CN105541326A - Preparation method of zirconia ceramic slice - Google Patents

Preparation method of zirconia ceramic slice Download PDF

Info

Publication number
CN105541326A
CN105541326A CN201510981527.1A CN201510981527A CN105541326A CN 105541326 A CN105541326 A CN 105541326A CN 201510981527 A CN201510981527 A CN 201510981527A CN 105541326 A CN105541326 A CN 105541326A
Authority
CN
China
Prior art keywords
oxide powder
zirconia ceramics
powder
solvent
tetragonal phase
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510981527.1A
Other languages
Chinese (zh)
Other versions
CN105541326B (en
Inventor
刘锋
陈兰桂
孙亮
王文利
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dongguan CSG Ceramics Technology Co Ltd
Original Assignee
Dongguan CSG Ceramics Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dongguan CSG Ceramics Technology Co Ltd filed Critical Dongguan CSG Ceramics Technology Co Ltd
Priority to CN201510981527.1A priority Critical patent/CN105541326B/en
Publication of CN105541326A publication Critical patent/CN105541326A/en
Application granted granted Critical
Publication of CN105541326B publication Critical patent/CN105541326B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63404Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/10Esters
    • C08F120/26Esters containing oxygen in addition to the carboxy oxygen
    • C08F120/28Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/46Polymerisation initiated by wave energy or particle radiation
    • C08F2/48Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227Lanthanum oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229Cerium oxides or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron

Abstract

A preparation method of a zirconia ceramic slice comprises the following steps: providing stable tetragonal phase zirconia powder, rare earth oxide powder, a solvent, a dispersant, an ultraviolet initiating agent, a photosensitive polymeric monomer and an assistant; mixing the tetragonal phase zirconia powder, the rare earth oxide powder and the solvent, performing ultrasonic dispersion agglomeration operation, and then performing evaporation to remove the solvent, thus obtaining mixed powder; mixing the mixed powder, the dispersant, the ultraviolet initiating agent, the photosensitive polymeric monomer and the assistant, and then performing ball-milling and bubble removing operation, thus obtaining zirconia ceramic slurry; adding the zirconia ceramic slurry into a ceramic casting machine, and then enabling a base plate of the ceramic casting machine loading the zirconia ceramic slurry to pass through an ultraviolet curing machine, thus forming a zirconia ceramic slice green body; sintering the zirconia ceramic slice green body, thus obtaining the zirconia ceramic slice. By adopting the preparation method, a conventional drying process can be avoided, and a prepared product is enabled to have better quality.

