CN110981472A - High-strength green zirconia ceramic powder and preparation method and application thereof - Google Patents

High-strength green zirconia ceramic powder and preparation method and application thereof Download PDF

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CN110981472A
CN110981472A CN201911400836.XA CN201911400836A CN110981472A CN 110981472 A CN110981472 A CN 110981472A CN 201911400836 A CN201911400836 A CN 201911400836A CN 110981472 A CN110981472 A CN 110981472A
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green
oxide
ceramic powder
zirconia
yttrium
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袁爱灵
胡礼军
刘志
方东阳
毛翔鹏
刘琪
蔡玉珺
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Jiangxi Saici Materials Co ltd
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Abstract

The invention discloses high-strength green zirconia ceramic powder, which consists of yttrium-stabilized zirconia and a green toner; the dosage of the yttrium oxide in the yttrium-stabilized zirconia is 3.5-5.5 mol% of the zirconium oxide; the green colorant comprises the components of aluminum oxide, zinc oxide, chromium oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 16-50: 1.5-10: 0.8-25: 0.2-17: 0.04-2: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2-7.5 wt% of yttrium-stabilized zirconia. In addition, a preparation method and application of the high-strength green zirconia ceramic powder are also disclosed. The green zirconia ceramic powder has the advantages that the adopted raw materials are green and environment-friendly, the sources are rich and easy to obtain, the obtained product has high strength, good toughness, good color development, high glossiness and few defects, and can meet the harsh use requirements in practical application; and the preparation process is simple and efficient, and is beneficial to popularization, application and development.

