CN111205089B - High-wave-transmittance green zirconia ceramic, preparation method thereof and prepared product - Google Patents

High-wave-transmittance green zirconia ceramic, preparation method thereof and prepared product Download PDF

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CN111205089B
CN111205089B CN202010056149.7A CN202010056149A CN111205089B CN 111205089 B CN111205089 B CN 111205089B CN 202010056149 A CN202010056149 A CN 202010056149A CN 111205089 B CN111205089 B CN 111205089B
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zirconia
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CN111205089A (en
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袁爱灵
胡礼军
刘志
方东阳
毛翔鹏
刘琪
姜波
蔡玉珺
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Jiangxi Saici Materials Co ltd
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Abstract

The invention discloses a high-wave-transmittance green zirconia ceramic, which comprises yttrium-stabilized zirconia and a green colorant as raw materials; 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, nickel oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide according to the molar ratio of 16-60: 1.5-10: 0.8-25: 0.2-17: 0.05-10: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2.0-7.0 wt% of the yttrium-stabilized zirconia; the ceramic is of a sandwich gradient composite structure, the upper layer and the lower layer are compact layers, and the middle layer is a porous layer. In addition, the preparation method of the high-wave-transparent green zirconia ceramic and the prepared product are also disclosed. The raw materials adopted by the invention are green and environment-friendly, the sources are rich and easy to obtain, and the high-wave-transparent green zirconia ceramic formed by optimizing the formula composition and the structural design of the raw materials has excellent dielectric properties and excellent color generation, and can well meet the market requirements and the harsh use requirements in practical application.