Description

Zirconia ceramics method for preparing slices
Technical field
The present invention relates to zirconia ceramics applied technical field, particularly relate to a kind of zirconia ceramics method for preparing slices.
Background technology
At present, zirconia ceramics is increasingly extensive in industrial civil area application, because zirconia ceramics can use under intensity and the high envrionment conditions of toughness reguirements, therefore, zirconia ceramics is often used in and manufactures the less sheet material of thin slice, substrate, liner or other thickness.
These sheet materials not only can use as structure unit, as being applied to the field such as artwork and mechanical part, but also be extensively incorporated in the electronic component of electronics microminiaturization, as, plate type oxygen sensor and circuit board substrate etc., and in super large-scale integration, therefore, these zirconia ceramics sheet materials have boundless application prospect.
But, existing zirconia ceramics sheet manufacturing process, as, isostatic pressing, compression molding, injection molding or gel casting forming need through this step of super-dry in the preparation, namely loft drier is used to carry out drying to carry out crystallization operation to zirconia ceramics green compact in advance, for follow-up sintering, but, because zirconia ceramics sheet material structurally has the characteristic that thickness is more frivolous, area is comparatively large, surface is more smooth, be easy in drying process, occur following problem:
1, the cracking phenomena that excessively causes because drying of green compact local or all surfaces, namely there is slight crack in surface;
2, there is excess shrinkage in dried green compact, cannot meet the demand of near net-shape;
3, the rear local structure of sintering loosely; And other various problems, after causing its sintering, quality does not reach industry requirement.When especially preparing ultra-thin zirconia ceramics sheet material, the defect of existing zirconia ceramics sheet manufacturing process is more outstanding.
Summary of the invention
Based on this, be necessary to provide a kind of and can exempt the zirconia ceramics method for preparing slices that drying process and the product for preparing more meet industry quality requirements.
A kind of zirconia ceramics method for preparing slices, comprises the steps:
Stable tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersion agent, ultraviolet initiator, photosensitive polymerization monomer and auxiliary agent are provided;
By described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, and carry out ultrasonicly breaing up reunion operation, then carry out evaporation operation described solvent is removed, obtain mixed powder;
After described mixed powder, described dispersion agent, described ultraviolet initiator, described photosensitive polymerization monomer and described auxiliary agent are mixed, carry out ball milling and de-bubble operation, obtain zirconia ceramics slurry;
Described zirconia ceramics slurry is added in ceramic casting machine, then will the substrate of the ceramic casting machine of described zirconia ceramics slurry be carried by after uv cure machine, the substrate of ceramic casting machine is formed zirconia ceramics thin slice green compact;
After being sintered by described zirconia ceramics thin slice green compact, obtain described zirconia ceramics thin slice.
Wherein in an embodiment, during by described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, every Preset Time carry out ultrasonic break up reunion operation.
Wherein in an embodiment, described Preset Time is 5 seconds ~ 10 seconds.
Wherein in an embodiment, described Preset Time is 7 seconds ~ 10 seconds.
Wherein in an embodiment, described Preset Time is 8 seconds.
Wherein in an embodiment, by the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, adopt magnetic agitation married operation.
Wherein in an embodiment, by in the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, specifically comprise the steps: in advance by after described RE oxide powder and described solvent, then add described tetragonal phase zirconium oxide powder.
The UV-light that adopts above-mentioned zirconia ceramics method for preparing slices causes cross-linking and curing reaction and realizes in-situ solidifying effect, thus traditional drying process can be exempted, thus because drying is excessive there is excess shrinkage in the cracking phenomena caused, dried green compact can to avoid the surface of green compact, demand and the rear local structure problem loosely of sintering of near net-shape cannot be met, and then can guarantee that the product quality prepared is better, reach industry requirement.
Accompanying drawing explanation
Fig. 1 is the schema of the zirconia ceramics method for preparing slices of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, the zirconia ceramics method for preparing slices of an embodiment comprises the steps:
S110: stable tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersion agent, ultraviolet initiator, photosensitive polymerization monomer and auxiliary agent are provided.
In one embodiment, the D50 (median particle diameter) of described stable tetragonal phase zirconium oxide powder is 0.5 μm ~ 2.5 μm, adopt the stable tetragonal phase zirconium oxide powder of above-mentioned median particle diameter can prepare dispersion evenly zirconia ceramic slurry, thus make the mechanical property of the zirconia ceramics thin slice prepared better, especially ultra-thin zirconia ceramics thin slice, as the zirconia ceramics thin slice that thickness is 0.1 ~ 0.8mm, its mechanical property is better, as toughness, anti-fracture performance and hardness better, and surface finish is also better.
