CN106673627A - Method for preparing toughened aluminum oxide ceramic based on stereo lithography appearance namely 3D printing - Google Patents

Method for preparing toughened aluminum oxide ceramic based on stereo lithography appearance namely 3D printing Download PDF

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CN106673627A
CN106673627A CN201710051789.7A CN201710051789A CN106673627A CN 106673627 A CN106673627 A CN 106673627A CN 201710051789 A CN201710051789 A CN 201710051789A CN 106673627 A CN106673627 A CN 106673627A
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degreasing
product
stereolithography
base substrate
preparation
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刘伟
伍海东
伍尚华
吴子薇
蒋强国
黄容基
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Guangdong University of Technology
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Guangdong University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped 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 aluminium oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing 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
    • C04B35/632—Organic additives
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
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    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms

Abstract

The invention belongs to the technical field of 3D printing, and particularly relates to a method for preparing toughened aluminum oxide ceramic based on stereo lithography appearance namely 3D printing. The invention provides a composition. The composition comprises the following raw materials: aluminum oxide ceramic powder, a liquid premix, a photoinitiator, a dispersant and a surfactant. The invention further provides a preparation method for preparing zirconium oxide-toughened aluminum oxide ceramic by using the composition. The preparation method comprises the following steps: preparing a slurry, moulding, drying and degreasing, wherein a blank is dried primarily, degreased and post-treated. According to the technical scheme provided by the invention, the ceramic blank is prepared by stereo lithography appearance, so that the moulding efficiency is high and the dimensional accuracy of the product is high; through optimization of parameters in the degreasing step, the blank does not deform and does not crack in the degreasing process; by an infiltrating step, the growth of aluminum oxide crystal grains is inhibited, and through electronic microscopic observation on the product structure, the microstructure of the product is uniform; the technical defect that in the prior art, the structure of the zirconium oxide-toughened aluminum oxide ceramic is nonuniform is overcome.

Description

A kind of method that 3D printing based on Stereolithography prepares aluminum oxide toughening ceramic
Technical field
The invention belongs to 3D printing technique field, more particularly to a kind of 3D printing based on Stereolithography prepares aluminum oxide The method of toughening ceramic.
Background technology
3D printing technique is Stereolithography technology (Stereo lithography Appearance, abridge SLA), its Principle is：It is scanned in x-y faces with the laser beam of intensity by computer controls specific wavelength, is allowed to by point to line, by line To face consecutive solidification, ceramic size is selectively solidified, complete the drawing performance of an aspect, then lifting platform is in vertical direction The height of a mobile synusia, resolidification another aspect, one ceramic body of the composition that is so layering.However, using light Although cure process can be easy to prepare the alumina ceramic component of labyrinth, aluminum oxide base substrate is through sintering Afterwards, at high temperature crystal grain is susceptible to abnormal growth, reduces its intensity, hardness and related mechanical property, therefore have very much must Will be to alumina doped second phase, to regulate and control its mechanical property.
In prior art, it will usually improve above-mentioned deficiency by being mixed into Zirconium powder.Conventional meanses are mixed into zirconia powder Body, is not only difficult to prepare the Zirconia reinforced alumina material of homogeneous texture, and the inhomogeneities of microstructure can be aggravated on the contrary. In prior art, zirconic aluminium oxide ceramics is mixed with, with the uneven technological deficiency of structure.
Therefore, develop a kind of preparation method of aluminium oxide ceramics, for solving prior art in, be mixed with zirconic oxygen Change aluminium ceramics with the uneven technological deficiency of structure, become those skilled in the art's problem demanding prompt solution.
The content of the invention
In view of this, the invention provides a kind of preparation method of aluminium oxide ceramics, for solving prior art in, be mixed with Zirconic aluminium oxide ceramics has the uneven technological deficiency of structure.
The invention provides a kind of composition, the raw material of the composition includes：Alumina ceramic powder, premixed liquid, light Initiator, dispersant and surfactant；
The solute of the premixed liquid is selected from：Dimethylacrylate, Methacrylamide, 2-hydroxyethyl methacrylate With one or more in N-N ' methylene-bisacrylamides.
Preferably, in terms of mass parts, the raw material of the composition includes：20~85 parts of alumina ceramic powder, premixed liquid 1~3 part of 10~70 parts, 1~3 part of light trigger, 1~3 part of dispersant and surfactant.
Preferably, the alumina ceramic powder is α-Al2O3, the purity of the alumina ceramic powder is more than 99%, institute The particle diameter for stating aluminium oxide ceramics is：0.1~0.5 μm.
