CN105565841A - Shading ceramic and preparation method thereof - Google Patents

Shading ceramic and preparation method thereof Download PDF

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CN105565841A
CN105565841A CN201511033433.8A CN201511033433A CN105565841A CN 105565841 A CN105565841 A CN 105565841A CN 201511033433 A CN201511033433 A CN 201511033433A CN 105565841 A CN105565841 A CN 105565841A
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refraction
low
ceramic
shading
ceramic layer
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CN105565841B (en
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徐苏龙
彭伟
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Chaozhou Three Circle Group Co Ltd
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Abstract

The invention discloses a shading ceramic, especially a shading ceramic that can be applied to the field of fingerprint identification. The shading ceramic comprises ceramic layers with a low refractive index and ceramic layers with a high refractive index, wherein the ceramic layers with a low refractive index and ceramic layers with a high refractive index are laminated together alternatively. The disclosed shading ceramic is prepared by alternatively laminating ceramic layers with a low refractive index and ceramic layers with a high refractive. Because the difference of refractive indexes of two neighbored ceramic layers is large, the amount of scattering is low, and thus the provided ceramic has an excellent shading effect. At the same time, the invention also discloses a preparation method of the shading ceramic. The operation of the method is simple and the method is easy to realize. The obtained shading ceramic has the advantages of good whiteness value, high light transmittance, good shading effect, and low cost.

Description

A kind of shading pottery and preparation method thereof
Technical field
The present invention relates to ceramic field, especially a kind of have shading performance, the pottery that can be used for fingerprint recognition field and preparation method thereof.
Background technology
The characteristic that stupalith has that intensity is large, hardness is high, wear-resisting and good corrosion resistance etc. is excellent, is widely used in every field, as cutter, watchcase, mould, phone housing and various ceramic structures etc.In recent years, what require ornament along with people improves constantly, pottery without features such as allergy, becomes the new lover of high-grade furnishing fields with the mechanical property of its excellence, metalluster and environmental friendliness, toxicological harmless, as the watchcase of high-grade wrist-watch, watch chain, phone housing and senior button etc.
But in the middle of thinner ceramic, general whiteware is once lower thickness, and the transmittance of pottery then increases, and have impact on whiteness and the obscurity of laminar ceramic product.The treatment process of usual shading pottery is the effect being reached white shading by the mode of screen printing ink black-out paint, but the sticking power of ink is limited, and poor reliability, easily comes off, and causes its resistance to environmental test capability poor.These factors limit the production of shading pottery and apply more widely.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art part and a kind of shading pottery with multilayered structure is provided; Meanwhile, present invention also offers the preparation method of described shading pottery.
For achieving the above object, the technical scheme that the present invention takes is: a kind of shading pottery, comprises low-refraction ceramic layer and the high index ceramic layer of alternative stacked.
The scattering power of light depends on the refringence of adjacent material, and refractive index difference is less, and scattered quantum is lower, easier printing opacity.Shading pottery described in the present invention, (specific refractory power of described low-refraction ceramic layer refers generally to be less than or equal to 1.8 to adopt low-refraction ceramic layer and high index ceramic layer alternative stacked to form respectively; The specific refractory power of described high index ceramic layer refers generally to be more than or equal to 2.0), the refractive index of adjacent two ceramic layers is comparatively large, and therefore scattered quantum is lower, and pottery of the present invention has excellent shaded effect.
As the preferred implementation of shading pottery of the present invention, described low-refraction ceramic layer comprises low-refraction frame material, and described low-refraction frame material is Al 2o 3, SiO 2, MgO, MgF 2in a kind of or at least two kinds of stupaliths be composited;
Described high index ceramic layer comprises high refractive index frame material, and described high refractive index frame material is TiO 2, ZrO 2, Y 2o 3, Si 3n 4, AlN, PZT, BaTiO 3and Ta 2o 5in a kind of or at least two kinds of stupaliths be composited.
As the preferred implementation of shading pottery of the present invention, the low-refraction frame material in described low-refraction ceramic layer is SiO 2; In described high index ceramic layer, high refractive index frame material is ZrO 2.When described low-refraction frame material and high refractive index frame material are aforesaid combination, the intensity of gained shading pottery is higher.