In one embodiment, described RE oxide powder comprises yttrium oxide powder and other auxiliary RE oxide powder, such as, described stable tetragonal phase zirconium oxide powder, the mass ratio of described yttrium oxide powder and other auxiliary RE oxide powder described is (85 ~ 95): (2 ~ 15): (0.5 ~ 10), preferably, described stable tetragonal phase zirconium oxide powder, the mass ratio of described yttrium oxide powder and other auxiliary RE oxide powder described is 90:7:0.5, like this, by described RE oxide powder of adulterating at described stable tetragonal phase zirconium oxide powder, the mechanical property of described zirconia ceramics thin slice can be improved further, and, can also in follow-up sintering process, suppress growing up of crystal grain, thus it is tiny to obtain crystal grain, density is high, the described zirconia ceramics thin slice that electric property is good.
Further, other auxiliary RE oxide powder described comprise lanthanum oxide powder, cerium oxide powder, Praseodymium trioxide powder, Neodymium trioxide powder, promethium oxide powder, Samarium trioxide powder, europium oxide powder, gadolinium sesquioxide powder, terbium sesquioxide powder, dysprosium oxide powder, Holmium trioxide powder, Erbium trioxide powder, trioxide powder, ytterbium oxide powder, lutecium oxide powder, Scium trioxide powder, such as, lanthanum oxide powder, cerium oxide powder, Praseodymium trioxide powder, Neodymium trioxide powder, promethium oxide powder, Samarium trioxide powder, europium oxide powder, gadolinium sesquioxide powder, terbium sesquioxide powder, dysprosium oxide powder, Holmium trioxide powder, Erbium trioxide powder, trioxide powder, ytterbium oxide powder, lutecium oxide powder, the mass ratio of Scium trioxide powder is (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5), preferably, lanthanum oxide powder, cerium oxide powder, Praseodymium trioxide powder, Neodymium trioxide powder, promethium oxide powder, Samarium trioxide powder, europium oxide powder, gadolinium sesquioxide powder, terbium sesquioxide powder, dysprosium oxide powder, Holmium trioxide powder, Erbium trioxide powder, trioxide powder, ytterbium oxide powder, lutecium oxide powder, the mass ratio of Scium trioxide powder is 1.5:1:1.5:1:1:1.5:1.5:1:1.5:1:1:1.5:1.5:1:1.5:1, like this, is more conducive in follow-up sintering process, suppress growing up of crystal grain, thus it is tiny to obtain crystal grain, density is high, the described zirconia ceramics thin slice that electric property is good.
It should be noted that, described rare earth oxide refers to that period of element atom ordinal number is 15 kinds of lanthanide oxides of 57 to 71, and the oxide compound of the scandium similar to lanthanon chemical property (Sc) and yttrium (Y) totally 17 kinds of elements.Namely described rare earth oxide comprises lanthanum trioxide, cerium oxide, Praseodymium trioxide, Neodymium trioxide, promethium oxide, Samarium trioxide, europium sesquioxide, gadolinium sesquioxide, terbium sesquioxide, dysprosium oxide, Holmium trioxide, Erbium trioxide, trioxide, ytterbium oxide, lutecium oxide, Scium trioxide and yttrium oxide.
S120: by described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, then carry out evaporation operation described solvent is removed, obtain mixed powder.
In one embodiment, choose the solvent that boiling point is lower.Such as, described solvent comprises binary azeotropic mixed solvent, and described binary azeotropic mixed solvent comprises at least one in ethanol/methylethylketone binary azeotropic mixed solvent, ethanol/trieline binary azeotropic mixed solvent, trieline/methylethylketone binary azeotropic mixed solvent.Such as, described binary azeotropic mixed solvent is ethanol/methylethylketone binary azeotropic mixed solvent, and both mol ratios are 1:1.Adopt above-mentioned binary azeotropic mixed solvent in follow-up Light Curing, low, the easy evaporation removing of boiling point can be had, namely volatilize soon, time of drying is short, solvent load is few, without the need to drying process, to the better simply advantage of strong, the follow-up de-bubble of powder wettability.
In addition, the surface tension that described solvent adopts above-mentioned binary azeotropic mixed solvent can reduce with described tetragonal phase zirconium oxide powder and described RE oxide powder, thus the wettability to described tetragonal phase zirconium oxide powder and described RE oxide powder can be improved.
In one embodiment, the mass ratio of described stable tetragonal phase zirconium oxide powder and described RE oxide powder is (85 ~ 95): (2.5 ~ 25), and for example, described stable tetragonal phase zirconium oxide powder, the mass ratio of described RE oxide powder and described solvent is (85 ~ 95): (2.5 ~ 25): (15 ~ 20), preferably, described stable tetragonal phase zirconium oxide powder, the mass ratio of described RE oxide powder and described solvent is 90:15:20, like this, both can make described stable tetragonal phase zirconium oxide powder and described RE oxide powder mixedly more even, make the described mixed powder that obtains mixedly more even, and, adopt the described solvent of above-mentioned mass ratio, more be conducive to evaporation removing, obtain dry described mixed powder.