Preferably, the alumina ceramic powder has bimodal distribution structure, i.e.,：The particle diameter of the alumina ceramic powder Wider distribution.
Preferably, the alumina ceramic powder is obtained by the alumina ceramic powder compounding of two kinds of different-grain diameters.
Preferably, the light trigger is selected from：BASF 184, BASF 819, BASF 256, BASF 2959 and One or more in BASF 1173；
The dispersant is selected from：In BYK-9076, Sodium Polyacrylate, ammonium polyacrylate and polyvinylpyrrolidone one Plant or various；
The surfactant is selected from：Silanes activating agent or coupling agent.
Preferably, the solvent of the premixed liquid is selected from：One or more in deionized water, glycerine and absolute ethyl alcohol；
In the premixed liquid, the mass concentration of solute is 20~85%.
Present invention also offers the composition described in a kind of utilization any of the above one prepares the preparation side of aluminium oxide ceramics Method, the preparation method is：
Step one, prepare slurry：Ball milling after the mixing of alumina ceramic powder, premixed liquid, dispersant and surfactant, then Mix with light trigger, obtain slurry；
Step 2, shaping：The slurry Stereolithography, obtains base substrate；
Step 3, drying and degreasing：Successively Jing is dried for the first time and degreasing the base substrate, obtains porous body；
Step 4, infiltration：The porous body infiltrates in impregnating solution, obtains infiltration base substrate；
Step 5, post processing：Successively Jing is dried for second and sinters the infiltration base substrate, obtains alumina ceramic product.
Preferably, the preparation method of the slurry is：
Solute is dissolved in solvent and stirs to obtain premixed liquid；
After alumina ceramic powder, ethanol and dispersant, first time ball milling obtains the first product；
After the mixing of first product, premixed liquid, dispersant and surfactant, second ball milling obtains the second product；
Mix with light trigger after the second product bubble removing, obtain slurry.
Preferably, the ball-milling medium of the first time ball milling be aluminum oxide, the ball-milling medium shape of the first time ball milling For spherical, a diameter of 1~3mm of ball-milling medium of the first time ball milling, the material ball ratio of the first time ball milling is (2:1)~ (5:1), the time of the first time ball milling is 3~6h.
Preferably, the ball-milling medium of second ball milling be zirconium oxide, the ball-milling medium shape of second ball milling For spherical, a diameter of 5~10mm of ball-milling medium of second ball milling, the material ball ratio of second ball milling is (1:1)~ (3:1), the time of second ball milling is 6~12h.
Preferably, the method for the bubble removing is：Second product stirs 10~60min under condition of negative pressure.
Preferably, the impregnating solution is the mixed solution of zirconates and yttrium salt；
The zirconates is selected from：ZrOCl2·8H2O、Zr(NO3)4·5H2O and Zr (SO4)2·4H2One or more in O；
The yttrium salt is Y (NO3)3·6H2O or Y2(SO4)3·8H2O；
The time of the infiltration is 1~24h.
Preferably, the vacuum of the infiltration is more than 0.08MPa.
Preferably, the preparation method of the maceration solution is：10~60min of ultrasound after the mixing of zirconates, yttrium salt and solvent.
Preferably, the method that the first time is dried is liquid dried and/or microwave drying, the liquid of the liquid dried Drier is selected from：One or more in polyethylene glycol, ethanol and ethylene glycol；
The method of the degreasing is：Dried base substrate is first carried out after vacuum degreasing or atmosphere protection degreasing, then carries out sky Qi exhaustion fat, the porosity of the porous body is 40~60%；
The temperature being dried for described second is 60~150 DEG C, and the second dry time is 3~24h；
The method of the sintering is selected from：One or more in normal pressure-sintered, atmosphere sintering and HIP sintering.
Preferably, the time of the liquid dried is 6~72h.
Preferably, the time of the microwave drying is 5~36h.
Preferably, the vacuum degreasing or the method for atmosphere protection degreasing are：With the ramp of 3~10 DEG C/min extremely 600~1000 DEG C and be incubated in 2~3h, and temperature-rise period every 100~150 DEG C be incubated 0~60min after, be cooled to room temperature.
Preferably, the vacuum of the vacuum degreasing is less than 0.09MPa, and the shielding gas of the atmosphere protection degreasing is：N2 Or inert gas.
Preferably, the method for the air degreasing is：So that the ramp of 1~5 DEG C/min is to 600~1000 DEG C and is incubated 2~4h, is cooled to room temperature.
