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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, affect film quality, structural transformation, etc., and achieve the effects of improving fluidity, avoiding splashing, and reducing pores

Active Publication Date: 2020-07-10
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

AI Technical Summary

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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  • Preparation method of cerium oxide particles for coating
  • Preparation method of cerium oxide particles for coating
  • Preparation method of cerium oxide particles for coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A method for preparing high-purity, high-density, and low-splashing cerium oxide particles includes the following steps:

[0033] Weigh 5000g of cerium oxide powder with a purity of ≥99.99%, add a certain amount of deionized water to granulate to obtain flake cerium oxide, and weigh 5.3kg after granulation. The flake cerium oxide is ground and crushed into fine particles, and the pretreated powder with a particle size of 3 And 5.25g / cm 3 . Place the two blanks together in a smart box-type muffle furnace for high-temperature sintering. The sintering process is: heat up to 400°C for 1h in 3 hours, heat up to 600°C in 2 hours, hold for 1h, and heat up to 1000°C for 1h in 4 hours. The temperature is raised to 1300°C in 4 hours for 1 hour, the temperature is raised to 1400°C in 2 hours, and the temperature is raised to 1550°C for 3 hours.

[0034] The highest sintering temperature is 1550°C. After cooling in a high-temperature furnace, a high-density cerium oxide block is obtain...

Embodiment 2

[0035] Example 2 (comparative example)

[0036] A method for preparing cerium oxide particles includes the following steps:

[0037] Weigh 5000g of cerium oxide powder with purity ≥99.99%, add a certain amount of deionized water to granulate into flakes, and weigh 5.3kg after granulation. Grind and crush the flake-shaped cerium oxide, use a special standard sieve to screen out 3-6mm particles, and place them directly in a smart box-type muffle furnace for high-temperature sintering. The sintering process is: heating up to 400 degrees Celsius for 1 hour, The temperature is raised to 600°C in 1 hour for 1 hour, the temperature is raised to 1000°C in 3 hours, and the temperature is raised to 1300°C for 3 hours. The highest sintering temperature is 1300℃, and the mercury intrusion analysis results are as follows image 3 As shown, the obtained cerium oxide particles are measured by mercury intrusion method to test the particle volume density of 5.95g / cm 3 , The relative density is 83....

Embodiment 3

[0038] Example 3 (comparative example)

[0039] A method for preparing cerium oxide particles includes the following steps:

[0040] Weigh 5000g of cerium oxide powder with a purity of ≥99.99%, add a certain amount of deionized water to granulate to obtain flake cerium oxide, and weigh 5.3kg after granulation. The flake cerium oxide is ground and crushed into fine particles, and the pretreated powder with a particle size of 3 . The green body is placed in a smart box-type muffle furnace for high-temperature sintering. The sintering process is as follows: 2 hours to heat up to 400 degrees for 1 hour, 1 hour to 600 degrees for 1 hour, 3 hours to 1000 degrees for 1 hour, 3 hours to heat up Keep the temperature at 1300 degrees for 3 hours. The highest sintering temperature is 1300℃, and the mercury intrusion analysis results are as follows Figure 4 As shown, the obtained cerium oxide particles are measured by mercury intrusion method to test the particle volume density of 6.0295g / cm...

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Abstract

The invention discloses a preparation method of cerium oxide particles for coating, which comprises the following steps: (1) by using high-purity cerium oxide powder as a raw material, adding deionized water into the high-purity cerium oxide powder, and carrying out granulation treatment to obtain cerium oxide flakes which are tightly combined; (2) grinding and crushing the obtained flakes, and screening out pretreated powder with the particle size of less than 0.1 mm; (3) putting the obtained pretreated powder into a rubber sleeve, and carrying out isostatic cool pressing to form a green body; and (4) sintering the obtained green body according to the following sintering process, raising the temperature to 300 to 400 DEG C within 2 to 3 hours and keeping the temperature for 1 to 2 hours;raising the temperature to 600-800 DEG C within 2 hours and preserving heat for 1-2 hours, raising the temperature to 1000-1200 DEG C within 4 hours and preserving heat for 1-2 hours, raising the temperature to 1300 DEG C within 4 hours and preserving heat for 1-2 hours, raising the temperature to 1400 DEG C within 2 hours and preserving heat for 1-2 hours, and raising the temperature to 1450-1550DEG C within 1 hour and preserving heat for 3-5 hours; and (5) cooling to obtain a cerium oxide sintered blank, and crushing and screening the blank to obtain cerium oxide particles for coating. Thecerium 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 evaporation coating, and the film can be used in different industries such as semiconductor chips, optoelectronic devices, sensors, and OLEDs. [0003] CeO 2 It belongs to the cubic crystal system. The cerium ion in cerium oxide has 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 realize the transformation of these two valence states, enabling it to store and release oxygen and maintain the fluorite-type structure. Therefore, it has been widely used in permanent magnet materials, optical glass, fast ion conductors, and automotive catalysts. [0004] High-purity, high-density, low-spray cerium oxide particles are high-qual...

Claims

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Application Information

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Patent Type & Authority Applications(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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