In one embodiment, by described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, and carry out ultrasonic break up reunion operation.Be appreciated that, described tetragonal phase zirconium oxide powder and described RE oxide powder are producing or/and when storing, reuniting effect can be produced, as, after making moist, the effect of its particle aggregation is more obvious, and by described ultrasonic reunion operation of breaing up, namely to described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent send ultrasonic wave, to break up the reunion macrobead of described tetragonal phase zirconium oxide powder and described RE oxide powder, more be conducive to mixing of described tetragonal phase zirconium oxide powder and described RE oxide powder, thus the follow-up described zirconia ceramics slurry obtained can be made mixedly more even, and then can prevent from reuniting in described zirconia ceramics slurry macrobead, to avoid the planeness affecting green surface.
Further, during by described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, every Preset Time carry out ultrasonic break up reunion operation, such as, described Preset Time is 5 seconds ~ 10 seconds; And for example, described Preset Time is 7 seconds ~ 10 seconds, preferably, described Preset Time is 8 seconds, like this, what can produce " impact type " to reunion macrobead breaks up effect, as, " wave " or " intermittent type " break up effect, make reunion macrobead inner or/and outside is subject to the surging force of sound wave, there is " loose group " phenomenon, thus can obtain disperseing more uniform described tetragonal phase zirconium oxide powder, described RE oxide powder, and both can be made more uniformly to mix.
In one embodiment, by the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, adopt magnetic agitation married operation; And for example, described magnetic agitation married operation and describedly ultrasonicly break up reunion and operate and carry out simultaneously, like this, the reunion macrobead of described tetragonal phase zirconium oxide powder and described RE oxide powder can be broken up better, more be conducive to mixing of described tetragonal phase zirconium oxide powder and described RE oxide powder, thus the follow-up described zirconia ceramics slurry obtained can be made mixedly more even, and then can prevent from reuniting in described zirconia ceramics slurry macrobead, to avoid the planeness affecting green surface.
In one embodiment, described evaporation operation adopts hot blast process, like this, the evaporation operation of " intrusive mood " can be carried out, namely, when the described solvent evaporates on the surface of described mixed powder, the gap between dried described mixed powder is utilized constantly to be blown into by hot blast in this gap, and then better its inside is heated, promote described solvent evaporates, the method of evaporating box relative to traditional drying, adopt hot blast process to carry out evaporation operation, vaporization efficiency can be improved, and the effect of preferably short described solvent evaporates can also be produced in the situation that temperature is lower.
Further, described hot blast adopts multiple hot blast output port to export; And for example, the rectangular array arrangement of multiple described hot blast output port; And for example, multiple described hot blast output port successively interval is arranged, and like this, adopts hot blast process that is distributed and cover type comprehensively, can improve vaporization efficiency further, and can also produce the effect of preferably short described solvent evaporates in the situation that temperature is lower.
In one embodiment, by in the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, specifically comprise the steps: in advance by after described RE oxide powder and described solvent, add described tetragonal phase zirconium oxide powder again, like this, both can be prevented simultaneously to be added to the secondary agglomeration problem produced in described solvent, thus both powders are mixed more equably.
In one embodiment, after adopting hot blast process to carry out described evaporation operation, also perform following steps: described mixed powder is left standstill cooling under vacuum, like this, described mixed powder can be prevented when cooling, vapor adhesion in air on described mixed powder, thus can be avoided occurring condensation water problem at described mixed powder, to guarantee the quality of described mixed powder.
In one embodiment, after adopting hot blast process to carry out described evaporation operation, also perform following steps: carry out smashing operation to pieces, and obtain described mixed powder, and for example, after smashing operation to pieces described in carrying out, also carry out grinding operation, like this, be beneficial to the described mixed powder obtaining uniform particle sizes.
S130: after described mixed powder, described dispersion agent, described ultraviolet initiator, described photosensitive polymerization monomer and described auxiliary agent being mixed, carries out ball milling and de-bubble operation, obtains zirconia ceramics slurry.
In one embodiment, described mixed powder, described dispersion agent, described ultraviolet initiator, the mass ratio of described photosensitive polymerization monomer and described auxiliary agent is (87.5 ~ 120): (15 ~ 20): (10 ~ 12): (4 ~ 6): (27 ~ 34), and for example, described mixed powder, described dispersion agent, described ultraviolet initiator, the mass ratio of described photosensitive polymerization monomer and described auxiliary agent is (95 ~ 120): (15 ~ 19): (11 ~ 12): (5 ~ 6): (27 ~ 30), preferably, described mixed powder, described dispersion agent, described ultraviolet initiator, the mass ratio of described photosensitive polymerization monomer and described auxiliary agent is 115:16:11:6:28.