Description

High-wave-transmittance green zirconia ceramic, preparation method thereof and prepared product
Technical Field
The invention relates to the technical field of ceramic materials, in particular to high-wave-transmittance green zirconia ceramic for consumer electronics products, a preparation method thereof and a prepared product.
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, kitchen ware materials, molds, solid fuel cells, oxygen sensors and the like.
In recent years, zirconia has been used in consumer products, such as bracelets, watch chains, necklaces, smartwatches, smartphones, etc., due to its excellent properties, good biocompatibility, no stimulation to the human body, etc. Due to the strict requirements of manufacturing and inspection of consumer electronics (such as smart watches, smart phones and the like), higher requirements are put on the performance aspect and the processing aspect of zirconia ceramics. In addition, as the standard of living of people is continuously improved, the aesthetic demands of consumers on the product devices are also synchronously improved. However, most of the existing consumer electronic products use black and white zirconia ceramics, and the existing consumer electronic products lack more beautiful color products and cannot better follow the market trend. In addition, due to the application and popularization of 5G communication technology and wireless charging technology, the dielectric performance of the housing is also more and more required by the consumer electronics. However, no appearance structural part product with extremely excellent dielectric property appears at present, and the market demand is difficult to meet.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-wave-transmittance green zirconia ceramic, and the green zirconia ceramic with high strength, good toughness, good color development, high glossiness and excellent dielectric property is obtained by optimizing the formula composition and the structural characteristics. The invention also aims to provide a preparation method of the high-wave-transparent green zirconia ceramic and a product prepared by the method.
The purpose of the invention is realized by the following technical scheme:
the invention provides a high-wave-transmission green zirconia ceramic, which comprises yttrium-stabilized zirconia and a green colorant as raw materials; 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, nickel oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide according to the molar ratio of 16-60: 1.5-10: 0.8-25: 0.2-17: 0.05-10: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2.0-7.0 wt% of yttrium-stabilized zirconia; the ceramic is of a sandwich gradient composite structure, the upper layer and the lower layer are compact layers, and the middle layer is a porous layer.
Preferably, the green toner comprises the components of 20-50: 2-8: 1-20: 0.5-14: 0.5-5: 0.05-3: 0.05-0.3 according to the molar ratio of aluminum oxide, zinc oxide, nickel oxide, iron oxide, titanium oxide, cobalt oxide and manganese oxide; the addition amount of the green colorant is 2.5-6.5 wt% of yttrium-stabilized zirconia.
Furthermore, the porosity of the porous layer is 2-8.5%, and the thickness of the porous layer accounts for 20-40% of the total thickness of the ceramic; the thicknesses of the upper layer and the lower layer respectively account for 30-40% of the total thickness of the ceramic.
The other purpose of the invention is realized by the following technical scheme
The preparation method of the high-wave-transmission green zirconia ceramic provided by the invention comprises the following steps:
(1) preparation of ceramic powder
Preparing and uniformly mixing the raw materials according to the composition, and performing ball milling, drying and crushing to obtain ceramic powder;
(2) preparation of the dense layer
Adding the ceramic powder into water, adding an additive at the same time to prepare compact layer water-based tape casting slurry with the solid content of 50-70 wt%, and then performing tape casting to obtain a compact layer monomer;
(3) preparation of porous layer
Adding the ceramic powder into water, adding an additive and a pore-forming agent simultaneously to prepare porous layer water-based tape casting slurry with the solid content of 47-65 wt%, and then carrying out tape casting to obtain a porous layer monomer;
(4) preparation of the Green bodies-lamination
Laminating and laminating the compact layer monomer and the porous layer monomer according to the sequence of the compact layer, the porous layer and the compact layer to obtain a ceramic green body with a sandwich structure;
(5) sintering of ceramics
And sintering the ceramic green body to obtain the high-wave-transmission green zirconia ceramic.
In the scheme, the additive prepared by the preparation method disclosed by the invention consists of a dispersing agent, a binder and a plasticizer, and the dosage of the additive is respectively 0.25-0.75 wt%, 2.0-7.5 wt% and 2.5-9.0 wt% of the ceramic powder; the dispersing agent is sodium polyacrylate and/or ammonium citrate; the binder is one or the combination of polyacrylic acid (PAA), polyvinyl alcohol (PVA), Methyl Cellulose (MC) and hydroxyethyl cellulose (HEC); the plasticizer is one or the combination of polyethylene glycol (PEG), glycerol and dimethyl phthalate. The pore-forming agent is polymethyl methacrylate (PMMA), carbon black or starch, and the usage amount of the pore-forming agent is 2-8.5 wt% of the ceramic powder.
Further, the pressing in the step (4) of the preparation method is carried out at the temperature of 80-90 ℃ and the pressure of 90-110 MPa. And (3) the sintering temperature in the step (5) is 1350-1450 ℃.
The product prepared by the preparation method of the high-wave-transmittance green zirconia ceramic has the dielectric constant of 5-20 and the color value of a being-20 or less*≤-8、-10≤b*≤10、10≤L*Less than or equal to 50. Preferably, the dielectric constant of the product is 6-18, and the color value is-18 ≤ a*≤-12、-9≤b*≤9、15≤L*≤40。
The invention has the following beneficial effects:
(1) according to the invention, through optimizing the raw material formula composition and structural design, the formed high-wave-transparent green zirconia ceramic has excellent dielectric property and excellent color generation, and can well meet the market demand.
(2) The raw materials adopted by the invention are green and environment-friendly, the sources are rich and easy to obtain, and the obtained product has high breaking strength (more than or equal to 800MPa), good toughness, good color development, high glossiness, few defects and excellent dielectric property, and can meet the harsh use requirements in practical application.
The present invention will be described in further detail with reference to examples.
Detailed Description
The embodiment of the invention provides a high-wave-transmittance green zirconia ceramic, which comprises yttrium-stabilized zirconia and a green colorant as raw materials; wherein 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, nickel oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide according to the molar ratio of 20-50: 2-8: 1-20: 0.5-14: 0.5-5: 0.05-3: 0.05-0.3; the addition amount of the green colorant is 2.5-6.5 wt% of the yttrium-stabilized zirconia; the ceramic is of a sandwich gradient composite structure, the upper layer and the lower layer are compact layers, and the thicknesses of the compact layers respectively account for 30-40% of the total thickness of the ceramic; the middle layer is a porous layer with the porosity of 2-8.5% and the thickness of 20-40% of the total thickness of the ceramic. The raw material composition and structural data of each example are shown in table 1.
TABLE 1 raw material composition and structural data of high wave-transparent green zirconia ceramics of the examples of the present invention
Figure BDA0002372904150000031
The proportion of green toner is mole proportion
The addition amount of green colorant to yttrium-stabilized zirconia
The preparation method of the high-wave-transmittance green zirconia ceramic provided by the embodiment of the invention comprises the following steps:
(1) preparation of ceramic powder
The preparation method comprises the following steps of (1) mixing the raw materials according to the composition shown in the table 1, uniformly mixing, and carrying out ball milling, drying and crushing to obtain ceramic powder;
(2) preparation of dense layer monomer
Adding the ceramic powder into pure water, adding an additive at the same time, preparing compact layer water system casting slurry with the solid content of 50-70 wt%, and then performing casting to obtain a compact layer monomer;
(3) preparation of porous layer monomer
Adding the ceramic powder into pure water, adding an additive and a pore-forming agent simultaneously to prepare porous layer water system tape-casting slurry with the solid content of 47-65 wt%, and then carrying out tape-casting to obtain a porous layer monomer;
wherein the additives used in the step (2) and the step (3) are the same, and consist of a dispersant, a binder and a plasticizer, and the use amounts of the additives are respectively 0.25-0.75 wt%, 2.0-7.5 wt% and 2.5-9.0 wt% of the ceramic powder; the dispersant is sodium polyacrylate and/or ammonium citrate; the binder is one or the combination of polyacrylic acid (PAA), polyvinyl alcohol (PVA), Methyl Cellulose (MC) and hydroxyethyl cellulose (HEC); the plasticizer is one or the combination of polyethylene glycol (PEG), glycerol and dimethyl phthalate;
the pore-forming agent is polymethyl methacrylate (PMMA), carbon black or starch, and the dosage of the pore-forming agent is 2-8.5 wt% of the ceramic powder;
(4) preparation of the Green bodies-lamination
Laminating the compact layer monomer and the porous layer monomer according to the sequence of the compact layer, the porous layer and the compact layer, and carrying out warm isostatic pressing at the temperature of 80-90 ℃ and the pressure of 90-110 MPa to obtain a ceramic green body with a sandwich structure;
(5) sintering of ceramics
And sintering the ceramic green body at the temperature of 1350-1450 ℃, and preserving heat for 2 hours to obtain the high-wave-transmission green zirconia ceramic.
The process parameters of the preparation method of each example are shown in table 2.
Table 2 technological parameters of the preparation method of high wave-transparent green zirconia ceramic of the embodiment of the present invention
Figure BDA0002372904150000041
Figure BDA0002372904150000051
The performance indexes of the high-wave-transmittance green zirconia ceramics prepared by the embodiment of the invention are shown in Table 3; further machining, polishing and other steps are carried out to obtain the finished product of the shell of the consumer electronic product and other products.
TABLE 3 Performance index of high wave-transparent green zirconia ceramics prepared by the examples of the present invention
Figure BDA0002372904150000052

Claims (4)

1. A preparation method of high-wave-transparent green zirconia ceramic is characterized by comprising the following steps: the raw materials of the ceramic comprise 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, nickel oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide according to the molar ratio of 16-60: 1.5-10: 0.8-25: 0.2-17: 0.05-10: 0.04-4: 0.04-0.4; the addition amount of the green colorant is 2.0-7.0 wt% of yttrium-stabilized zirconia; the preparation method comprises the following steps:
(1) preparation of ceramic powder
The raw materials are proportioned and uniformly mixed, and are subjected to ball milling, drying and crushing to obtain ceramic powder;
(2) preparation of the dense layer
Adding the ceramic powder into water, adding an additive at the same time to prepare dense layer casting slurry with solid content of 50-70 wt%, and then carrying out casting to obtain a dense layer monomer;
(3) preparation of porous layer
Adding the ceramic powder into water, adding an additive and a pore-forming agent simultaneously to prepare porous layer water-based tape casting slurry with the solid content of 47-65 wt%, and then carrying out tape casting to obtain a porous layer monomer;
the additive in the step (2) and the step (3) is composed of a dispersing agent, a binder and a plasticizer, the dosage of the additive is 0.25-0.75 wt%, 2.0-7.5 wt% and 2.5-9.0 wt% of the ceramic powder respectively, wherein the dispersing agent is sodium polyacrylate and/or ammonium citrate, the binder is one or a combination of polyacrylic acid, polyvinyl alcohol, methyl cellulose and hydroxyethyl cellulose, and the plasticizer is one or a combination of polyethylene glycol, glycerol and dimethyl phthalate; the pore-forming agent in the step (3) is polymethyl methacrylate, carbon black or starch, and the dosage of the pore-forming agent is 2-8.5 wt% of the ceramic powder;
(4) preparation of green bodies-lamination
Laminating and laminating the compact layer monomer and the porous layer monomer according to the sequence of the compact layer, the porous layer and the compact layer, wherein the laminating temperature is 80-90 ℃, and the pressure is 90-110 MPa, so as to obtain a ceramic green body with a sandwich structure;
(5) sintering of ceramics
Sintering the ceramic green body at the temperature of 1350-1450 ℃ to obtain the high-wave-transmission green zirconia ceramic with the porosity of 2-8.5% and the thickness of 20-40% of the total thickness of the ceramic, wherein the thicknesses of the upper layer and the lower layer respectively account for 30-40% of the total thickness of the ceramic, the dielectric constant of the high-wave-transmission green zirconia ceramic is 5-20, and the color value a is-20 or more*≤-8、-10≤b*≤10、10≤L*≤50。
2. The method for preparing the high-wave-transparent green zirconia ceramic according to claim 1, wherein the method comprises the following steps: the green toner comprises the components of aluminum oxide, zinc oxide, nickel oxide, ferric oxide, titanium oxide, cobalt oxide and manganese oxide according to the molar ratio of 20-50: 2-8: 1-20: 0.5-14: 0.5-5: 0.05-3: 0.05-0.3; the addition amount of the green colorant is 2.5-6.5 wt% of yttrium-stabilized zirconia.
3. The method for preparing the high-wave-transparent green zirconia ceramic according to claim 1, wherein the method comprises the following steps: the high-wave-transmission green zirconia ceramic has a dielectric constant of 6-18 and a color value of-18 to a*≤-12、-9≤b*≤9、15≤L*≤40。
4. A product obtained by the method for producing a highly wave-transmitting green zirconia ceramic according to any one of claims 1 to 3.
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