As the preferred implementation of shading pottery of the present invention, the low-refraction frame material in described low-refraction ceramic layer is SiO 2; In described high index ceramic layer, high refractive index frame material is Si 3n 4.When described low-refraction frame material and high refractive index frame material are aforesaid combination, the intensity of gained shading pottery is higher.
As the preferred implementation of shading pottery of the present invention, the low-refraction frame material in described low-refraction ceramic layer is MgO; In described high index ceramic layer, high refractive index frame material is Si 3n 4.When described low-refraction frame material and high refractive index frame material are aforesaid combination, the intensity of gained shading pottery is higher.
As the preferred implementation of shading pottery of the present invention, the low-refraction frame material in described low-refraction ceramic layer is MgF 2; In described high index ceramic layer, high refractive index frame material is ZrO 2.When described low-refraction frame material and high refractive index frame material are aforesaid combination, the intensity of gained shading pottery is higher.As the preferred implementation of shading pottery of the present invention, described low-refraction ceramic layer and high index ceramic layer all also comprise binding agent, softening agent, dispersion agent and organic solvent;
Described binding agent is at least one in polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, acrylic resin, methylcellulose gum, ethyl cellulose, nitrocotton ester, urethane resin and resol; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, TXA-15, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent is at least one in ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether.When described low-refraction ceramic layer and high index ceramic layer also comprise binding agent, softening agent, dispersion agent and organic solvent, the preparation simple operations more of described low-refraction ceramic layer and high index ceramic layer, and preparation-obtained low-refraction ceramic layer and high index ceramic layer performance more excellent.Between described low-refraction ceramic layer and high index ceramic layer, the selection of binding agent, softening agent, dispersion agent and organic solvent is independent separately, can choose same or different materials.
As the preferred implementation of shading pottery of the present invention, in described low-refraction ceramic layer, low-refraction frame material is low-refraction frame material is SiO 2, MgO, MgF 2in a kind of or at least two kinds of stupaliths be composited described in binding agent be polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, methylcellulose gum, at least one; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent be ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, at least one;
In described high index ceramic layer, high refractive index frame material is ZrO 2, Si 3n 4in one or both stupaliths be composited; Described binding agent be polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, methylcellulose gum, at least one; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent be ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, at least one.As the preferred implementation of shading pottery of the present invention, in described low-refraction ceramic layer, the mass percentage of each composition is respectively: low-refraction frame material 60 ~ 85%, binding agent 2 ~ 20%, softening agent 1 ~ 5%, dispersion agent 1 ~ 5%, organic solvent 10 ~ 30%; In described high index ceramic layer, the mass percentage of each composition is respectively: high refractive index frame material 60 ~ 85%, binding agent 2 ~ 20%, softening agent 1 ~ 5%, dispersion agent 1 ~ 5%, organic solvent 10 ~ 30%.
As the preferred implementation of shading pottery of the present invention, in described low-refraction ceramic layer, the mass percentage of each composition is respectively: low-refraction frame material 65 ~ 75%, binding agent 5 ~ 12%, softening agent 3 ~ 4%, dispersion agent 3 ~ 4%, organic solvent 16 ~ 20%; In described high index ceramic layer, the mass percentage of each composition is respectively: high refractive index frame material 65 ~ 75%, binding agent 6 ~ 14%, softening agent 3 ~ 4%, dispersion agent 3 ~ 4%, organic solvent 15 ~ 25%.
As the preferred implementation of shading pottery of the present invention, the thickness of described low-refraction ceramic layer is 1 ~ 3000 μm; The thickness of described high index ceramic layer is 1 ~ 3000 μm.The thickness of described low-refraction ceramic layer and high index ceramic layer is independent separately, in described shading pottery, the thickness of low-refraction ceramic layer and high index ceramic layer can be identical or different, and in described shading pottery, the thickness between multilayer low-refraction ceramic layer or multilayer high index ceramic layer also can be identical or different.
As the preferred implementation of shading pottery of the present invention, the shape of described low-refraction ceramic layer is trilateral, ellipse, circle, track type or Polygons; The shape of described high index ceramic layer is trilateral, ellipse, circle, track type or Polygons.The shape of described low-refraction ceramic layer and high index ceramic layer is independent separately, can be identical or different.