Preferably, the method for the sintering is：So that the ramp of 10~15 DEG C/min is to 1350~1550 DEG C and is incubated 1 ~4h, is cooled to room temperature.
Preferably, the sweep speed of the Stereolithography be 1000~3000mm/s, the scanning of the Stereolithography Mode is X-Y, and the sweep span of the Stereolithography is 0.1~0.5mm, the light wave of the Stereolithography is a length of 365~ 405nm。
In sum, the invention provides a kind of composition, the raw material of the composition includes：Alumina ceramic powder, Premixed liquid, light trigger, dispersant and surfactant；The solute of the premixed liquid is selected from：Dimethylacrylate, methyl-prop One or more in acrylamide, 2-hydroxyethyl methacrylate and N-N ' methylene-bisacrylamides.The present invention is also provided A kind of utilization above-mentioned composition prepares the preparation method of aluminium oxide ceramics, and the preparation method is：Step one, prepare slurry： Ball milling after the mixing of alumina ceramic powder, premixed liquid, dispersant and surfactant, then mix with light trigger, obtain slurry；Step Rapid two, it is molded：The slurry Stereolithography, obtains base substrate；Step 3, drying and degreasing：Successively Jing is dry for the first time for the base substrate Dry and degreasing, obtains porous body；Step 4, infiltration：The porous body infiltrates in impregnating solution, obtains infiltration base substrate；Step 5th, post-process：Successively Jing is dried for second and sinters the infiltration base substrate, obtains alumina ceramic product.The skill that the present invention is provided In art scheme, ceramic body is prepared by Stereolithography method, shaping efficiency is high, product size high precision；By defatting step The optimization of parameter, skimming processes base substrate is indeformable, do not ftracture；By impregnation step, it is suppressed that the production of zirconia grains, Jing is electric Sem observation product structure, product microstructure is uniform；In solving prior art, it is mixed with zirconic aluminium oxide ceramics and there is knot The uneven technological deficiency of structure.
Specific embodiment
The invention provides a kind of method that 3D printing based on Stereolithography prepares aluminum oxide toughening ceramic, for solving Certainly in prior art, it is mixed with zirconic aluminium oxide ceramics and there is the uneven technological deficiency of structure.
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement Example is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection Enclose.
In order to the present invention is described in more detail, a kind of preparation of the present invention is provided aluminium oxide ceramics with reference to embodiment Method and its preparing raw material, are specifically described.
Embodiment 1
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 1 Specific embodiment.
Step one, prepare slurry
20g solutes are dissolved in 80g solvents, and premixed liquid 1 is stirred to obtain after mixing.In the present embodiment, solute is methacryl Amine, solvent is glycerine.
After 100g alumina ceramic powders, 300g ethanol and 1.5g dispersants, first time ball milling obtains the first product 1. In first time ball milling, ball-milling medium is aluminum oxide, and a diameter of 3mm of ball-milling medium, being shaped as ball-milling medium is spherical, material ball ratio For 2:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, oxidation Aluminium ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is polyvinylpyrrolidone.
After the mixing of the first products of 40g 1,60g premixed liquids 1,0.5g dispersants and 0.5g surfactants, second ball milling, Obtain the second product 1.In second ball milling, ball-milling medium is aluminum oxide, a diameter of 1mm of ball-milling medium, the shape of ball-milling medium For spherical, material ball ratio is 2:1.In the present embodiment, dispersant is polyvinylpyrrolidone, and surfactant is titanate esters.
The second products of 50g 1 are stirred after 10min bubble removings under condition of negative pressure, are mixed with 0.2g light triggers, obtain slurry 1. In the present embodiment, light trigger is BASF 819.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 1, according to designed ceramic shape base substrate 1 is drawn to obtain.Its In, the sweep speed of Stereolithography is 1000mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.5, a length of 365nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 1 is placed in liquid drier and is dried after 6h, and degreasing obtains porous body 1；Wherein, the porosity of porous body 1 For 40%.In the present embodiment, liquid drier is polyethylene glycol.
Degreasing method is：Dried base substrate 1 is first carried out after vacuum degreasing, then carries out air degreasing.
In the present embodiment, the method for vacuum degreasing is：So that the ramp of 3 DEG C/min is to 600 DEG C and is incubated 3h, and heat up During every 100 DEG C be incubated 10min after, cool to room temperature with the furnace；Wherein, the vacuum of vacuum degreasing is less than 0.09MPa.It is empty The method of qi exhaustion fat is：So that the ramp of 1 DEG C/min is to 600 DEG C and is incubated 3h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 1 infiltrates 3h in impregnating solution 1, must infiltrate base substrate 1.
In the present embodiment, impregnating solution 1 is obtained by the mixed solution ultrasound 10min of zirconates and yttrium salt；Wherein, zirconates is ZrOCl2·8H2O, yttrium salt is Y (NO3)3·6H2O。
Step 5, post processing
Infiltration base substrate 1 is normal pressure-sintered after being dried 12h under the conditions of 30 DEG C, obtains alumina ceramic product 1.
In the present embodiment, the method for sintering is：So that the ramp of 10 DEG C/min is to 1350 DEG C and is incubated 1h, along with the furnace cooling To room temperature.
Embodiment 2
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 2 Specific embodiment.
Step one, prepare slurry
35g solutes are dissolved in 65g solvents, and premixed liquid 2 is stirred to obtain after mixing.In the present embodiment, solute is dimethyl allene Acid esters, solvent is glycerine and deionized water.
After 100g alumina ceramic powders, 300g ethanol and 2.0g dispersants, first time ball milling obtains the first product 2. In first time ball milling, ball-milling medium is aluminum oxide, and a diameter of 3mm of ball-milling medium, being shaped as ball-milling medium is spherical, material ball ratio For 5:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, oxidation Aluminium ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is Sodium Polyacrylate.
After the mixing of the first products of 45g 2,55g premixed liquids 2,1g dispersants and 1g surfactants, second ball milling obtains the Two products 2.In second ball milling, ball-milling medium is aluminum oxide, a diameter of 1mm of ball-milling medium, and ball-milling medium is shaped as ball Shape, material ball ratio is 1:1.In the present embodiment, dispersant is Sodium Polyacrylate, and surfactant is silane coupling agent.
The second products of 50g 2 are stirred after 20min bubble removings under condition of negative pressure, are mixed with 0.3g light triggers, obtain slurry 2. In the present embodiment, light trigger is BASF 1173.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 2, according to designed ceramic shape base substrate 2 is drawn to obtain.Its In, the sweep speed of Stereolithography is 2000mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.3, a length of 365nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 2 is placed in liquid drier and is dried after 36h, and degreasing obtains porous body 2；Wherein, the hole of porous body 2 Rate is 60%.In the present embodiment, liquid drier is ethylene glycol and polyethylene glycol.
Degreasing method is：Dried base substrate 2 is first carried out after vacuum degreasing, then carries out air degreasing.
In the present embodiment, the method for vacuum degreasing is：So that the ramp of 5 DEG C/min is to 800 DEG C and is incubated 3h, and heat up During every 100 DEG C be incubated 30min after, cool to room temperature with the furnace；Wherein, the vacuum of vacuum degreasing is less than 0.09MPa.It is empty The method of qi exhaustion fat is：So that the ramp of 3 DEG C/min is to 700 DEG C and is incubated 1h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 2 infiltrates 6h in impregnating solution 2, must infiltrate base substrate 2.
In the present embodiment, impregnating solution 2 is obtained by the mixed solution ultrasound 25min of zirconates and yttrium salt；Wherein, zirconates is Zr (NO3)4·5H2O, yttrium salt is Y (NO3)3·6H2O。
Step 5, post processing
Atmosphere sintering after base substrate 2 is dried 6h under the conditions of 60 DEG C is infiltrated, alumina ceramic product 2 is obtained.
In the present embodiment, the method for sintering is：So that the ramp of 10 DEG C/min is to 1450 DEG C and is incubated 1h, along with the furnace cooling To room temperature.
Embodiment 3
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 3 Specific embodiment.
Step one, prepare slurry
50g solutes are dissolved in 50g solvents, and premixed liquid 3 is stirred to obtain after mixing.In the present embodiment, solute is dimethyl allene Acid esters, solvent is deionized water.
After 100g alumina ceramic powders, 300g ethanol and 2.5g dispersants, first time ball milling obtains the first product 3. In first time ball milling, ball-milling medium is zirconium oxide, and a diameter of 1mm of ball-milling medium, being shaped as ball-milling medium is spherical, material ball ratio For 4:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, oxidation Aluminium ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is Sodium Polyacrylate.
After the mixing of the first products of 50g 3,50g premixed liquids 3,1.5g dispersants and 1.5g surfactants, second ball milling, Obtain the second product 3.In second ball milling, ball-milling medium is zirconium oxide, a diameter of 8mm of ball-milling medium, the shape of ball-milling medium For spherical, material ball ratio is 3:1.In the present embodiment, dispersant is BYK-9076, and surfactant is coupling agent.
The second products of 50g 3 are stirred after 30min bubble removings under condition of negative pressure, are mixed with 0.6g light triggers, obtain slurry 3. In the present embodiment, light trigger is BASF 1173 and BASF 819.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 3, according to designed ceramic shape base substrate 3 is drawn to obtain.Its In, the sweep speed of Stereolithography is 3000mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.1, a length of 365nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 3 is placed in liquid drier and is dried after 72h, and degreasing obtains porous body 3；Wherein, the hole of porous body 3 Rate is 50%.In the present embodiment, liquid drier is ethylene glycol.
Degreasing method is：Dried base substrate 3 is first carried out after vacuum degreasing, then carries out air degreasing.
In the present embodiment, the method for vacuum degreasing is：So that the ramp of 6 DEG C/min is to 900 DEG C and is incubated 2h, and heat up During every 100 DEG C be incubated 60min after, cool to room temperature with the furnace；Wherein, the vacuum of vacuum degreasing is less than 0.09MPa.It is empty The method of qi exhaustion fat is：So that the ramp of 5 DEG C/min is to 900 DEG C and is incubated 4h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 3 infiltrates 6h in impregnating solution 3, must infiltrate base substrate 3.
In the present embodiment, impregnating solution 3 is obtained by the mixed solution ultrasound 30min of zirconates and yttrium salt；Wherein, zirconates is Zr (SO4)2·4H2O, yttrium salt is Y2(SO4)3·8H2O。
Step 5, post processing
HIP sintering after base substrate 3 is dried 10h under the conditions of 80 DEG C is infiltrated, alumina ceramic product 3 is obtained.
In the present embodiment, the method for sintering is：So that the ramp of 10 DEG C/min is to 1550 DEG C and is incubated 1h, along with the furnace cooling To room temperature.
Embodiment 4
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 4 Specific embodiment.
Step one, prepare slurry
65g solutes are dissolved in 35g solvents, and premixed liquid 4 is stirred to obtain after mixing.In the present embodiment, solute is methacrylic acid 2- hydroxy methacrylates, solvent is deionized water.
After 100g alumina ceramic powders, 300g ethanol and 3g dispersants, first time ball milling obtains the first product 4.The In ball milling, ball-milling medium is zirconium oxide, and a diameter of 1mm of ball-milling medium, being shaped as ball-milling medium is spherical, and material ball ratio is 2:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, aluminum oxide Ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is BYK-9076 and Sodium Polyacrylate.
After the mixing of the first products of 60g 4,40g premixed liquids 4,2g dispersants and 2g surfactants, second ball milling obtains the Two products 4.In second ball milling, ball-milling medium is zirconium oxide, a diameter of 8mm of ball-milling medium, and ball-milling medium is shaped as ball Shape, material ball ratio is 2:1.In the present embodiment, dispersant is Sodium Polyacrylate, and surfactant is silanes activating agent.
The second products of 50g 4 are stirred after 40min bubble removings under condition of negative pressure, are mixed with 0.8g light triggers, obtain slurry 4. In the present embodiment, light trigger is BASF 184.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 4, according to designed ceramic shape base substrate 4 is drawn to obtain.Its In, the sweep speed of Stereolithography is 2500mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.5, a length of 405nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 4 is placed in after microwave drying 12h, degreasing, obtains porous body 4；Wherein, the porosity of porous body 4 is 40%.
Degreasing method is：After the advanced row atmosphere protection degreasing of dried base substrate 4, then carry out air degreasing.
In the present embodiment, the method for atmosphere protection degreasing is：So that the ramp of 3 DEG C/min is to 600 DEG C and is incubated 3h, and It is incubated after 30min every 150 DEG C in temperature-rise period, cools to room temperature with the furnace；Wherein, the shielding gas of atmosphere protection degreasing is：N2。 The method of air degreasing is：So that the ramp of 5 DEG C/min is to 1000 DEG C and is incubated 2h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 4 infiltrates 10h in impregnating solution 4, must infiltrate base substrate 4.
In the present embodiment, impregnating solution 4 is obtained by the mixed solution ultrasound 35min of zirconates and yttrium salt；Wherein, zirconates is ZrOCl2·8H2O、Zr(NO3)4·5H2O, yttrium salt is Y (NO3)3·6H2O or Y2(SO4)3·8H2O。
Step 5, post processing
Infiltration base substrate 4 is normal pressure-sintered after being dried 12h under the conditions of 100 DEG C, obtains alumina ceramic product 4.
In the present embodiment, the method for sintering is：So that the ramp of 10 DEG C/min is to 1350 DEG C and is incubated 4h, along with the furnace cooling To room temperature.
Embodiment 5
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 5 Specific embodiment.
Step one, prepare slurry
75g solutes are dissolved in 25g solvents, and premixed liquid 5 is stirred to obtain after mixing.In the present embodiment, solute is N-N ' methylene Bisacrylamide, solvent is glycerine.
After 100g alumina ceramic powders, 300g ethanol and 5g dispersants, first time ball milling obtains the first product 5.The In ball milling, ball-milling medium is aluminum oxide, and a diameter of 2mm of ball-milling medium, being shaped as ball-milling medium is spherical, and material ball ratio is 5:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, aluminum oxide Ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is BYK-9076.
After the mixing of the first products of 70g 5,30g premixed liquids 5,2.5g dispersants and 2.5g surfactants, second ball milling, Obtain the second product 5.In second ball milling, ball-milling medium is zirconium oxide, a diameter of 8mm of ball-milling medium, the shape of ball-milling medium For spherical, material ball ratio is 5:1.In the present embodiment, dispersant is ammonium polyacrylate, and surfactant is coupling agent.
The second products of 50g 5 are stirred after 50min bubble removings under condition of negative pressure, are mixed with 1g light triggers, obtain slurry 5.This In embodiment, light trigger is BASF 256.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 5, according to designed ceramic shape base substrate 5 is drawn to obtain.Its In, the sweep speed of Stereolithography is 1500mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.1, a length of 405nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 5 is placed in after microwave drying 24h, degreasing, obtains porous body 5；Wherein, the porosity of porous body 5 is 50%.
Degreasing method is：After the advanced row atmosphere protection degreasing of dried base substrate 5, then carry out air degreasing.
In the present embodiment, the method for atmosphere protection degreasing is：So that the ramp of 6 DEG C/min is to 800 DEG C and is incubated 3h, and It is incubated after 20min every 100 DEG C in temperature-rise period, cools to room temperature with the furnace；Wherein, the shielding gas of atmosphere protection degreasing is：It is lazy Property gas.The method of air degreasing is：So that the ramp of 1 DEG C/min is to 600 DEG C and is incubated 2h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 5 infiltrates 12h in impregnating solution 5, must infiltrate base substrate 5.
In the present embodiment, impregnating solution 5 is obtained by the mixed solution ultrasound 45min of zirconates and yttrium salt；Wherein, zirconates is ZrOCl2·8H2O, yttrium salt is Y2(SO4)3·8H2O。
Step 5, post processing
Infiltration base substrate 5 is normal pressure-sintered after being dried 18h under the conditions of 120 DEG C, obtains alumina ceramic product 5.
In the present embodiment, the method for sintering is：So that the ramp of 10 DEG C/min is to 1450 DEG C and is incubated 2h, along with the furnace cooling To room temperature.
Embodiment 6
A kind of preparation method of aluminium oxide ceramics of the present embodiment to be provided using the present invention prepares alumina ceramic product 6 Specific embodiment.
Step one, prepare slurry
85g solutes are dissolved in 15g solvents, and premixed liquid 6 is stirred to obtain after mixing.In the present embodiment, solute is methacryl Amine and 2-hydroxyethyl methacrylate, solvent is glycerine.
After 100g alumina ceramic powders, 300g ethanol and 8g dispersants, first time ball milling obtains the first product 6.The In ball milling, ball-milling medium is zirconium oxide, and a diameter of 3mm of ball-milling medium, being shaped as ball-milling medium is spherical, and material ball ratio is 4:1.In the present embodiment, the purity that alumina ceramic powder has two peak structure, alumina ceramic powder is more than 99%, aluminum oxide Ceramic powder is α-Al2O3, the particle diameter of aluminium oxide ceramics is：0.1~0.5 μm；Dispersant is ammonium polyacrylate and polyvinyl pyrrole Alkanone.
After the mixing of the first products of 80g 6,20g premixed liquids 6,3g dispersants and 3g surfactants, second ball milling obtains the Two products 6.In second ball milling, ball-milling medium is zirconium oxide, a diameter of 7mm of ball-milling medium, and ball-milling medium is shaped as ball Shape, material ball ratio is 2:1.In the present embodiment, dispersant is polyvinylpyrrolidone, and surfactant is coupling agent.
The second products of 50g 6 are stirred after 60min bubble removings under condition of negative pressure, are mixed with 1.5g light triggers, obtain slurry 6. In the present embodiment, light trigger is BASF 2959.
Step 2, shaping
The Stereolithography in Stereolithography equipment of slurry 6, according to designed ceramic shape base substrate 6 is drawn to obtain.Its In, the sweep speed of Stereolithography is 1000mm/s, and the scan mode of Stereolithography is X-Y, the scanning of Stereolithography Spacing is 0.2, a length of 405nm of light wave of Stereolithography.
Step 3, drying and degreasing：
Base substrate 6 is placed in after microwave drying 36h, degreasing, obtains porous body 6；Wherein, the porosity of porous body 6 is 60%.
Degreasing method is：Dried base substrate 6 is first carried out after vacuum degreasing or atmosphere protection degreasing, then carry out air take off Fat.
In the present embodiment, the method for atmosphere protection degreasing is：So that the ramp of 10 DEG C/min is to 1000 DEG C and is incubated 3h, And be incubated after 60min every 150 DEG C in temperature-rise period, cool to room temperature with the furnace；Wherein, the shielding gas of atmosphere protection degreasing is： N2.The method of air degreasing is：So that the ramp of 5 DEG C/min is to 1000 DEG C and is incubated 4h, room temperature is cooled to.
Step 4, infiltration
Under the conditions of vacuum is more than 0.08MPa, porous body 6 infiltrates 16h in impregnating solution 6, must infiltrate base substrate 6.
In the present embodiment, impregnating solution 6 is obtained by the mixed solution ultrasound 60min of zirconates and yttrium salt；Wherein, zirconates is Zr (SO4)2·4H2O and Zr (NO3)4·5H2O, yttrium salt is Y (NO3)3·6H2O and Y2(SO4)3·8H2O。
Step 5, post processing
Infiltration base substrate 6 is normal pressure-sintered after being dried 24h under the conditions of 150 DEG C, obtains alumina ceramic product 6.
In the present embodiment, the method for sintering is：So that the ramp of 15 DEG C/min is to 1550 DEG C and is incubated 2h, along with the furnace cooling To room temperature.
Embodiment 7
The present embodiment is the embodiment for verifying product 1 to the beneficial effect of product 6 obtained in embodiment 1 to embodiment 6.
Electron microscopic observation：The structure of 1~product of product 6 is observed by sem image, show that zirconium oxide is evenly distributed in oxygen In changing aluminium crystal boundary, the abnormal growth of alumina grain is successfully inhibited, while promoting the sintering densification of aluminium oxide ceramics.
The Vickers hardness of product 1 is 18.0GPa, and toughness is 3.2MPa m1/2, crystallite dimension is 1.0 μm.
The Vickers hardness of product 2 is 18.5GPa, and toughness is 3.5MPa m1/2, crystallite dimension is 1.3 μm.
The Vickers hardness of product 3 is 19.1GPa, and toughness is 3.8MPa m1/2, crystallite dimension is 1.8 μm.
The Vickers hardness of product 4 is 20.1GPa, and toughness is 3.7MPa m1/2, crystallite dimension is 1.5 μm.
The Vickers hardness of product 5 is 20.3GPa, and toughness is 4.2MPa m1/2, crystallite dimension is 1.8 μm.
The Vickers hardness of product 6 is 21.1GPa, and toughness is 4.5MPa m1/2, crystallite dimension is 2.0 μm.
In sum, the invention provides a kind of composition, the raw material of the composition includes：Alumina ceramic powder, Premixed liquid, light trigger, dispersant and surfactant；The solute of the premixed liquid is selected from：Dimethylacrylate, methyl-prop One or more in acrylamide, 2-hydroxyethyl methacrylate and N-N ' methylene-bisacrylamides.The present invention is also provided A kind of utilization above-mentioned composition prepares the preparation method of aluminium oxide ceramics, and the preparation method is：Step one, prepare slurry： Ball milling after the mixing of alumina ceramic powder, premixed liquid, dispersant and surfactant, then mix with light trigger, obtain slurry；Step Rapid two, it is molded：The slurry Stereolithography, obtains base substrate；Step 3, drying and degreasing：Successively Jing is dry for the first time for the base substrate Dry and degreasing, obtains porous body；Step 4, infiltration：The porous body infiltrates in impregnating solution, obtains infiltration base substrate；Step 5th, post-process：Successively Jing is dried for second and sinters the infiltration base substrate, obtains alumina ceramic product.The skill that the present invention is provided In art scheme, ceramic body is prepared by Stereolithography method, shaping efficiency is high, product size high precision；By defatting step The optimization of parameter, skimming processes base substrate is indeformable, do not ftracture；By impregnation step, it is suppressed that the production of zirconia grains, Jing is electric Sem observation product structure, product microstructure is uniform；In solving prior art, it is mixed with zirconic aluminium oxide ceramics and there is knot The uneven technological deficiency of structure.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

1. a kind of composition, it is characterised in that the raw material of the composition includes：It is alumina ceramic powder, premixed liquid, light-initiated Agent, dispersant and surfactant；
The solute of the premixed liquid is selected from：Dimethylacrylate, Methacrylamide, 2-hydroxyethyl methacrylate and N- One or more in N ' methylene-bisacrylamides.
2. composition according to claim 1, it is characterised in that in terms of mass parts, the raw material of the composition includes：Oxygen Change 20~85 parts of aluminium ceramic powder, 10~70 parts of premixed liquid, 1~3 part of light trigger, 1~3 part of dispersant and surfactant 1 ~3 parts.
3. composition according to claim 1, it is characterised in that the alumina ceramic powder is α-Al2O3, the oxygen The purity for changing aluminium ceramic powder is more than 99%, and the particle diameter of the aluminium oxide ceramics is：0.1~0.5 μm.
4. composition according to claim 1, it is characterised in that the light trigger is selected from：BASF 184, BASF 819th, one or more in BASF 256, BASF 2959 and BASF 1173；
The dispersant is selected from：One kind in BYK-9076, Sodium Polyacrylate, ammonium polyacrylate and polyvinylpyrrolidone or It is various；
The surfactant is selected from：Silanes activating agent or coupling agent.
5. composition according to claim 1, it is characterised in that the solvent of the premixed liquid is selected from：Deionized water, glycerine And one or more in absolute ethyl alcohol；
In the premixed liquid, the mass concentration of solute is 20~85%.
6. the composition described in a kind of utilization claim 1 to 5 any one prepares the preparation method of aluminium oxide ceramics, its feature It is that the preparation method is：
Step one, prepare slurry：Alumina ceramic powder, premixed liquid, dispersant and surfactant mixing after ball milling, then with light Initiator mixes, and obtains slurry；
Step 2, shaping：The slurry Stereolithography, obtains base substrate；
Step 3, drying and degreasing：Successively Jing is dried for the first time and degreasing the base substrate, obtains porous body；
Step 4, infiltration：The porous body infiltrates in impregnating solution, obtains infiltration base substrate；
Step 5, post processing：Successively Jing is dried for second and sinters the infiltration base substrate, obtains alumina ceramic product.
7. preparation method according to claim 6, it is characterised in that the preparation method of the slurry is：
Solute is dissolved in solvent and stirs to obtain premixed liquid；
After alumina ceramic powder, ethanol and dispersant, first time ball milling obtains the first product；
After the mixing of first product, premixed liquid, dispersant and surfactant, second ball milling obtains the second product；
Mix with light trigger after the second product bubble removing, obtain slurry.
8. preparation method according to claim 6, it is characterised in that the impregnating solution is that the mixing of zirconates and yttrium salt is molten Liquid；
The zirconates is selected from：ZrOCl2·8H2O、Zr(NO3)4·5H2O and Zr (SO4)2·4H2One or more in O；
The yttrium salt is Y (NO3)3·6H2O or Y2(SO4)3·8H2O；
The time of the infiltration is 1~24h.
9. preparation method according to claim 6, it is characterised in that the method that the first time is dried is liquid dried And/or microwave drying, the liquid drier of the liquid dried is selected from：One kind in polyethylene glycol, ethanol and ethylene glycol or It is various；
The method of the degreasing is：Dried base substrate is first carried out after vacuum degreasing or atmosphere protection degreasing, then carry out air take off Fat, the porosity of the porous body is 40~60%；
The temperature being dried for described second is 60~150 DEG C, and the second dry time is 3~24h；
The method of the sintering is selected from：One or more in normal pressure-sintered, atmosphere sintering and HIP sintering.
10. preparation method according to claim 6, it is characterised in that the sweep speed of the Stereolithography is 1000 ~3000mm/s, the scan mode of the Stereolithography is X-Y, the sweep span of the Stereolithography is 0.1~ 0.5mm, a length of 365~405nm of light wave of the Stereolithography.
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CN113956025A (en) * 2021-11-17 2022-01-21 中国科学院金属研究所 Photocuring 3D printing impregnation reinforced ceramic core and preparation method thereof
CN113956025B (en) * 2021-11-17 2022-11-15 中国科学院金属研究所 Photocuring 3D printing impregnation reinforced ceramic core and preparation method thereof
CN114380583A (en) * 2022-01-26 2022-04-22 重庆恩辰新材料科技有限责任公司 Preparation method of ceramic material

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