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A kind of preparation method of cerium oxide particles for coating

A cerium oxide and particle technology, which is applied in the field of preparation of cerium oxide particles for coating, can solve the problems of difficult densification of cerium oxide, influence film quality, structural transformation, etc. Effect

Active Publication Date: 2022-04-15
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Cerium oxide is prone to oxygen loss reaction during vacuum sintering, resulting in structural transformation. This transformation will become a resistance to densification, making it difficult to densify cerium oxide during vacuum sintering.
The density of cerium oxide particles prepared by granulation combined with atmospheric pressure sintering process is generally 75-85%, often containing a large number of closed pores, and the gas in the closed pores is suddenly released during the evaporation process, resulting in splashing, which seriously affects the quality of the film
CeO with sintering aid 2 The particle density is improved, but the impurities introduced by the additives will also cause splashing

Method used

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  • A kind of preparation method of cerium oxide particles for coating
  • A kind of preparation method of cerium oxide particles for coating
  • A kind of preparation method of cerium oxide particles for coating

Examples

Experimental program
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Effect test

Embodiment 1

[0032] A method for preparing high-purity, high-density, low-sputter cerium oxide particles, comprising the steps of:

[0033] Weigh 5000 g of cerium oxide powder with a purity of ≥99.99%, add a certain amount of deionized water and granulate to obtain flaky cerium oxide, with a weight of 5.3 kg after granulation. The flaky cerium oxide is ground and crushed into fine particles, and the pretreated powder with a particle size of less than 0.1 mm is sieved through a standard sieve with an aperture of 0.1 mm, and loaded into two special rubber cylinders, with 863 g and 832.9 g of materials respectively, and then Placed in a cold isostatic press for molding, the molding pressure is 200Mpa, and the initial density of the two green bodies measured after taking out is 5.5g / cm 3 and 5.25g / cm 3 . Place the two blanks together in an intelligent box-type muffle furnace for high-temperature sintering. The sintering process is as follows: heat up to 400 degrees for 1 hour in 3 hours, hea...

Embodiment 2

[0035] Embodiment 2 (comparative example)

[0036] A method for preparing cerium oxide particles, comprising the steps of:

[0037] Weigh 5000g of cerium oxide powder with a purity ≥ 99.99%, add a certain amount of deionized water and granulate it into flakes, with a weight of 5.3kg after granulation. Grinding and crushing the formed flake cerium oxide, using a special standard sieve to screen out 3-6mm particles, and directly placing them in an intelligent box-type muffle furnace for high-temperature sintering. The sintering process is: heat up to 400 degrees for 2 hours and hold for 1 hour. 1 hour to 600 degrees for 1 hour, 3 hours for 1000 degrees for 1 hour, 3 hours for 1300 degrees for 3 hours. The highest sintering temperature is 1300°C, and the mercury intrusion analysis results are as follows image 3 As shown, the obtained cerium oxide particles are tested by mercury porosimetry and have a particle volume density of 5.95g / cm 3 , The relative density is 83.4%, the o...

Embodiment 3

[0038] Embodiment 3 (comparative example)

[0039] A method for preparing cerium oxide particles, comprising the steps of:

[0040] Weigh 5000 g of cerium oxide powder with a purity of ≥99.99%, add a certain amount of deionized water and granulate to obtain flaky cerium oxide, with a weight of 5.3 kg after granulation. The flaky cerium oxide is ground and broken into fine particles, and the pretreated powder with a particle size of less than 0.1mm is sieved through a standard sieve with a hole diameter of 0.1mm, and put into a special rubber cylinder with a charge of 860g, and then placed in a cold isostatic press Molded in the machine, the molding pressure is 200Mpa, and the initial density of the green body after taking out is 5.5g / cm 3 . Place the green body in an intelligent box-type muffle furnace for high-temperature sintering. The sintering process is as follows: heat up to 400 degrees for 1 hour for 2 hours, heat for 1 hour for 600 degrees for 1 hour, heat for 1 hour...

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Abstract

The invention discloses a method for preparing cerium oxide particles for coating, which comprises the following steps: (1) using high-purity cerium oxide powder as a raw material, adding deionized water to it and performing granulation treatment to obtain tightly bound cerium oxide Flakes; (2) Grinding and crushing the obtained flakes, and sieving the pretreated powders <0.1mm; (3) Packing the obtained pretreated powders into rubber sleeves for cold isostatic pressing into body. (4) Sinter the obtained green body according to the following sintering process: heat up to 300-400°C for 2-3 hours and keep it for 1h-2h, raise it to 600-800°C for 1h-2h in 2 hours, and heat it up to 1000°C-4 hours 1200°C for 1h-2h, 4 hours to 1300°C for 1h-2h, 2 hours to 1400°C for 1-2h, 1 hour to 1450-1550°C for 3h-5h; (5) cooling to obtain cerium oxide sintering The blank is crushed and sieved to obtain cerium oxide particles for coating. The cerium oxide particles produced by the method have the advantages of high purity, high density, low splashing and the like.

Description

technical field [0001] The invention relates to a method for preparing cerium oxide particles for coating, and belongs to the technical field of coating materials. Background technique [0002] Cerium oxide particles are used for evaporative coating, and its thin films can be used in different industries such as semiconductor chips, optoelectronic devices, sensors, and OLEDs. [0003] CeO 2 Belonging to the cubic crystal system, cerium ions in cerium oxide have two valence states of +3 and +4, and under different oxygen environments, oxygen-rich and oxygen-poor can realize the transition between the two valence states. Cerium oxide itself can achieve these two valence transitions, allowing it to store and release oxygen and maintain a fluorite-type structure. Therefore, it has been widely used in permanent magnet materials, optical glass, fast ion conductors, and catalysts for automobiles. [0004] High-purity, high-density, low-sputter cerium oxide particles are high-qua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/50C04B35/622C23C14/08C23C14/24C23C14/30
CPCC04B35/50C04B35/622C23C14/08C23C14/24C23C14/30C04B2235/3229C04B2235/6562C04B2235/6567C04B2235/6583C04B2235/96
Inventor 白雪刘宇阳桂涛杨磊王星明储茂友韩沧段华英
Owner 有研资源环境技术研究院(北京)有限公司
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