As the preferred implementation of shading pottery of the present invention, in described shading pottery, the number of plies sum of low-refraction ceramic layer and high index ceramic layer is more than or equal to 2, surface roughness value Ra≤0.1 μm of described shading pottery.
In shading pottery of the present invention, adopt multilayer low-refraction ceramic layer and high index ceramic layer to tell somebody what one's real intentions are to be formed by stacking, in described shading pottery, specific refractory power between multilayer low-refraction ceramic layer can be identical or different, and the specific refractory power between multilayer high index ceramic layer also can be identical or different.
Another object of the present invention is to the preparation method providing a kind of shading pottery described above, for realizing this object, the technical scheme that the present invention takes is: a kind of preparation method of shading pottery described above, comprises the following steps:
(1) slurry is prepared: add in ball grinder by the material contained by low-refraction ceramic layer and high index ceramic layer respectively, take out after ball milling, obtain low-refraction ceramic size and high index ceramic slurry respectively;
(2) powder compacting: the low-refraction ceramic size obtained step (1) respectively and high index ceramic slurry powder compacting, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively;
(3) lamination precompressed: the low-refraction biscuit of ceramics obtain step (2) and the precompressed of high index ceramic biscuit alternative stacked, obtain multilayer ceramic biscuit;
(4) porcelain body sintering: by the multilayer ceramic biscuit high temperature sintering in step (3), obtain multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out polishing, obtains shading pottery;
In described step (1), the Ball-milling Time in ball grinder of material contained by low-refraction ceramic layer is 24 ~ 48h, and the Ball-milling Time in ball grinder of material contained by high index ceramic layer is 24 ~ 48h;
In described step (2), low-refraction ceramic size and high index ceramic slurry powder compacting mode are flow casting molding, at least one of rolling in film, dry-pressing;
In described step (4), sintering processing is at least one in gas-protecting sintering, gas pressure sintering, HIP sintering, hot pressed sintering, plasma sintering, and sintering temperature is 1000 ~ 1700 DEG C, and soaking time is 0.5 ~ 10h;
In described step (5), polishing mode is at least one in mechanical polishing, chemical rightenning, electropolishing.
The preparation method of shading pottery of the present invention, first the material of low-refraction ceramic layer and high index ceramic layer is joined container for stirring even, make low-refraction ceramic size and high index ceramic slurry respectively, then respectively moulding process is carried out to low-refraction ceramic size and high index ceramic slurry, thus obtain low-refraction biscuit of ceramics and high index ceramic biscuit, and by low-refraction biscuit of ceramics and high index ceramic biscuit alternative stacked, carry out precompressed, sintering, then polishing is made.Described low-refraction ceramic size and high index ceramic slurry can adopt multiple different material proportion respectively, thus can obtain the ceramic layer of multiple different refractivity.
Shading pottery of the present invention, the ceramic layer with different refractivity is alternately formed by stacking, add the refringence of adjacent two layers ceramic layer in shading pottery, thus effectively improve the scattered quantum of shading pottery, there is excellent shaded effect, can be used as fingerprint recognition module cover plate and wearable device use.The preparation method of shading pottery of the present invention, simple to operate, be easy to realize, shading that the method prepares pottery, not only ceramic whiteness value is good, transmittance is high, but also has good shading effect and the low advantage of cost.
Embodiment
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the SiO of the material by contained by low-refraction ceramic layer: 60wt.% 2, the polyvinyl alcohol of 4wt.%, DOP, 4wt.% of 2wt.% the ethanol of TXA-15 and 30wt.% add in ball grinder, take out after ball milling 36h, obtain low-refraction ceramic size; The ZrO of the material by contained by high index ceramic layer: 60wt.% 2, the polyvinyl butyral of 6wt.%, the dibutyl ester of 2wt.%, TXA-15 and 30wt.% of 2wt.% ethanol add in ball grinder, take out after ball milling 8h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry flow casting molding, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 300 μm, and shape is trilateral; The thickness of high index ceramic biscuit is 200 μm, and shape is trilateral;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 2 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out gas-protecting sintering, and sintering temperature is 1500 DEG C, and soaking time is 0.5h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out mechanical polishing, makes its surfaceness reach Ra=0.05 μm, obtains ganoid ZrO 2-SiO 2pottery, obtains shading pottery.
