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A kind of preparation method of rod-shaped zirconia whisker

A technology of zirconia and phase zirconia, applied in the field of preparation of new inorganic structural materials, can solve the problems of difficult control of heat treatment and washing process, great influence on performance, long production cycle, etc., and achieve good uniformity of reaction system and easy monitoring and control, low cost effect

Active Publication Date: 2019-07-26
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of zirconia whiskers in this application is similar to the sol-gel method, the process is relatively complicated, and the production cycle is long. When the gel inorganic polymer is transformed into an amorphous zirconia structure during heat treatment, the homogeneity and microcrystallization of the structure have a great influence on the performance

Method used

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  • A kind of preparation method of rod-shaped zirconia whisker
  • A kind of preparation method of rod-shaped zirconia whisker
  • A kind of preparation method of rod-shaped zirconia whisker

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A kind of preparation method of rod-shaped zirconia whisker of the present embodiment, comprises the following steps:

[0037] (1) Add 1.00g tetragonal zirconia, 3.5g flux-zinc sulfate (ZnSO 4 ·7H 2 O) Grinding to a particle size of 80 mesh powdery particles respectively, mixing uniformly to obtain the reaction raw materials; wherein, the tetragonal phase zirconia and the flux--zinc sulfate (ZnSO 4 ·7H 2 The molar ratio of O) is 1:1.5; the mass of absolute ethanol added when the flux is ground is 30% of the mass of the flux.

[0038] (2) Put the reaction raw materials into a corundum crucible, and place it in a heating device—resistance furnace, raise the temperature to 900°C at a heating rate of 5°C / min, keep the temperature constant for 60min, and cool naturally to obtain a sintered product.

[0039] (3) According to the mass ratio of material to liquid of 1:15, add deionized water to the sintered product to soak, and stir and soak in a water bath crucible at 80°C ...

Embodiment 2

[0043] A kind of preparation method of rod-shaped zirconia whisker of the present embodiment, comprises the following steps:

[0044] (1) Mix 0.8g tetragonal zirconia, 1.20g flux -- sodium sulfate (Na 2 SO 4 ) were ground to a particle size of 100 mesh powdery particles, mixed uniformly to obtain the reaction raw materials; wherein, the tetragonal phase zirconia and the flux--sodium sulfate (Na 2 SO 4 ) in a molar ratio of 1:1.3; the quality of absolute ethanol added when the flux is ground is 20% of the mass of the flux.

[0045] (2) Put the reaction raw materials into a corundum crucible, place it in a heating device—resistance furnace, raise the temperature to 850°C at a heating rate of 10°C / min, keep the temperature constant for 75min, and cool naturally to obtain a sintered product.

[0046] (3) According to the mass ratio of material to liquid of 1:15, add deionized water to the sintered product for soaking, and stir and soak for 3 hours in a constant temperature wate...

Embodiment 3

[0050] A kind of preparation method of rod-shaped zirconia whisker of the present embodiment, comprises the following steps:

[0051] (1) 1.2g tetragonal zirconia, 4.74g composite flux -- sodium sulfate (Na 2 SO 4 ) and zinc sulfate (ZnSO 4 ·7H 2 O) Grinding to a particle size of 70 mesh powdery particles respectively, mixing uniformly to obtain the reaction raw materials; wherein, tetragonal phase zirconia and flux--sodium sulfate (Na 2 SO 4 ) in a molar ratio of 1:1; sodium sulfate (Na 2 SO 4 ) and zinc sulfate (ZnSO 4 ·7H 2 The molar ratio of O) is 1:1.2; the quality of dehydrated alcohol added when the composite flux is ground is 40% of the mass of the flux.

[0052] (2) Put the reaction raw materials into a corundum crucible, and place it in a heating device—a muffle furnace, raise the temperature to 950°C at a heating rate of 8°C / min, keep the temperature constant for 45min, and cool naturally to obtain a sintered product.

[0053] (3) According to the mass rati...

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Abstract

The invention discloses a preparation method of a rod-like zirconium oxide crystal whisker and belongs to the field of inorganic structure materials. The preparation method of the rod-like zirconium oxide crystal whisker comprises the following steps: grinding tetragonal-phase zirconium oxide and a fluxing agent into powdery grains respectively; uniformly mixing the powdery grains to obtain a reaction raw material, wherein the mol ratio of the tetragonal-phase zirconium oxide to the fluxing agent ranges from (1 to 1) to (1 to 1.5); raising the temperature of the reaction raw material to 850 DEG C to 1000 DEG C and carrying out calcination treatment for 30min to 90min; cooling to obtain a corresponding sintered product; adding the sintered product into de-ionized water and carrying out stirring and immersion treatment under the condition that the temperature is controlled to 70 DEG C to 90 DEG C; filtering to obtain a white solid powder cake; carrying out drying treatment on the obtained white solid powder cake to obtain the white rod-like zirconium oxide crystal whisker. The preparation method disclosed by the invention has a simple technological process and moderate calcining temperature; a reaction system has good uniformity and the cost is low; the yield of a product is 80 percent or above; the rod-like zirconium oxide crystal whisker product has a uniform microcosmic shape and high yield; the fluxing agent is easy to wash off and the rod-like zirconium oxide crystal whisker product is suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of preparation of novel inorganic structural materials, more specifically, to a preparation method of rod-shaped zirconia whiskers, a material with toughening properties. Background technique [0002] Whiskers are artificially prepared or naturally formed nanofibers that exist in the form of single crystals. They are micro-nano-scale rod-shaped fibers grown from single crystals with high purity. Their diameters are very small and do not exist in conventional materials. Defects such as grain boundaries, dislocations and holes, etc., and the atomic arrangement is highly ordered, so its strength is close to the theoretical value of a complete grain, so whiskers have excellent mechanical properties: high mechanical strength, high elastic modulus , high strength, high hardness and other properties. Due to the above characteristics of whiskers, it is used as a reinforcing and toughening additive for emerging comp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B29/62C30B9/12
CPCC30B9/12C30B29/16C30B29/62
Inventor 方一航张梦贤张平赵先锐冯尚申吴建波陈基根薛双喜王天乐霍颜秋
Owner TAIZHOU UNIV