Description

High-strength green zirconia ceramic powder and preparation method and application thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to high-strength green zirconia ceramic powder suitable for consumer electronics products and a preparation method and application thereof.
Background
The zirconia ceramics has the advantages of high strength, high hardness, corrosion resistance and the like, and in addition, the zirconia ceramics also has the advantages of low thermal conductivity coefficient, low thermal expansion coefficient, low friction coefficient, high chemical stability and the like. Therefore, the zirconia ceramics have wide application and are widely used in the fields of refractory materials, high-temperature structural materials, electronic materials, materials for daily-use kitchenware, molds, solid fuel cells, oxygen sensors and the like.
In recent years, due to the characteristics of excellent performance and good biocompatibility of zirconia, no stimulation to human bodies and the like, the zirconia has been widely used in consumer products such as bracelets, watch chains, buttons, smart watches, smart phones, computers and the like. Due to the strict requirements of manufacturing and inspection of consumer electronics (such as smart watches, smart phones, computers and the like), higher requirements are put forward on both performance and processing of zirconia ceramics. In addition, as the living standard of people is continuously improved, the aesthetic requirements of consumers on product devices are also synchronously improved; moreover, with the application and popularization of new technologies such as 5G network and wireless charging, the market demand of zirconia aesthetic ceramics is further expanded. However, most of the existing consumer electronics products are made of black and white zirconia ceramics, and the existing consumer electronics products lack more beautiful color products and cannot well meet the use requirements of consumers. Therefore, in recent years, colored zirconia ceramics have been studied and developed, but they have defects such as dull color, poor appearance, and particularly low mechanical properties, and it is difficult to satisfy practical requirements of manufacturing, processing, market, and application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-strength green zirconia ceramic and the powder thereof, and the ceramic product with high strength, good toughness, good color development, high glossiness and few defects can be obtained by optimizing the composition. The invention also aims to provide a preparation method and application of the high-strength green zirconia ceramic powder.
The purpose of the invention is realized by the following technical scheme:
the invention provides high-strength green zirconia ceramic powder which consists of yttrium-stabilized zirconia and a green toner; the dosage of the yttrium oxide in the yttrium-stabilized zirconia is 3.5-5.5 mol% of the zirconium oxide; the green colorant comprises the components of aluminum oxide, zinc oxide, chromium oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 16-50: 1.5-10: 0.8-25: 0.2-17: 0.04-2: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2-7.5 wt% of yttrium-stabilized zirconia.
Furthermore, the green colorant comprises the components of aluminum oxide, zinc oxide, chromium oxide, iron oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 20-44: 2-8: 1-20: 0.5-14: 0.05-1.5: 0.05-3: 0.05-0.3.
In the scheme, the yttrium-stabilized zirconia primary crystal has a mesopore with the aperture of 30-40 nm; the primary crystal size of the green colorant is 30-50 nm, and the green colorant is loaded into the mesopores of the yttrium-stabilized zirconia primary crystal.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the high-strength green zirconia ceramic powder provided by the invention comprises the following steps:
(1) synthesis of nano green color agent by coprecipitation method
According to the molar ratio of the components of the green colorant, aluminum ammonium sulfate, zinc nitrate, chromium nitrate, ferric nitrate, titanium nitrate, cobalt nitrate and manganese nitrate are used as raw materials to be mixed, dissolved in pure water to form a salt solution with the concentration of 50-100 g/L, and ammonia water is added to control the pH value of a reaction system to be 7.0-9.0 for precipitation reaction, so that the nano green colorant with the primary crystal size of 30-50 nm is prepared;
(2) preparation of mesoporous yttrium-stabilized zirconia by hydrothermal method
Zirconium oxychloride, yttrium nitrate, ammonia water and a surfactant are used as raw materials, the dosage of the surfactant is 0.5-3.5% of the mass of equimolar zirconium oxide of the zirconium oxychloride, the pH value of a reaction system is controlled to be 7.0-9.0, hydrothermal reaction is carried out at the temperature of 150-190 ℃, and solid-liquid separation is carried out on a reaction product, so that the mesoporous yttrium-stabilized zirconium oxide with the aperture of 30-40 nm is prepared;
(3) preparation of green zirconia ceramic powder
Adding the nano green toner and the mesoporous yttrium stabilized zirconia into pure water to form mixed liquid in which the toner is loaded into mesopores; calcining the product obtained after the solid-liquid separation of the mixed solution to obtain a toner-zirconia complex, and crushing and spray drying to obtain the high-strength green zirconia ceramic powder.
Further, in the preparation method, in the step (3), the calcination temperature is 900-1100 ℃, and the heat preservation time is 3-12 hours.
Further, the surfactant in the preparation method of the invention is one or a combination of LAS (sodium dodecyl benzene sulfonate), APAM (polyacrylamide), CTAB (cetyl trimethyl ammonium bromide).
According to the application of the high-strength green zirconia ceramic powder, the ceramic powder is used as a raw material to manufacture a ceramic blank, and the ceramic blank is sintered at 1350-1450 ℃, so that the high-strength green zirconia aesthetic ceramic product is obtained.
In the scheme, the strength of the ceramic product is 800-1150 MPa, and the color value is-20-a*≤-8、-10≤b*≤10、10≤L*Less than or equal to 50. Preferably, the strength of the ceramic product is 900-1100 MPa, and the color value is-18 & lt & gta*≤-10、-9≤b*≤9、15≤L*≤40。
The invention has the following beneficial effects:
(1) the green zirconia ceramic powder has the advantages of green and environment-friendly raw materials, abundant and easily-obtained sources, high strength, good toughness, good color development, high glossiness and few defects of the obtained product, and can meet the harsh use requirements in practical application.
(2) The preparation method has simple and efficient preparation process and is beneficial to popularization, application and development.
The present invention will be described in further detail with reference to examples.
Detailed Description
The embodiment of the invention relates to high-strength green zirconia ceramic powder which is composed of yttrium-stabilized zirconia and a green toner; the dosage of the yttrium oxide in the yttrium-stabilized zirconia is 3.5-5.5 mol% of the zirconium oxide; the green toner comprises the components of aluminum oxide, zinc oxide, chromium oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 20-44: 2-8: 1-20: 0.5-14: 0.05-1.5: 0.05-3: 0.05-0.3; the addition amount of the green colorant is 2-7.5 wt% of the yttrium-stabilized zirconia. Wherein the yttrium-stabilized zirconia primary crystal contains 30-40 nm mesopores, the primary crystal size of the green colorant is 30-50 nm, and the green colorant is loaded into the mesopores of the yttrium-stabilized zirconia primary crystal. The compositions of the examples of the present invention are shown in table 1.
TABLE 1 composition of high-strength green zirconia ceramic powder of the examples of the present invention
Figure BDA0002347406820000031
The proportion of green toner is mole proportion
The addition amount of green colorant to yttrium-stabilized zirconia
The preparation method of the high-strength green zirconia ceramic powder provided by the embodiment of the invention comprises the following steps:
(1) synthesis of nano green color agent by coprecipitation method
According to the molar ratio of the components of the green colorant, aluminum ammonium sulfate, zinc nitrate, chromium nitrate, ferric nitrate, titanium nitrate, cobalt nitrate and manganese nitrate are used as raw materials to be mixed, dissolved in pure water to form a salt solution with the concentration of 50-100 g/L, and ammonia water is added to control the pH value of a reaction system to be 7.0-9.0 to carry out precipitation reaction, so that the nano green colorant with the primary crystal size of 30-50 nm is prepared;
(2) preparation of mesoporous yttrium-stabilized zirconia by hydrothermal method
Zirconium oxychloride, yttrium nitrate, ammonia water and a surfactant are used as raw materials, wherein the dosage of the surfactant is 0.5-3.5 wt% of the mass of equimolar zirconium oxide of the zirconium oxychloride, the pH value of a reaction system is controlled to be 7.0-9.0, the hydrothermal reaction is carried out for 20 hours at the temperature of 150-190 ℃, and the solid-liquid separation is carried out on the reaction product, so that the mesoporous yttrium-stabilized zirconium oxide with the aperture of 30-40 nm is prepared;
(3) preparation of green zirconia ceramic powder
Adding the nano green toner and the mesoporous yttrium stabilized zirconia into pure water to form mixed liquid in which the toner is loaded into mesopores; calcining the product obtained after the solid-liquid separation of the mixed solution at the temperature of 900-1100 ℃ for 3-12 h to obtain a toner-zirconia composite, and crushing and spray drying to obtain the high-strength green zirconia ceramic powder. The process parameters of the preparation method of each example are shown in table 2.
TABLE 2 Process parameters of the preparation method of high-strength green zirconia ceramic powder of the embodiment of the invention
Figure BDA0002347406820000041
LAS: sodium dodecylbenzenesulfonate; APAM: polyacrylamide; CTAB: cetyl trimethylammonium bromide;
the amount of surfactant used relative to the mass of zirconium oxide in an equimolar amount to zirconium oxychloride.
According to the application of the high-strength green zirconia ceramic powder disclosed by the embodiment of the invention, the ceramic powder is used as a raw material to manufacture a ceramic blank, and the ceramic blank is sintered at 1350-1450 ℃, so that the high-strength green zirconia aesthetic ceramic product is obtained. The sintering temperatures of the examples and the performance indexes of the ceramic products are shown in Table 3.
TABLE 3 sintering temperature and Performance index of high-strength Green zirconia ceramic products according to the examples of the present invention
Figure BDA0002347406820000042