In one embodiment, described dispersion agent comprises trolamine, at least one in Terpineol 350 and tbp, and for example, described dispersion agent is trolamine, the mixture of described Terpineol 350 and described tbp, and for example, in the mixture, described trolamine, the mass ratio of described Terpineol 350 and described tbp is (1 ~ 1.5): (1 ~ 1.5): (1 ~ 1.5), preferably, described dispersion agent is trolamine, the mass ratio of described Terpineol 350 and described tbp is 1:1.5:1.5, like this, adopt above-mentioned dispersion agent not only can dissolve described mixed powder better, described ultraviolet initiator, described photosensitive polymerization monomer and described auxiliary agent, to be mixed evenly, less and the larger described zirconia ceramics slurry of solid content of viscosity, and above-mentioned dispersion agent can not with described mixed powder, described ultraviolet initiator, chemistry side occurs for described photosensitive polymerization monomer and described auxiliary agent should, ensure that the stability of described zirconia ceramics slurry.
In one embodiment, described ultraviolet initiator comprises 2, 4, at least one in 6-trimethylbenzoy-dipheny phosphine oxide and 2-hydroxy-2-methyl-1-phenyl-1-acetone, and for example, described ultraviolet initiator is 2, 4, the mixture of 6-trimethylbenzoy-dipheny phosphine oxide and 2-hydroxy-2-methyl-1-phenyl-1-acetone, and for example, in the mixture, described 2, 4, the mass ratio of 6-trimethylbenzoy-dipheny phosphine oxide and described 2-hydroxy-2-methyl-1-phenyl-1-acetone is (1 ~ 1.5): (1 ~ 1.5), preferably, described 2, 4, the mass ratio of 6-trimethylbenzoy-dipheny phosphine oxide and described 2-hydroxy-2-methyl-1-phenyl-1-acetone is 1.5:1.
Wherein, the molecular structural formula of 2,4,6-trimethylbenzoy-dipheny phosphine oxide (DAROCURTPO) is as follows:
Wherein, the molecular structural formula of 2-hydroxy-2-methyl-1-phenyl-1-acetone (DAROCUR1173) is as follows:
In one embodiment, described photosensitive polymerization monomer comprises at least one in methacrylic acid-2-hydroxy methacrylate, bisphenol A epoxy acrylate, urethane acrylate, amino acrylates, tri (propylene glycol) diacrylate and Propylene glycol monoacrylate.
Further, described ultraviolet initiator and described photosensitive polymerization monomer adopt following composite mode, it forms green compact for described zirconia ceramics slurry and has fabulous in-situ solidifying effect, namely be beneficial to and whole components of described zirconia ceramics slurry are carried out in-situ solidifying technique, shaping to complete rapidly, can direct demold and without the drying process of time-consuming complexity, dry shrinkage and cracking phenomena can be avoided, improve the rate that manufactures a finished product, such as, 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, the mass ratio of 2-hydroxy-2-methyl-1-phenyl-1-acetone and methacrylic acid-2-hydroxy methacrylate is (1 ~ 1.5): (1 ~ 1.5): (0.7 ~ 1.2), preferably, 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, the mass ratio of 2-hydroxy-2-methyl-1-phenyl-1-acetone and methacrylic acid-2-hydroxy methacrylate is 1.5:1:0.7, good facilitation effect can be played to in-situ solidifying.
In one embodiment, described auxiliary agent comprises binding agent and fluidizer, such as, described binding agent comprises at least one in polyacrylic acid formicester and ethyl cellulose, like this, can when follow-up tape casting operation, guarantee that described zirconia ceramics slurry has suitable thermoplasticity, preferably dimensional stability and higher tensile strength, thus it is more smooth and easy that described tape casting operation can be made to carry out by adding described binding agent.And for example, described fluidizer comprises at least one in diethyl oxalate ester, tri-ethylene glycol hexane dibutyl phthalate, dioctyl phthalate (DOP) and polyoxyethylene glycol.
Further, in order to strengthen the sticky power of holding in described zirconia ceramics slurry between each component, to guarantee that there is higher tensile strength and good dimensional stability, such as, described auxiliary agent also comprises tackifying resin, and described tackifying resin comprises at least one in single acrylic resin and aliphatic polyurethane acrylic resin, like this, the sticky power of holding between each component in described zirconia ceramics slurry can be strengthened further, to guarantee that there is higher tensile strength and good dimensional stability.It should be noted that, single acrylic resin and aliphatic polyurethane acrylic resin have the advantage that low viscosity and height glue the power of holding, while the described zirconia ceramics slurry viscous of increase holds power, can also guarantee that described zirconia ceramics slurry has the advantage of low viscosity, good fluidity and high solids content.
In one embodiment, wherein, described de-bubble operation is carried out under vacuum; And for example, described de-bubble operation adopts concussion process; And for example, described de-bubble operation adopts concussion up and down and left and right concussion alternate treatment, like this, can improve de-bubble effect.
In one embodiment, described ball milling operation adopts wet ball grinding operation; And for example, described ball milling operation adopts zirconia balls as ball-milling medium, like this, is conducive to the mixture homogeneity improving described zirconia ceramics slurry, and can not introduces new impurity.
