Method for synthesis of black zirconia ceramic powder by organic network process

Abstract

The invention relates to a method for synthesis of black zirconia ceramic powder by an organic network process. The method utilizes organic polymerization reaction to form a network structure by one-step synthesis. Specifically, inorganic Zr<4+>, Y<3+>, Fe<3+>, Cr<3+>, Co<2+>, and Ni<2+> ions occupy an organic three-dimensional network micro-region, and undergoes precipitation reaction with OH<-> diffusing therein, and finally heat treatment is carried out so as to obtain tetragonal crystal form black zirconia ceramic powder. The preparation method provided by the invention has the characteristics of simple technological operation, low cost, high powder purity, high mixability of coloring ions and zirconia, and good present color, is suitable for industrial mass production of black zirconia powder, and is used for production of various black zirconia ceramic products.

Description

technical field

[0001] The invention relates to an organic network preparation method for synthesizing black zirconia ceramic powder, and relates to the field of preparation of inorganic ceramic powder and ceramic materials. Background technique

[0002] Color ZrO 2 With its excellent mechanical properties, such as high hardness, wear resistance, bright colors, metallic luster and no allergy to the human body, ceramics have gradually become a hot material for artificial gemstone decoration materials.

[0003] The common preparation techniques of colored zirconia ceramics are mainly solid phase method and chemical precipitation method. The solid phase method uses micron or nanometer ZrO 2 The solid ceramic powder is fully mixed with various ceramic pigments and sintering aids in a certain proportion, and then sintered at high temperature after molding. Generally speaking, solid-phase sintering adopts the mixing of zirconia and ceramic pigments in zirconia ceramics as physi...

Examples

Embodiment 1

[0040] 1. Preparation of organic network precursor:

[0041] The concentration of 4% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then allowed to stand and cooled to room temperature to obtain a polyvinyl alcohol aqueous solution.

[0042] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0043] Take 70ml of the above-prepared polyvinyl alcohol solution, add 30g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.10g of yttrium nitrate hexahydrate and stir until dissolved; then add 1.60g of ferric nitrate nonahydrate, 2.59g of nonahydrate Chromium nitrate hydrate, 0.85g cobalt nitrate hexahydrate, 0.42g nickel nitrate hexahydrate and stir until uniform; after adding, add 3ml of glutaraldehyde, and stir quickly until a gel is formed;

[0044] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0045] After the above gel was left to s...

Embodiment 2

[0050] 1. Preparation of organic network precursor:

[0051] The concentration of 4% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then allowed to stand and cooled to room temperature to obtain a polyvinyl alcohol aqueous solution.

[0052] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0053] Take 60ml of the above-prepared polyvinyl alcohol solution, add 40g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.46g of yttrium nitrate hexahydrate and stir until dissolved; then add 1.57g of ferric nitrate nonahydrate, Chromium nitrate hydrate, 0.71g cobalt nitrate hexahydrate, 0.29g nickel nitrate hexahydrate and stir until uniform; then add 3ml of glutaraldehyde, and stir quickly until a gel is formed;

[0054] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0055] After the above gel was left to stand for 3 hours, it was soake...

Embodiment 3

[0059] 1. Preparation of organic network precursor:

[0060] The concentration of 6% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then left to cool to room temperature.

[0061] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0062] Take 50ml of the above-prepared polyvinyl alcohol solution, add 50g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.83g of yttrium nitrate hexahydrate and stir until dissolved; then add 2.40g of ferric nitrate nonahydrate, 3.96g of nonahydrate Chromium nitrate hydrate, 0.56g cobalt nitrate hexahydrate, 0.58g nickel nitrate hexahydrate and stir until uniform; then add 5ml of glutaraldehyde, and stir quickly until a gel is formed;

[0063] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0064] After the above gel was left to stand for 3 hours, it was soaked in ammonia water (25% concentration by ...

technical field

[0001] The invention relates to an organic network preparation method for synthesizing black zirconia ceramic powder, and relates to the field of preparation of inorganic ceramic powder and ceramic materials. Background technique

[0002] Color ZrO 2 With its excellent mechanical properties, such as high hardness, wear resistance, bright colors, metallic luster and no allergy to the human body, ceramics have gradually become a hot material for artificial gemstone decoration materials.

[0003] The common preparation techniques of colored zirconia ceramics are mainly solid phase method and chemical precipitation method. The solid phase method uses micron or nanometer ZrO 2 The solid ceramic powder is fully mixed with various ceramic pigments and sintering aids in a certain proportion, and then sintered at high temperature after molding. Generally speaking, solid-phase sintering adopts the mixing of zirconia and ceramic pigments in zirconia ceramics as physi...

Examples

Embodiment 1

[0040] 1. Preparation of organic network precursor:

[0041] The concentration of 4% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then allowed to stand and cooled to room temperature to obtain a polyvinyl alcohol aqueous solution.

[0042] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0043] Take 70ml of the above-prepared polyvinyl alcohol solution, add 30g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.10g of yttrium nitrate hexahydrate and stir until dissolved; then add 1.60g of ferric nitrate nonahydrate, 2.59g of nonahydrate Chromium nitrate hydrate, 0.85g cobalt nitrate hexahydrate, 0.42g nickel nitrate hexahydrate and stir until uniform; after adding, add 3ml of glutaraldehyde, and stir quickly until a gel is formed;

[0044] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0045] After the above gel was left to s...

Embodiment 2

[0050] 1. Preparation of organic network precursor:

[0051] The concentration of 4% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then allowed to stand and cooled to room temperature to obtain a polyvinyl alcohol aqueous solution.

[0052] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0053] Take 60ml of the above-prepared polyvinyl alcohol solution, add 40g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.46g of yttrium nitrate hexahydrate and stir until dissolved; then add 1.57g of ferric nitrate nonahydrate, Chromium nitrate hydrate, 0.71g cobalt nitrate hexahydrate, 0.29g nickel nitrate hexahydrate and stir until uniform; then add 3ml of glutaraldehyde, and stir quickly until a gel is formed;

[0054] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0055] After the above gel was left to stand for 3 hours, it was soake...

Embodiment 3

[0059] 1. Preparation of organic network precursor:

[0060] The concentration of 6% polyvinyl alcohol and water are mixed in proportion, heated and stirred at about 85° C. for 2-3 hours, and then left to cool to room temperature.

[0061] 2.Zr 4+ and preparation of colored ionic / organic network gels:

[0062] Take 50ml of the above-prepared polyvinyl alcohol solution, add 50g of zirconium oxychloride according to the proportion and stir until it is completely dissolved; then add 1.83g of yttrium nitrate hexahydrate and stir until dissolved; then add 2.40g of ferric nitrate nonahydrate, 3.96g of nonahydrate Chromium nitrate hydrate, 0.56g cobalt nitrate hexahydrate, 0.58g nickel nitrate hexahydrate and stir until uniform; then add 5ml of glutaraldehyde, and stir quickly until a gel is formed;

[0063] 3. Zr 4+ and color ionic / organic network gel post-treatment:

[0064] After the above gel was left to stand for 3 hours, it was soaked in ammonia water (25% concentration by ...

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