Claims (9)

1. The high-strength green zirconia ceramic powder is characterized in that: consists of yttrium stabilized zirconia and a green toner; the dosage of the yttrium oxide in the yttrium-stabilized zirconia is 3.5-5.5 mol% of the zirconium oxide; the green colorant comprises the components of aluminum oxide, zinc oxide, chromium oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 16-50: 1.5-10: 0.8-25: 0.2-17: 0.04-2: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2-7.5 wt% of yttrium-stabilized zirconia.
2. The high-strength green zirconia ceramic powder of claim 1, wherein: the green toner comprises the components of aluminum oxide, zinc oxide, chromium oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide in a molar ratio of 20-44: 2-8: 1-20: 0.5-14: 0.05-1.5: 0.05-3: 0.05-0.3.
3. The high-strength green zirconia ceramic powder according to claim 1 or 2, characterized in that: the yttrium-stabilized zirconia primary crystal has a mesopore with the aperture of 30-40 nm; the primary crystal size of the green colorant is 30-50 nm, and the green colorant is loaded into the mesopores of the yttrium-stabilized zirconia primary crystal.
4. A method for preparing the high-strength green zirconia ceramic powder according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) synthesis of nano green color agent by coprecipitation method
According to the molar ratio of the components of the green colorant, aluminum ammonium sulfate, zinc nitrate, chromium nitrate, ferric nitrate, titanium nitrate, cobalt nitrate and manganese nitrate are used as raw materials to be mixed, dissolved in pure water to form a salt solution with the concentration of 50-100 g/L, and ammonia water is added to control the pH value of a reaction system to be 7.0-9.0 for precipitation reaction, so that the nano green colorant with the primary crystal size of 30-50 nm is prepared;
(2) preparation of mesoporous yttrium-stabilized zirconia by hydrothermal method
Zirconium oxychloride, yttrium nitrate, ammonia water and a surfactant are used as raw materials, the dosage of the surfactant is 0.5-3.5 wt% of the mass of equimolar zirconium oxide of the zirconium oxychloride, the pH value of a reaction system is controlled to be 7.0-9.0, a hydrothermal reaction is carried out at the temperature of 150-190 ℃, and a reaction product is subjected to solid-liquid separation to obtain mesoporous yttrium-stabilized zirconium oxide with the aperture of 30-40 nm;
(3) preparation of green zirconia ceramic powder
Adding the nano green toner and the mesoporous yttrium stabilized zirconia into pure water to form mixed liquid in which the toner is loaded into mesopores; calcining the product obtained after the solid-liquid separation of the mixed solution to obtain a toner-zirconia complex, and crushing and spray drying to obtain the high-strength green zirconia ceramic powder.
5. The method for preparing high-strength green zirconia ceramic powder according to claim 4, wherein the method comprises the following steps: in the step (3), the calcining temperature is 900-1100 ℃, and the heat preservation time is 3-12 h.
6. The method for preparing high-strength green zirconia ceramic powder according to claim 4, wherein the method comprises the following steps: the surfactant is one or the combination of sodium dodecyl benzene sulfonate, polyacrylamide and hexadecyl trimethyl ammonium bromide.
7. The use of the high-strength green zirconia ceramic powder of any one of claims 1 to 3, wherein: and (3) manufacturing a ceramic blank by using the ceramic powder as a raw material, and sintering at 1350-1450 ℃ to obtain the high-strength green zirconia aesthetic ceramic product.
8. The use of the high strength green zirconia ceramic powder of claim 7, wherein: the strength of the ceramic product is 800-1150 MPa, and the color value is-20 ≤ a*≤-8、-10≤b*≤10、10≤L*≤50。
9. The use of the high strength green zirconia ceramic powder of claim 8, wherein: the strength of the ceramic product is 900-1100 MPa, and the color value is-18 to a*≤-10、-9≤b*≤9、15≤L*≤40。
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