remove impurities

[0039] Prepare a sulfuric acid solution with a mass fraction of 70%, put the z...

Embodiment 2

[0041] Step 1: Prepare raw materials for ball milling:

[0042] According to molar ratio ZrO 2 :C:Ni:NaF=1:3:0.2:0.3 Prepare 30g of raw material for ball milling, perform ball milling according to mass ratio of ball to material=3:1, speed of 90r / min, ball milling time is 4h. A uniform precursor powder is obtained.

[0043] Step 2: Sifting:

[0044] The precursor powder obtained in step 1 is sieved with 100 meshes to obtain a powder with uniform particle size.

[0045] Step 3: Carbothermal Reduction

[0046] Weigh 2 g of the powder obtained in step 2, put it into a graphite crucible, and carry out carbothermal reduction reaction in a tube furnace. Reaction temperature: 1500°C, holding time: 4h, heating rate: 5K / min, atmosphere: Ar, Ar gas flow: 20cc / min, zirconium carbide whiskers were prepared by carbothermal reduction reaction.

[0047] Step 4: pickling to remove impurities

[0048] Prepare a sulfuric acid solution with a mass fraction of 70%, put the zirconium carbide ...

Embodiment 3

[0050] Step 1: Prepare raw materials for ball milling:

[0051]According to the molar ratio of ZrO2:C:Ni:NaF=1:4:0.2:0.3, 30g of raw materials were prepared, ball milling was carried out according to the mass ratio of ball to material=3:1, and the rotation speed was 90r / min, and the ball milling time was 5h. A uniform precursor powder is obtained.

[0052] Step 2: Sifting:

[0053] The precursor powder obtained in step 1 is sieved with 100 meshes to obtain a powder with uniform particle size.

[0054] Step 3: Carbothermal Reduction

[0055] Weigh 2g of the powder obtained in step 2, put it into a graphite crucible, and carry out carbothermal reduction reaction in a tube furnace. Reaction temperature: 1500°C, holding time: 4h, heating rate: 5K / min, atmosphere: Ar, Ar gas flow: 20cc / min, zirconium carbide whiskers were prepared by carbothermal reduction reaction.

[0056] Ni

[0057] Step 4: pickling to remove impurities

[0058] Prepare a sulfuric acid solution with a mas...

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Abstract

The invention relates to a preparation method for a micron zirconium carbide whisker. The preparation method comprises the following steps: taking ZrO2-C (carbon black)-Ni-NaF as a reaction system; uniformly ball-milling a precursor powder and then sieving; performing carbon thermal reduction reaction under a high-temperature argon environment; removing impurities by acid pickling, thereby acquiring the zirconium carbide whisker with a good appearance. The invention has the beneficial effects that parameters involved in carbon thermal reduction reaction can be easily controlled and process reliability and repeatability are higher; the method is simple in operation in the whole process, simple in steps, short in period and low in cost, has low requirements for equipment and is suitable forvolume production of zirconium carbide whisker; the zirconium carbide whisker prepared according to the preparation method provided by the invention has a diameter of about 1-3um, a length of about 30-100um, a higher ratio of length to diameter (20-50), few impurities and good appearance; the zirconium carbide whisker prepared according to the preparation method provided by the invention can be used as a reinforcing phase for reinforcing and toughening a superhigh temperature composite ceramic or superhigh temperature ceramic-based composite material.

Description

technical field [0001] The invention belongs to a preparation method of zirconium carbide whiskers, and relates to a preparation method of micron zirconium carbide whiskers, which is mainly used in the field of preparation of ultra-high temperature ceramic matrix composite material reinforcements. Background technique [0002] Silicon carbide whiskers (SiC W ) as a reinforcement can meet the requirements of high modulus, high strength and low thermal expansion rate at the same time. It is currently one of the most widely used and most mature whisker reinforcements. Methods A porous prefabricated body was prepared, and then a matching interface layer and matrix were prepared in the prefabricated body by processes such as precursor immersion cracking and chemical vapor deposition to form a ceramic matrix composite material. Silicon carbide whiskers can play a good bearing capacity and crack deflection effect in composite materials, and play an effective role in strengthening ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/36C30B29/62C30B1/10
CPCC30B1/10C30B29/36C30B29/62
Inventor 成来飞程硕叶昉张立同
Owner NORTHWESTERN POLYTECHNICAL UNIV
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