S140: described zirconia ceramics slurry is added in ceramic casting machine, then will the substrate of the ceramic casting machine of described zirconia ceramics slurry be carried by after uv cure machine, the substrate of ceramic casting machine is formed zirconia ceramics thin slice green compact.
By described zirconia ceramics slurry is added in ceramic casting machine, described zirconia ceramics stream of slurry can be extended down in the substrate of ceramic casting machine self by pottery casting machine, as, pottery casting machine has substrate, namely substrate is the parts of ceramic casting machine self, so, described zirconia ceramics slurry just can be divided on the substrate of ceramic casting machine, afterwards, to the substrate of the ceramic casting machine of described zirconia ceramics slurry be carried by after uv cure machine again, uv cure machine is to the zirconia ceramics slurry emitting ultraviolet light line on the substrate of ceramic casting machine, under the irradiation of ultraviolet light, described ultraviolet initiator can cause described photosensitive polymerization monomer and UV-crosslinked curing reaction occurs, i.e. in-situ solidifying reaction, so, can complete rapidly shaping, can direct demold and without the drying process of time-consuming complexity, dry shrinkage and cracking phenomena can be avoided, improve the rate that manufactures a finished product.That is, adopt UV-light to cause cross-linking and curing reaction and realize in-situ solidifying effect, traditional drying process can be exempted, thus because drying is excessive there is excess shrinkage in the cracking phenomena caused, dried green compact can to avoid the surface of green compact, demand and the rear local structure problem loosely of sintering of near net-shape cannot be met, the product quality making it prepare is better, reaches industry requirement.
In one embodiment, in advance described zirconia ceramics slurry is heated to 50 DEG C ~ 60 DEG C, and while hot described zirconia ceramics slurry is added in ceramic casting machine, like this, by in advance described zirconia ceramics slurry being heated to 50 DEG C ~ 60 DEG C, can guarantee that the mobility of described zirconia ceramics slurry reaches the requirement required for curtain coating, namely while high solids content, also will guarantee low viscosity.
In one embodiment, described uv cure machine is provided with the first default walking path connected successively, second presets walking path, 3rd presets walking path, fourth line walks path and fifth line walks path, and described first presets walking path, described second presets walking path, described 3rd presets walking path, described fourth line is walked the linear speed that path and described fifth line walk path and is increased successively, and such as, described first presets walking path, described second presets walking path, described 3rd presets walking path, described fourth line walks linear speed 10m/min ~ 15m/min respectively that path and described fifth line walk path, 8m/min ~ 10m/min, 6m/min ~ 8m/min, 4m/min ~ 6m/min and 1m/min ~ 2m/min, wherein, m/min represents m/min, the linear speed unit that the substrate namely carrying the ceramic casting machine of described zirconia ceramics slurry is walked on uv cure machine, and further, described first presets walking path, described second presets walking path, described 3rd presets walking path, described fourth line is walked the UV-irradiation intensity that path and described fifth line walk path and is respectively 260mw/cm 2~ 320mw/cm 2, 350mw/cm 2~ 380mw/cm 2, 380mw/cm 2~ 400mw/cm 2, 400mw/cm 2~ 420mw/cm 2and 450mw/cm 2~ 500mw/cm 2, like this, adopt above-mentioned linear speed and UV-irradiation intensity, zirconia ceramics thin slice green compact can be conducive to and carry out in-situ solidifying reaction, and the problem that brittleness is excessive and ftracture can not be produced.
S150: after being sintered by described zirconia ceramics thin slice green compact, obtain described zirconia ceramics thin slice.
After being sintered by described zirconia ceramics thin slice green compact, the organism in it can be removed, and then obtain described zirconia ceramics thin slice.
In one embodiment, the step that described zirconia ceramics thin slice green compact carry out sintering is as follows: be 0.5 DEG C/min at 0 DEG C ~ 120 DEG C temperature rise rates, between 120 DEG C ~ 550 DEG C, temperature rise rate is 0.4 DEG C/min, between 550 DEG C ~ 800 DEG C, temperature rise rate is 0.5 DEG C/min, and to guarantee in described zirconia ceramics thin slice various organism all to get rid of, because getting rid of, speed is too fast does not cause defect.Preferably, more than 800 DEG C, be raised to 1450 DEG C respectively with the temperature rise rate of 2 DEG C/min, 1500 DEG C, 1550 DEG C, and at 1450 DEG C, 1500 DEG C, 1550 DEG C are incubated 5h, 3h, 2h respectively, so, can guarantee the quality of described zirconia ceramics thin slice.Such as, 1450 DEG C time, be incubated 5 hours, 1500 DEG C time, be incubated 3 hours, 1550 DEG C time, be incubated 2 hours.
The UV-light that adopts above-mentioned zirconia ceramics method for preparing slices causes cross-linking and curing reaction and realizes in-situ solidifying effect, thus traditional drying process can be exempted, thus because drying is excessive there is excess shrinkage in the cracking phenomena caused, dried green compact can to avoid the surface of green compact, demand and the rear local structure problem loosely of sintering of near net-shape cannot be met, and then can guarantee that the product quality prepared is better, reach industry requirement.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (7)