Embodiment 2
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the Al of the material by contained by low-refraction ceramic layer: 80wt.% 2o 3, the polyvinyl butyral of 2wt.% and the mixture (mass ratio of polyvinyl butyral and polyvinyl chloride is 1:1) of polyvinyl chloride, the acetone of the dibutyl ester of 1wt.%, PMMA and 12wt.% of 5wt.% adds in ball grinder, take out after ball milling 32h, obtain low-refraction ceramic size; The TiO of the material by contained by high index ceramic layer: 85wt.% 2, the polyvinyl chloride of 2wt.%, the Yelkin TTS of DOP, 1wt.% of 2wt.% and the acetone of 10wt.% adds in ball grinder, take out after ball milling 48h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry rolling formation, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 300 μm, and shape is oval; The thickness of high index ceramic biscuit is 400 μm, and shape is oval;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 4 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out gas pressure sintering, and sintering temperature is 1700 DEG C, and soaking time is 2h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out chemical rightenning, makes its surfaceness reach Ra=0.05 μm, obtains ganoid TiO 2-Al 2o 3pottery, obtains shading pottery.
Embodiment 3
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the acrylic resin of MgO, 3wt.% of the material by contained by low-refraction ceramic layer: 85wt.%, the dibutyl ester of 1wt.%, the Yelkin TTS of 1wt.% and the diethylene glycol monobutyl ether of 10wt.% add in ball grinder, take out after ball milling 48h, obtain low-refraction ceramic size; The Si of the material by contained by high index ceramic layer: 60wt.% 3n 4, the polyvinyl alcohol of 20wt.%, PEG, 5wt.% of 3wt.% the toluene of PMMA and 12wt.% add in ball grinder, take out after ball milling 2h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry dry-pressing formed, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 100 μm, and shape is circular; The thickness of high index ceramic biscuit is 100 μm, and shape is circular;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 6 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out HIP sintering, and sintering temperature is 1600 DEG C, and soaking time is 4h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out electropolishing, makes its surfaceness reach Ra=0.08 μm, obtains ganoid Si 3n 4-MgO pottery, obtains shading pottery.
Embodiment 4
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the MgF of the material by contained by low-refraction ceramic layer: 75wt.% 2, the resol of 10wt.%, the mixture (mass ratio of PEG and DOP is 1:3) of PEG and DOP of 3wt.%, the fish oil of 2wt.% and the mixture (mass ratio of fish oil and Yelkin TTS is 2:1) of Yelkin TTS, the ethylene glycol monobutyl ether of 10wt.% add in ball grinder, take out after ball milling 2h, obtain low-refraction ceramic size; The ZrO of the material by contained by high index ceramic layer: 70wt.% 2, the acrylic resin of 10wt.%, the dibutyl ester of 5wt.%, the Sodium hexametaphosphate 99 of 5wt.% and the dimethylbenzene of 10wt.% and the mixture (mass ratio of dimethylbenzene and acetone is 1:1) of acetone add in ball grinder, take out after ball milling 10h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry flow casting molding, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 3000 μm, and shape is track type; The thickness of high index ceramic biscuit is 3000 μm, and shape is track type;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 2 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out hot pressed sintering, and sintering temperature is 1580 DEG C, and soaking time is 5h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out mechanical polishing, makes its surfaceness reach Ra=0.1 μm, obtains ganoid ZrO 2-MgF 2pottery, obtains shading pottery.
Embodiment 5
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: MgO and Al of the material by contained by low-refraction ceramic layer: 65wt.% 2o 3mixture (MgO and Al 2o 3mass ratio be 3:1), the mixture (mass ratio of butylacetate and ethanol is 4:1) of the urethane resin of 20wt.%, the Sodium hexametaphosphate 99 of PEG, 3wt.% of 2wt.% and the butylacetate of 10wt.% and ethanol adds in ball grinder, take out after ball milling 25h, obtain low-refraction ceramic size; The fish oil of DOP, 3wt.% and the Virahol of 19wt.% of the methylcellulose gum of AlN, 2wt.% of the material by contained by high index ceramic layer: 75wt.% and the mixture (mass ratio of methylcellulose gum and ethyl cellulose is 2:1) of ethyl cellulose, 1wt.% add in ball grinder, take out after ball milling 15h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry rolling formation, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 1 μm, and shape is hexagon; The thickness of high index ceramic biscuit is 1 μm, and shape is hexagon;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 4 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out plasma agglomeration, and sintering temperature is 1550 DEG C, and soaking time is 1h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out chemical rightenning, makes its surfaceness reach Ra=0.06 μm, obtains ganoid AlN-Al 2o 3pottery, obtains shading pottery.
Embodiment 6
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the SiO of the material by contained by low-refraction ceramic layer: 70wt.% 2, the nitrocotton ester of 4wt.%, DOP, 1wt.% of 5wt.% the ethylene glycol monoethyl ether of TXA-15 and 20wt.% add in ball grinder, take out after ball milling 15h, obtain low-refraction ceramic size; The Terpineol 350 of the mixture (mass ratio of PEG and dioctyl ester is 6:1) of the ethyl cellulose of PZT, 2wt.% of the material by contained by high index ceramic layer: 65wt.%, the PEG of 4wt.% and dioctyl ester, PMMA and 25wt.% of 4wt.% adds in ball grinder, take out after ball milling 25h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry dry-pressing formed, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 600 μm, and shape is pentagon; The thickness of high index ceramic biscuit is 500 μm, and shape is pentagon;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 2 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out gas-protecting sintering, and sintering temperature is 1000 DEG C, and soaking time is 0.5h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out electropolishing, makes its surfaceness reach Ra=0.04 μm, obtains ganoid PZT-SiO 2pottery, obtains shading pottery.
Embodiment 7
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the ethyl cellulose of MgO, 10wt.% of the material by contained by low-refraction ceramic layer: 66wt.%, the fish oil of PEG, 4wt.% of 4wt.% and the Terpineol 350 of 16wt.% add in ball grinder, take out after ball milling 30h, obtain low-refraction ceramic size; The BaTiO of the material by contained by high index ceramic layer: 78wt.% 3and ZrO 2mixture (BaTiO 3and ZrO 2mass ratio be 1:2), the ethyl acetate of the nitrocotton ester of 3wt.%, the dibutyl ester of 3wt.%, the Yelkin TTS of 1wt.% and 15wt.% adds in ball grinder, take out after ball milling 18h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry flow casting molding, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 1200 μm, and shape is trilateral; The thickness of high index ceramic biscuit is 1000 μm, and shape is trilateral;
(3) lamination precompressed: the low-refraction biscuit of ceramics obtain step (2) and high index ceramic biscuit are according to the sequence alternate lamination 3 layers of low-refraction biscuit of ceramics-high index ceramic biscuit-low-refraction biscuit of ceramics, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out gas pressure sintering, and sintering temperature is 1700 DEG C, and soaking time is 0.6h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out mechanical polishing, makes its surfaceness reach Ra=0.09 μm, obtains ganoid BaTiO 3-MgO pottery, obtains shading pottery.
Embodiment 8
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the SiO of the material by contained by low-refraction ceramic layer: 73wt.% 2and MgF 2mixture (SiO 2and MgF 2mass ratio be 1:1), the Virahol of the polyvinyl chloride of 12wt.%, the dibutyl ester of 1wt.%, PMMA and 12wt.% of 2wt.% adds in ball grinder, take out after ball milling 22h, obtain low-refraction ceramic size; The TiO of the material by contained by high index ceramic layer: 72wt.% 2, the urethane resin of 6wt.%, DOP, 2wt.% of 3wt.% the butylacetate of TXA-15 and 17wt.% add in ball grinder, take out after ball milling 27h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry rolling formation, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 800 μm, and shape is circular; The thickness of high index ceramic biscuit is 800 μm, and shape is circular;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 2 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out HIP sintering, and sintering temperature is 1560 DEG C, and soaking time is 8h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out chemical rightenning, makes its surfaceness reach Ra=0.05 μm, obtains ganoid TiO 2-MgF 2pottery, obtains shading pottery.
Embodiment 9
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the Al of the material by contained by low-refraction ceramic layer one: 70wt.% 2o 3, the methylcellulose gum of 5wt.%, the Yelkin TTS of DOP, 5wt.% of 1wt.% and the dimethylbenzene of 19wt.% adds in ball grinder, take out after ball milling 39h, obtain low-refraction ceramic size one; The MgF of the material by contained by low-refraction ceramic layer two: 53wt.% 2, the mixture (mass ratio of PEG and dioctyl ester is 2:1) of the resol of 18wt.% and the mixture (mass ratio of resol and urethane resin is 1:1) of urethane resin, the PEG of 1wt.% and dioctyl ester, the Sodium hexametaphosphate 99 of 3wt.% and the ethanol of 25wt.% adds in ball grinder, take out after ball milling 39h, obtain low-refraction ceramic size two; The Ta of the material by contained by high index ceramic layer: 69wt.% 2o 5and TiO 2mixture (Ta 2o 5and TiO 2mass ratio be 4:1), the Sodium hexametaphosphate 99 of the resol of 14wt.%, PEG, 5wt.% of 1wt.% and the mixture (mass ratio of Sodium hexametaphosphate 99 and PMMA is 8:1) of PMMA, the ethylene glycol monoethyl ether of 11wt.% add in ball grinder, take out after ball milling 21h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size one, low-refraction ceramic size two and the high index ceramic slurry that obtain step (1) are respectively dry-pressing formed, obtain low-refraction biscuit of ceramics one, index ceramic biscuit two and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics one is 300 μm, and shape is oval; The thickness of low-refraction biscuit of ceramics two is 350 μm, and shape is oval; The thickness of high index ceramic biscuit is 300 μm, and shape is oval;
(3) lamination precompressed: the low-refraction biscuit of ceramics one, low-refraction biscuit of ceramics two and the high index ceramic biscuit that step (2) are obtained are according to the sequence alternate lamination 5 layers of high index ceramic biscuit-low-refraction biscuit of ceramics one-high index ceramic biscuit-low-refraction biscuit of ceramics two-high index ceramic biscuit, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out hot pressed sintering, and sintering temperature is 1690 DEG C, and soaking time is 6h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out electropolishing, makes its surfaceness reach Ra=0.06 μm, obtains smooth surface pottery, obtain shading pottery.
Embodiment 10
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the SiO of the material by contained by low-refraction ceramic layer: 71wt.% 2, the resol of 5wt.%, PEG, 4wt.% of 2wt.% the ethyl acetate of TXA-15 and 18wt.% add in ball grinder, take out after ball milling 28h, obtain low-refraction ceramic size; The Si of the material by contained by high index ceramic layer: 75wt.% 3n 4, the polyvinyl chloride of 6wt.%, the dibutyl ester of 3wt.%, the fish oil of 1wt.% and 15wt.% ethylene glycol monobutyl ether add in ball grinder, take out after ball milling 35h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry flow casting molding, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 650 μm, and shape is track type; The thickness of high index ceramic biscuit is 600 μm, and shape is track type;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 6 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out plasma sintering, and sintering temperature is 1580 DEG C, and soaking time is 2h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out mechanical polishing, makes its surfaceness reach Ra=0.1 μm, obtains ganoid Si 3n 4-SiO 2pottery, obtains shading pottery.
Embodiment 11
A kind of embodiment of shading pottery of the present invention, the present embodiment shading pottery adopts following methods to be prepared from:
(1) slurry is prepared: the polyvinyl chloride of MgO, 13wt.% of the material by contained by low-refraction ceramic layer: 68wt.%, the dibutyl ester of 3wt.%, the Sodium hexametaphosphate 99 of 4wt.% and the toluene of 12wt.% add in ball grinder, take out after ball milling 32h, obtain low-refraction ceramic size; The Y of the material by contained by high index ceramic layer: 71wt.% 2o 3, the acrylic resin of 10wt.%, DOP, 2wt.% of 1wt.% the diethylene glycol monobutyl ether of PMMA and 16wt.% add in ball grinder, take out after ball milling 26h, obtain high index ceramic slurry;
(2) powder compacting: the low-refraction ceramic size respectively step (1) obtained and high index ceramic slurry rolling formation, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively, the thickness of low-refraction biscuit of ceramics is 900 μm, and shape is trilateral; The thickness of high index ceramic biscuit is 900 μm, and shape is trilateral;
(3) lamination precompressed: the low-refraction biscuit of ceramics that step (2) is obtained and high index ceramic biscuit alternative stacked, folded 6 layers, precompressed, obtains multilayer ceramic biscuit;
(4) porcelain body sintering: the multilayer ceramic biscuit in step (3) is carried out gas-protecting sintering, and sintering temperature is 1590 DEG C, and soaking time is 10h, obtains multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out chemical rightenning, makes its surfaceness reach Ra=0.05 μm, obtains ganoid AlN-MgO pottery, obtains shading pottery.
Embodiment 12
Performance test is carried out to the multilayer shading pottery that embodiment of the present invention 1-11 prepares
The four point bending strength of the shading pottery for preparing of testing example 1-11, transmittance and whiteness are wherein respectively, the sample size of four point bending strength is length a=60mm, width b=10mm, height c=0.1mm, the sample size of transmittance and whiteness is diameter phi=10mm, and test result is as following table 1.
The performance test of table 1 multilayer shading of the present invention pottery
As can be seen from Table 1, the transmitance of the shading pottery that embodiment of the present invention 1-11 prepares maintains near 2.0%, and whiteness maintains near 92%, and four point bending strength is different according to used frame material.
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.

Claims (10)

1. a shading pottery, is characterized in that, described shading pottery comprises low-refraction ceramic layer and the high index ceramic layer of alternative stacked.
2. shading pottery as claimed in claim 1, it is characterized in that, described low-refraction ceramic layer comprises low-refraction frame material, and described low-refraction frame material is Al 2o 3, SiO 2, MgO, MgF 2in a kind of or at least two kinds of stupaliths be composited;
Described high index ceramic layer comprises high refractive index frame material, and described high refractive index frame material is TiO 2, ZrO 2, Y 2o 3, Si 3n 4, AlN, PZT, BaTiO 3and Ta 2o 5in a kind of or at least two kinds of stupaliths be composited.
3. shading pottery as claimed in claim 1, it is characterized in that, described low-refraction ceramic layer and high index ceramic layer all also comprise binding agent, softening agent, dispersion agent and organic solvent;
Described binding agent is at least one in polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, acrylic resin, methylcellulose gum, ethyl cellulose, nitrocotton ester, urethane resin and resol; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, TXA-15, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent is at least one in ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether.
4. shading pottery as claimed in claim 3, it is characterized in that, in described low-refraction ceramic layer, low-refraction frame material is SiO 2, MgO, MgF 2in a kind of or at least two kinds of stupaliths be composited; Described binding agent be polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, methylcellulose gum, at least one; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent be ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, at least one;
In described high index ceramic layer, high refractive index frame material is ZrO 2, Si 3n 4in one or both stupaliths be composited; Described binding agent be polyvinyl chloride, polyvinyl alcohol, polyvinyl butyral, methylcellulose gum, at least one; Described softening agent is at least one in DOP, dioctyl ester and PEG; Described dispersion agent is at least one in Yelkin TTS, PMMA, Sodium hexametaphosphate 99 and fish oil; Organic solvent be ethanol, acetone, toluene, dimethylbenzene, Virahol, Terpineol 350, ethyl acetate, butylacetate, at least one.
5. the shading pottery as described in Claims 2 or 3 or 4, it is characterized in that, in described low-refraction ceramic layer, the mass percentage of each composition is respectively: low-refraction frame material 60 ~ 85%, binding agent 2 ~ 20%, softening agent 1 ~ 5%, dispersion agent 1 ~ 5%, organic solvent 10 ~ 30%; In described high index ceramic layer, the mass percentage of each composition is respectively: high refractive index frame material 60 ~ 85%, binding agent 2 ~ 20%, softening agent 1 ~ 5%, dispersion agent 1 ~ 5%, organic solvent 10 ~ 30%.
6. shading pottery as claimed in claim 5, it is characterized in that, in described low-refraction ceramic layer, the mass percentage of each composition is respectively: low-refraction frame material 65 ~ 75%, binding agent 5 ~ 12%, softening agent 3 ~ 4%, dispersion agent 3 ~ 4%, organic solvent 16 ~ 20%; In described high index ceramic layer, the mass percentage of each composition is respectively: high refractive index frame material 65 ~ 75%, binding agent 6 ~ 14%, softening agent 3 ~ 4%, dispersion agent 3 ~ 4%, organic solvent 15 ~ 25%.
7. shading pottery as claimed in claim 1, it is characterized in that, the thickness of described low-refraction ceramic layer is 1 ~ 3000 μm; The thickness of described high index ceramic layer is 1 ~ 3000 μm.
8. the shading pottery as described in claim 1 or 7, it is characterized in that, the shape of described low-refraction ceramic layer is trilateral, ellipse, circle, track type or Polygons; The shape of described high index ceramic layer is trilateral, ellipse, circle, track type or Polygons.
9. shading pottery as claimed in claim 1, it is characterized in that, in described shading pottery, the number of plies sum of low-refraction ceramic layer and high index ceramic layer is more than or equal to 2, surface roughness value Ra≤0.1 μm of described shading pottery.
10. a preparation method for shading pottery as described in as arbitrary in claim 1 ~ 9, is characterized in that, comprise the following steps:
(1) slurry is prepared: add in ball grinder by the material contained by low-refraction ceramic layer and high index ceramic layer respectively, take out after ball milling, obtain low-refraction ceramic size and high index ceramic slurry respectively;
(2) powder compacting: the low-refraction ceramic size obtained step (1) respectively and high index ceramic slurry powder compacting, obtain low-refraction biscuit of ceramics and high index ceramic biscuit respectively;
(3) lamination precompressed: the low-refraction biscuit of ceramics obtain step (2) and the precompressed of high index ceramic biscuit alternative stacked, obtain multilayer ceramic biscuit;
(4) porcelain body sintering: by the multilayer ceramic biscuit high temperature sintering in step (3), obtain multilayer ceramic blank;
(5) polishing: the multilayer ceramic blank in step (4) is carried out polishing, obtains shading pottery;
In described step (1), the Ball-milling Time in ball grinder of material contained by low-refraction ceramic layer is 24 ~ 48h, and the Ball-milling Time in ball grinder of material contained by high index ceramic layer is 24 ~ 48h;
In described step (2), low-refraction ceramic size and high index ceramic slurry powder compacting mode are flow casting molding, at least one of rolling in film, dry-pressing;
In described step (4), sintering processing is at least one in gas-protecting sintering, gas pressure sintering, HIP sintering, hot pressed sintering, plasma sintering, and sintering temperature is 1000 ~ 1700 DEG C, and soaking time is 0.5 ~ 10h;
In described step (5), polishing mode is at least one in mechanical polishing, chemical rightenning, electropolishing.
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CN106116703A (en) * 2016-06-30 2016-11-16 潮州三环(集团)股份有限公司 A kind of shading pottery and preparation method thereof
CN106336245A (en) * 2016-08-24 2017-01-18 潮州三环(集团)股份有限公司 Light-shielding substrate preparation method
CN111747756A (en) * 2019-03-26 2020-10-09 北京中材人工晶体研究院有限公司 Nitride ceramic tape-casting slurry and nitride ceramic substrate prepared from same
CN112430118A (en) * 2020-12-04 2021-03-02 湖北三江航天江北机械工程有限公司 Magnesium fluoride infrared hood bonding process method

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CN102163526A (en) * 2010-02-18 2011-08-24 佳能株式会社 Black matrix, manufacturing method thereof, and image display apparatus using the same
CN104118994A (en) * 2013-04-23 2014-10-29 旭硝子株式会社 Glass substrate with reflective films on both sides, and process for its production
CN104844198A (en) * 2014-02-18 2015-08-19 清华大学 Hand-held terminal product appearance ceramic thin type member and production method thereof

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Publication number Priority date Publication date Assignee Title
CN106116703A (en) * 2016-06-30 2016-11-16 潮州三环(集团)股份有限公司 A kind of shading pottery and preparation method thereof
CN106336245A (en) * 2016-08-24 2017-01-18 潮州三环(集团)股份有限公司 Light-shielding substrate preparation method
CN106336245B (en) * 2016-08-24 2019-06-04 潮州三环(集团)股份有限公司 A kind of preparation method of light-shielding substrate
CN111747756A (en) * 2019-03-26 2020-10-09 北京中材人工晶体研究院有限公司 Nitride ceramic tape-casting slurry and nitride ceramic substrate prepared from same
CN112430118A (en) * 2020-12-04 2021-03-02 湖北三江航天江北机械工程有限公司 Magnesium fluoride infrared hood bonding process method
CN112430118B (en) * 2020-12-04 2022-05-10 湖北三江航天江北机械工程有限公司 Magnesium fluoride infrared hood bonding process method

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