1. a zirconia ceramics method for preparing slices, is characterized in that, comprises the steps:
Stable tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersion agent, ultraviolet initiator, photosensitive polymerization monomer and auxiliary agent are provided;
By described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, and carry out ultrasonicly breaing up reunion operation, then carry out evaporation operation described solvent is removed, obtain mixed powder;
After described mixed powder, described dispersion agent, described ultraviolet initiator, described photosensitive polymerization monomer and described auxiliary agent are mixed, carry out ball milling and de-bubble operation, obtain zirconia ceramics slurry;
Described zirconia ceramics slurry is added in ceramic casting machine, then will the substrate of the ceramic casting machine of described zirconia ceramics slurry be carried by after uv cure machine, the substrate of ceramic casting machine is formed zirconia ceramics thin slice green compact;
After being sintered by described zirconia ceramics thin slice green compact, obtain described zirconia ceramics thin slice.
2. zirconia ceramics method for preparing slices according to claim 1, is characterized in that, during by described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, every Preset Time carry out ultrasonic break up reunion operation.
3. zirconia ceramics method for preparing slices according to claim 2, is characterized in that, described Preset Time is 5 seconds ~ 10 seconds.
4. zirconia ceramics method for preparing slices according to claim 3, is characterized in that, described Preset Time is 7 seconds ~ 10 seconds.
5. zirconia ceramics method for preparing slices according to claim 4, is characterized in that, described Preset Time is 8 seconds.
6. zirconia ceramics method for preparing slices according to claim 1, is characterized in that, by the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, adopts magnetic agitation married operation.
7. zirconia ceramics method for preparing slices according to claim 1, it is characterized in that, by in the operation of described tetragonal phase zirconium oxide powder, described RE oxide powder and described solvent, specifically comprise the steps: in advance by after described RE oxide powder and described solvent, then add described tetragonal phase zirconium oxide powder.
CN201510981527.1A 2015-12-22 2015-12-22 Zirconia ceramics method for preparing slices Active CN105541326B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510981527.1A CN105541326B (en) 2015-12-22 2015-12-22 Zirconia ceramics method for preparing slices

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510981527.1A CN105541326B (en) 2015-12-22 2015-12-22 Zirconia ceramics method for preparing slices

Publications (2)

Publication Number Publication Date
CN105541326A true CN105541326A (en) 2016-05-04
CN105541326B CN105541326B (en) 2018-05-15

Family

ID=55820949

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510981527.1A Active CN105541326B (en) 2015-12-22 2015-12-22 Zirconia ceramics method for preparing slices

Country Status (1)

Country Link
CN (1) CN105541326B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473729A (en) * 2017-09-18 2017-12-15 重庆文理学院 A kind of translucent YAG fluorescence ceramics method for preparing slices
CN110204313A (en) * 2018-02-28 2019-09-06 清华大学 A kind of method and shaping method of ceramics of dispersing agent crosslinking solidification ceramic suspension body in situ

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4957673A (en) * 1988-02-01 1990-09-18 California Institute Of Technology Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof
CN101541708A (en) * 2006-11-29 2009-09-23 康宁股份有限公司 Plasticized mixture and method for stiffening
CN104788096A (en) * 2015-03-31 2015-07-22 北京博曼迪汽车科技有限公司 Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4957673A (en) * 1988-02-01 1990-09-18 California Institute Of Technology Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof
CN101541708A (en) * 2006-11-29 2009-09-23 康宁股份有限公司 Plasticized mixture and method for stiffening
CN104788096A (en) * 2015-03-31 2015-07-22 北京博曼迪汽车科技有限公司 Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473729A (en) * 2017-09-18 2017-12-15 重庆文理学院 A kind of translucent YAG fluorescence ceramics method for preparing slices
CN110204313A (en) * 2018-02-28 2019-09-06 清华大学 A kind of method and shaping method of ceramics of dispersing agent crosslinking solidification ceramic suspension body in situ
CN110204313B (en) * 2018-02-28 2021-10-15 清华大学 Method for cross-linking and in-situ solidifying ceramic suspension by using dispersing agent and ceramic forming method

Also Published As

Publication number Publication date
CN105541326B (en) 2018-05-15

Similar Documents

Publication Publication Date Title
CN105585319B (en) Zirconia ceramics substrate preparation method
US20150232390A1 (en) Method for making ceramic thin exterior part
CN114149260B (en) Low-thermal-conductivity high-entropy ceramic thermal barrier coating material
CN106673627A (en) Method for preparing toughened aluminum oxide ceramic based on stereo lithography appearance namely 3D printing
CN101503297B (en) Tape casting preparation for gradient material in rotating magnetic field
CN101269977B (en) Method for preparing ceramic sheet with composite caking agent series water-based cast
CN104194020A (en) Method for preparing flexible inorganic/polymer composite film with high dielectric property
CN112608154A (en) Silicon nitride ceramic slurry and preparation method and application thereof
KR100448979B1 (en) Ceramic slurry composition, manufacturing method therefor and ceramic green sheet formed thereby
CN105541326A (en) Preparation method of zirconia ceramic slice
CN105461302A (en) Preparation method of zirconia ceramic backing
CN106630996A (en) Preparation method of gel injection molding MgAl2O4 biscuit
CN108998893A (en) A kind of gradient-structure Kynoar based composite dielectric and preparation method thereof
CN109534794A (en) A method of promoting increasing material manufacturing formed ceramic parts degreasing intensity
CN105272223A (en) Preparation method of large-size zirconia-based heat insulation material
CN1315754C (en) Method for precission shaping ceramic blank by semi-water-base injection-moulding gel process
CN113880588B (en) Method for preparing uniformly coated AlON powder and transparent ceramic thereof
CN103787650A (en) Method for preparing ITO (Indium Tin Oxide) target
CN110511021A (en) A kind of novel zirconia ceramics forming method
CN103208587B (en) Method for preparing piezoelectric fiber composite
CN113716951A (en) Preparation method of YAG-based transparent ceramic with large-size sheet composite structure
CN109516813B (en) Method for preparing high-light-transmittance AlON transparent ceramic by direct water injection molding
WO2017116000A1 (en) Method for manufacturing transparent ceramic phosphor plate
CN104476655B (en) A kind of gel centrifugal forming method of ceramic idiosome
CN102976726A (en) Method for preparing ultrathin type ferrite sheet by using microwave sintering

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant