CN117486588A - Preparation method for instant-firing high-purity alumina ceramic substrate - Google Patents
Preparation method for instant-firing high-purity alumina ceramic substrate Download PDFInfo
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- CN117486588A CN117486588A CN202311439160.1A CN202311439160A CN117486588A CN 117486588 A CN117486588 A CN 117486588A CN 202311439160 A CN202311439160 A CN 202311439160A CN 117486588 A CN117486588 A CN 117486588A
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- green body
- purity alumina
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000758 substrate Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000010304 firing Methods 0.000 title claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 83
- 239000006185 dispersion Substances 0.000 claims abstract description 79
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 230000035882 stress Effects 0.000 claims abstract description 24
- 239000003292 glue Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 230000001360 synchronised effect Effects 0.000 claims abstract description 9
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 24
- 238000007731 hot pressing Methods 0.000 claims description 21
- 238000005266 casting Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000004014 plasticizer Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 230000000007 visual effect Effects 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 description 8
- 238000000576 coating method Methods 0.000 description 5
- 238000003475 lamination Methods 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- 239000005341 toughened glass Substances 0.000 description 2
- WTFUTSCZYYCBAY-SXBRIOAWSA-N 6-[(E)-C-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-N-hydroxycarbonimidoyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C/C(=N/O)/C1=CC2=C(NC(O2)=O)C=C1 WTFUTSCZYYCBAY-SXBRIOAWSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
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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
- C04B35/111—Fine ceramics
- C04B35/117—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
-
- 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
- B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
- B28B17/02—Conditioning the material prior to shaping
- B28B17/026—Conditioning ceramic materials
-
- 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
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
- B28B3/025—Hot pressing, e.g. of ceramic materials
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention discloses a preparation method for an instant-firing high-purity alumina ceramic substrate, and belongs to the technical field of precise ceramic production and manufacturing processes. The preparation method for the instant-firing high-purity alumina ceramic substrate has relatively good dispersion effect and uniform volume density, and can effectively reduce the residual stress of the green body in the production process. The preparation method comprises the steps of preparing slurry in a synchronous circulation and double dispersion way, preparing a green body through hot press molding, and eliminating residual stress in the green body through aging treatmentAnd the steps of glue discharging and sintering to prepare the instant-heating type high-purity alumina ceramic substrate, wherein when the slurry is prepared by synchronous circulation and double dispersion, an ultrasonic dispersion circulation system arranged on mechanical dispersion equipment and the mechanical dispersion equipment synchronously circulate, and materials added into the mechanical dispersion equipment are subjected to double dispersion to obtain fully dispersed slurry, and the prepared instant-heating type high-purity alumina ceramic substrate has the warp degree smaller than 0.1mm, the flexural strength larger than or equal to 550Mpa and the volume density larger than or equal to 3.88g/cm 3 And no cracking and breakage.
Description
Technical Field
The invention relates to a preparation method, in particular to a preparation method for an instant-firing high-purity alumina ceramic substrate, belonging to the technical field of precise ceramic production and manufacturing processes.
Background
According to the different purities of alumina, the alumina substrate can be divided into 90 porcelain, 95 porcelain, 96 porcelain, 99 porcelain and the like, and the ceramic substrate with the purity of alumina being more than or equal to 99.6% is called as a high-purity alumina ceramic substrate; the high-purity alumina ceramic substrate is widely applied to high-frequency and high-power thin film integrated circuits because of the characteristics of excellent electrical insulation, high mechanical strength, low surface roughness, excellent dielectric property, good metal adhesion, thermal shock resistance and the like.
The instant-firing alumina ceramic substrate, i.e. the substrate which can be directly used without any processing after sintering; therefore, the preparation requirements are more strict than those of the fine grinding and polishing substrates, and high strength, extremely low warpage, no cracking and breakage, excellent surface state and the like are required. The cast green body quality is a key factor in determining whether a high quality sintered body can be obtained, and uneven density and residual stress of the green body can directly lead to warping, cracking, breakage, etc. of the sintered product.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the preparation method for the instant-firing high-purity alumina ceramic substrate has relatively good dispersion effect and uniform volume density, and can effectively reduce the residual stress of the green body in the production process.
The technical scheme adopted for solving the technical problems is as follows: a process for preparing the high-purity alumina ceramic substrate used for instant baking includes such steps as preparing slurry by synchronous circulation and double dispersion, preparing green body by hot press shaping, ageing to eliminate residual stress in green body, removing adhesive, sintering to obtain instant baking high-purity alumina ceramic substrate,
wherein, when the slurry is prepared by synchronous circulation and double dispersion, the ultrasonic dispersion circulation system arranged on the mechanical dispersion equipment and the mechanical dispersion equipment synchronously and circularly operate, the materials added into the mechanical dispersion equipment are subjected to double dispersion to obtain fully dispersed slurry,
when the aging treatment is carried out to eliminate the residual stress in the green body, the green body is subjected to ultrasonic oscillation, resistance wire heating, pressurizing and quenching treatment and then naturally standing, so as to obtain the green body with the residual stress eliminated fully; the cast green body is first hot pressed for bulk density and fracture toughness enhancement before the aging process eliminates residual stress in the green body.
The prepared instant-firing high-purity alumina ceramic substrate has the warp less than 0.1mm, the flexural strength more than or equal to 550Mpa and the volume density more than or equal to 3.88g/cm 3 And has no cracking and breakage and excellent surface state.
The preferable mode of the scheme is that the device of the hot pressing technology with the improved volume density and fracture toughness comprises a hot pressing die, a hydraulic press, a hydraulic pump, a heating device, a pressure gauge and a thermometer; during hot pressing, a hot pressing die is used as a green body to position opposite sides; the hydraulic press adopts unidirectional pressure application, and the pressure range is 0-200 Mpa; the inner diameter of the hydraulic pump is 150mm, and the precision is 5Mpa; the heating device is a bottom plate heating resistor, and the temperature range is 0-150 ℃.
Further, when the green body for eliminating the internal residual stress is subjected to glue discharging and sintering, the glue discharging temperature is 450 ℃ and the heat preservation time is 5 hours; sintering is high-temperature sintering, the sintering temperature is 1500-1580 ℃, and the sintering time is 4-6 h.
The preferable mode of the scheme is that the mechanical dispersing equipment is a vertical stirring mill, and the materials added into the vertical stirring mill comprise 65-70% by weight of high-purity alumina powder, 0.1-0.15% by weight of sintering auxiliary agent, 0.2-0.3% by weight of dispersing agent and 25-30% by weight of organic solvent, and the vertical stirring mill and an ultrasonic dispersion circulation system are simultaneously started to synchronously and circularly operate to perform double dispersion during dispersion to prepare the ceramic dispersion slurry.
Further, 15-20% of binder, 10-15% of plasticizer and 60-70% of organic solvent are mixed in a sol machine while preparing ceramic dispersion slurry, the mixture is stirred and dispersed at high speed and is kept stand for 12 hours to prepare pre-sol, finally, the ceramic dispersion slurry and the pre-sol are mixed and ball-milled to obtain mixed ceramic slurry,
the preferable mode of the scheme is that the high-purity alumina powder has the particle diameter D 50 Alpha-alumina with purity of not less than 99.9% and 0.4-0.5 um; the sintering aid has a particle diameter D 50 Magnesium oxide with particle diameter D between 0.3 and 0.4um 50 Mixed powder of yttrium oxide with the purity of 0.2-0.3 um, wherein the purity of the magnesium oxide and the purity of the yttrium oxide are all analytically pure; the dispersing agent is at least one of triethanolamine, polyacrylamide and polyethyleneimine with analytically pure purity; the binder is analytically pure polyvinyl butyral; the plasticizer is one of dibutyl phthalate and dioctyl phthalate with analytical purity; the organic solvent is at least one of toluene, acetone, xylene and isopropanol with industrial grade purity.
Further, the mixed ceramic slurry obtained by rolling ball milling is subjected to filtering treatment, vacuum defoamation, tape casting molding and drying to obtain a tape casting green body.
The preferable mode of the scheme is that when the slurry is prepared by adopting a vertical stirring mill and an ultrasonic dispersion circulation system for synchronous circulation and double dispersion, the dispersion time is 1-2 h, and the particle diameter D of the slurry after dispersion 50 0.35-0.45 um; when a sol machine is adopted to prepare the pre-sol, the stirring time is 6-8 h, and the viscosity of the prepared pre-sol is 1000-1500 cps; ball milling time is 10-15 h when a rolling ball mill is used as a glue mixing device to prepare glue mixing slurry, and glue mixing is carried outThe viscosity of the slurry is 500-1000 cps; when the vacuum deaerating machine is adopted to deaerate the mixed ceramic slurry of deaerating equipment, the deaerating time is 2-3 h, and the viscosity of the deaerated slurry is 15000-20000 cps.
Further, the materials added into the vertical stirring mill are sent into the grinding cavity through the upper part of the cylinder body by using a transmission device, the lower part of the cylinder body is externally connected with a slurry circulating conveying pipeline and a feed pump device, and the upper part of the cylinder body is connected in parallel to form a closed circulating dispersion system; the ultrasonic dispersion circulation system is arranged on the middle section of the circulation conveying pipe of the vertical stirring mill.
The preferable mode of the scheme is that the ultrasonic dispersion circulation system comprises an ultrasonic dispersion chamber, a cooling water device, a slurry inlet and outlet passage port, a circulation pipeline passage, an ultrasonic interface, a feed pump device, a flowmeter and a visual window; the ultrasonic dispersion chamber is a place where the slurry is subjected to ultrasonic dispersion and acoustic cavitation effects; the cooling water device is used for controlling the temperature of the slurry and preventing the quality of the slurry from being influenced by the overhigh temperature; the circulating pipeline passage is a place for slurry conveying and circulating; the ultrasonic interfaces are ultrasonic generators distributed around the dispersion chamber; the feed pump device is a circulating power device for providing solid-liquid slurry; the flowmeter displays the flow velocity and flow of the solid-liquid slurry in the circulation path of the dispersion circulation system; the visual window is used for observing the dispersion state of the slurry dispersion chamber.
The beneficial effects of the invention are as follows: according to the technical scheme, the ultrasonic dispersion circulation system is increased on the basis of mechanical dispersion, the ultrasonic dispersion circulation system is participated in to perform synchronous circulation double-dispersion operation while mechanical dispersion, materials in mechanical equipment are dispersed to achieve the purpose of improving dispersion effect, meanwhile, the volume density and homogenization of a green body are improved through hot press molding in the process of preparing the green body, and then the purpose of effectively reducing the residual stress of the green body in the production process is achieved through ageing treatment to eliminate the residual stress of the green body.
Drawings
FIG. 1 is a 10K-fold SEM image of the green surface of a green body involved in a method of making a high purity alumina ceramic substrate for use in accordance with the present invention;
FIG. 2 is a 5K-fold cross-sectional SEM image of a green body involved in a method of preparing a high purity alumina ceramic substrate for use in accordance with the present invention;
FIG. 3 is a 5K-fold SEM image of the surface of a sintered body of the present invention for use in a method for producing a high purity alumina ceramic substrate;
FIG. 4 is a 5K-fold cross-sectional SEM image of a sintered body of the present invention for use in a method for producing a high purity alumina ceramic substrate.
Detailed Description
From the aspects of improving the dispersion effect of ceramic slurry, eliminating the residual stress of the green body and the uneven volume density, as shown in fig. 1, 2, 3 and 4, the invention provides a preparation method for the instant firing type high-purity alumina ceramic substrate, which has relatively good dispersion effect and even volume density and can effectively reduce the residual stress of the green body in the production process. The preparation method comprises the following steps: 1. the slurry is dispersed, and a group of ultrasonic dispersion circulation systems are additionally arranged at the vertical mixer, so that the mechanical dispersion and the ultrasonic dispersion are synchronously and circularly carried out, and the optimal dispersion effect and efficiency are achieved; 2. the green body adopts a hot pressing process, so that the volume density and fracture toughness of the green body are improved; 3. aging the hot-pressed green body to eliminate residual stress in the green body, and performing ultrasonic oscillation, resistance wire heating, pressurizing and quenching treatment; finally, the adhesive is discharged and sintered, and the ready-to-burn high-purity alumina ceramic substrate with low warpage, high mechanical strength, no cracking and breakage and excellent surface state is prepared.
The scheme comprises the following specific implementation steps:
a) A group of ultrasonic dispersion circulation systems are additionally arranged on the vertical mixer, so that mechanical dispersion and ultrasonic dispersion are synchronously and circularly carried out; placing 65-70% by weight of high-purity alumina powder, 0.1-0.15% by weight of sintering aid, 0.2-0.3% by weight of dispersing agent and 25-30% by weight of organic solvent into a vertical mixer, and starting a mechanical stirring and ultrasonic dispersion circulation system to obtain ceramic dispersion slurry;
b) Preparing a pre-sol: mixing 15-20% of binder, 10-15% of plasticizer and 60-70% of organic solvent, stirring at high speed, dispersing and standing for 12h to obtain pre-sol;
c) And (3) mixing: mixing and rolling ball milling the ceramic dispersion slurry and the pre-sol to obtain mixed ceramic slurry;
d) Filtering, vacuum defoaming, casting, forming and drying the mixed ceramic slurry to obtain a casting green body;
e) The cast green body is subjected to a hot pressing process, so that the volume density and fracture toughness of the green body are improved;
f) And (3) performing ageing treatment after punching the hot-pressed green body, performing ultrasonic oscillation, heating, pressurizing and quenching treatment by using a resistance wire, naturally standing for 12 hours, and starting glue discharging and sintering to obtain the ready-to-burn high-purity alumina substrate.
Particle diameter D of the main phase material high-purity alumina powder 50 Alpha-alumina with the purity of 0.4-0.5 um, wherein the purity of the high-purity alumina powder is more than or equal to 99.9 percent; the sintering aid has a particle diameter D 50 Magnesium oxide and yttrium oxide powder with the purity of 0.3-0.4 and 0.2-0.3 um respectively, wherein the purity of the magnesium oxide and the purity of the yttrium oxide are analytically pure; the dispersing agent is at least one of triethanolamine, polyacrylamide and polyethyleneimine with analytically pure purity; the binder is analytically pure polyvinyl butyral; the plasticizer is one of dibutyl phthalate and dioctyl phthalate with analytically pure purity; the organic solvent is at least one of toluene, acetone, xylene and isopropanol with industrial-grade purity;
the dispersing equipment of the ceramic slurry is a vertical stirring mill and an ultrasonic dispersion circulating system, the dispersing time is 1-2 h, and the particle size D of the slurry after dispersion 50 About 0.35 to 0.45um; the pre-sol preparation equipment is a sol machine, the stirring time is 6-8 h, and the viscosity of the pre-sol is 1000-1500 cps; the glue mixing equipment is a rolling ball mill, the ball milling time is 10-15 h, and the viscosity of the glue mixing slurry is 500-1000 cps; the defoaming equipment is a vacuum defoaming machine, the defoaming time is 2-3 h, and the viscosity of the defoamed slurry is 15000-20000 cps;
the vertical mixer is characterized in that materials are sent into a grinding cavity through a transmission device at the upper part of a cylinder, the lower part of the cylinder is externally connected with a slurry circulating conveying pipeline and a feed pump device, and a closed circulating dispersion system is formed at the upper part of the cylinder; a group of ultrasonic dispersion circulation systems are additionally arranged at the middle section of a circulation conveying pipe of the vertical stirring mill, and the ultrasonic dispersion circulation systems comprise: the device comprises an ultrasonic dispersion chamber, a cooling water device, a slurry inlet and outlet channel port, a circulating pipeline passage, an ultrasonic interface, a feed pump device, a flowmeter and a visual window;
in the ultrasonic dispersion circulation system, an ultrasonic dispersion chamber is a place where ultrasonic dispersion and acoustic cavitation effect of slurry occur; the cooling water device is used for controlling the temperature of the slurry and preventing the quality of the slurry from being influenced by the excessive temperature; the circulating pipeline passage is a place for slurry conveying and circulating; the ultrasonic interfaces are ultrasonic generators distributed around the dispersion chamber; the feeding pump device is a circulating power device for providing solid-liquid slurry; the flowmeter displays the flow velocity and the flow rate of the solid-liquid slurry in the circulation path of the dispersion circulation system; the visual window is used for observing the dispersion condition of the slurry dispersion chamber;
the hot pressing process comprises the following steps: the device comprises a hot-pressing die, a hydraulic press, a hydraulic pump, a heating device, a pressure gauge and a thermometer; the hot press die is used for positioning opposite sides of the green body, and preferably, the thickness of the green body ranges from 0.12 mm to 1.0mm by taking 4 inches as an example; the hydraulic press adopts unidirectional pressure application, and the pressure range is 0-200 Mpa; the inner diameter of the hydraulic pump is 150mm, and the precision is 5Mpa; the heating device is a bottom plate heating resistor, and the temperature range is 0-150 ℃;
the aging treatment process is characterized in that the hot-pressed green body is subjected to ultrasonic oscillation, resistance wire heating, pressurizing, quenching and standing treatment, so that the residual stress in the green body is fully eliminated;
the glue discharging process is characterized in that the glue discharging temperature is 450 ℃, and the heat preservation time is 5 hours;
the high-temperature sintering is carried out at 1500-1580 ℃ for 4-6 h;
the instant-heating type high-purity alumina ceramic substrate is characterized in that: the warpage is less than 0.1mm, the flexural strength is more than or equal to 550Mpa, and the volume density is more than or equal to 3.88g/cm 3 The surface state is excellent without cracking and breakage.
The invention has the beneficial effects that:
the invention provides a preparation method of an instant firing type high-purity alumina ceramic substrate, which provides 3 treatment methods from the angles of improving the dispersion effect and efficiency of ceramic slurry, uneven volume density of a green body, eliminating residual stress of the green body and the like:
1) A group of ultrasonic dispersion circulation systems are additionally arranged during mechanical ball milling dispersion, so that ultrasonic dispersion and mechanical dispersion are synchronously and circularly carried out, and the dispersion effect and efficiency of ceramic slurry are improved;
2) Adopting a hot pressing process, and carrying out heat preservation and pressure maintaining at a temperature above the glass transition temperature of the binder to rearrange powder particles in the green body, fill gaps, ensure more uniform particle distribution and improve the volume density and fracture toughness of the green body;
3) And an aging treatment process is adopted for the hot-pressed green body, so that the residual stress and uneven stress distribution of the green body are eliminated, a sintered body with excellent flatness is prepared, the mechanical strength of the sintered body is improved, the early exposure of partial defects of a product is accelerated, defective products are screened out in advance, and the product yield is improved.
The technical scheme of the application is further described by the following specific examples:
the preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
the method comprises the steps of placing 65-70% by weight of high-purity alpha-alumina powder, 0.1-0.15% by weight of sintering aid, 0.2-0.3% by weight of dispersing agent and 25-30% by weight of organic solvent into a vertical mixer, starting a feed pump to circularly stir and disperse for 2-4 h to obtain the particle size D 50 Ceramic dispersion slurry of 0.35-0.45 um;
mixing 15-20% of binder, 10-15% of plasticizer and 60-70% of organic solvent, stirring at high speed for 6-8 h by a high-speed stirrer, and naturally standing for 12h to obtain a pre-sol with the viscosity of 1000-1500 cps;
the dispersion slurry and the pre-sol were mixed at a ratio of 10:1.2, ball milling for 10 to 15 hours by a rolling ball mill to prepare mixed ceramic slurry with the viscosity of 500 to 1000cps; then nitrogen is introduced into the ball milling tank for discharging, and vacuum defoaming treatment is carried out by a vacuum defoaming machine, so as to obtain casting slurry with the viscosity of 15000-20000 cps; and then carrying out casting molding by a casting machine to obtain a casting green body with the thickness of preferably 0.4-0.6 mm.
Example 1
The preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
1) Preferably, taking 4 inches as an example, cutting a casting green body with the thickness of 0.4-0.6 mm into a 4-inch-sized green body sheet, then carrying out a powder coating process, and naturally standing for 12 hours for waiting to burn after lamination placement;
2) Discharging glue from the green sheet through a box furnace at 450 ℃, and preserving heat for 5 hours; and then sintering at a high temperature of 1500-1580 ℃ in a high temperature furnace, and preserving heat for 4-6 hours to obtain the ready-to-burn high-purity alumina ceramic substrate with the thickness specification of 4 inches and 0.12-1.0 mm.
Example 2
The preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
1) Carrying out hot-pressing process treatment on the cast green body, preferably taking 4 inches as an example, cutting the green body into 125 mm-sized green body pieces, positioning the green body pieces opposite sides of a 125 mm-sized hot-pressing die, setting the pressure to 100Mpa, the temperature to 80 ℃, and the heat preservation and pressure maintaining time to 5 minutes to obtain the green body pieces with excellent flatness; cutting the green sheet to 120mm in size, then carrying out powder coating process, and naturally standing for 12 hours for waiting to burn after lamination placement;
2) Discharging glue from the green sheet through a box furnace at 450 ℃, and preserving heat for 5 hours; and then sintering at a high temperature of 1500-1580 ℃ in a high temperature furnace, and preserving heat for 4-6 hours to obtain the ready-to-burn high-purity alumina ceramic substrate with the thickness specification of 4 inches and 0.12-1.0 mm.
Example 3
The preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
1) A group of ultrasonic dispersion circulation system is additionally arranged at the middle section of a circulation conveying pipe of the vertical mixer, so that mechanical dispersion and ultrasonic dispersion are synchronously carried out, and a feed pump is started to circularly stir and disperse for 1-2 hours, thus obtaining the particle sizeD 50 Ceramic dispersion slurry of 0.3-0.4 um; mixing ceramic dispersion slurry with pre-sol, ball milling, vacuum defoaming to obtain casting slurry, and casting to obtain casting green body with thickness of 0.4-0.6 mm;
2) Preferably, taking 4 inches as an example, cutting the casting green body into 4 inches-sized green body pieces, then carrying out a powder coating process, and naturally standing for 12 hours for waiting to burn after lamination placement;
3) Discharging glue from the green sheet through a box furnace at 450 ℃, and preserving heat for 5 hours; and then sintering at a high temperature of 1500-1580 ℃ in a high temperature furnace, and preserving heat for 4-6 hours to obtain the ready-to-burn high-purity alumina ceramic substrate with the thickness specification of 4 inches and 0.12-1.0 mm.
Example 4
The preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
1) A group of ultrasonic dispersion circulation system is additionally arranged at the middle section of a circulation conveying pipe of the vertical mixer, so that mechanical dispersion and ultrasonic dispersion are synchronously carried out, and a feed pump is started to circularly stir and disperse for 1-2 hours, thus obtaining the particle size D 50 Ceramic dispersion slurry of 0.3-0.4 um; mixing ceramic dispersion slurry with pre-sol, ball milling, vacuum defoaming to obtain casting slurry, and casting to obtain casting green body with thickness of 0.4-0.6 mm;
2) Carrying out hot-pressing process treatment on the cast green body, preferably taking 4 inches as an example, cutting the green body into 125 mm-sized green body pieces, positioning the green body pieces opposite sides of a hot-pressing die with the size of 125mm, setting the pressure to 100Mpa, the temperature to 80 ℃, and the heat preservation and pressure maintaining time to 5 minutes to obtain the green body pieces with excellent flatness; cutting the green sheet to 120mm in size, then carrying out powder coating process, and naturally standing for 12 hours for waiting to burn after lamination placement;
3) Discharging glue from the green sheet through a box furnace at 450 ℃, and preserving heat for 5 hours; and then sintering at a high temperature of 1500-1580 ℃ in a high temperature furnace, and preserving heat for 4-6 hours to obtain the ready-to-burn high-purity alumina ceramic substrate with the thickness specification of 4 inches and 0.12-1.0 mm.
Example 5
The preparation method of the instant-firing high-purity alumina ceramic substrate comprises the following specific steps:
1) A group of ultrasonic dispersion circulation system is additionally arranged at the middle section of a circulation conveying pipe of the vertical mixer, so that mechanical dispersion and ultrasonic dispersion are synchronously and circularly carried out, and a feed pump is started to circularly stir and disperse for 1-2 hours, thus obtaining the particle size D 50 Ceramic dispersion slurry of 0.3-0.4 um; mixing ceramic dispersion slurry with pre-sol, ball milling, vacuum defoaming to obtain casting slurry, and casting to obtain casting green body with thickness of 0.4-0.6 mm;
2) Carrying out hot-pressing process treatment on the cast green body, preferably taking 4 inches as an example, cutting the green body into 125 mm-sized green body pieces, positioning the green body pieces opposite sides of a hot-pressing die with the size of 125mm, setting the pressure to 100Mpa, the temperature to 80 ℃, and the heat preservation and pressure maintaining time to 5 minutes to obtain the green body pieces with excellent flatness; then cutting the green sheet to a size of 120 x 120 mm;
3) Aging the green body after the hot pressing treatment, vacuum-packaging each green body piece by using a plastic packaging film, placing the green body piece in an ultrasonic dispersion instrument, eliminating partial residual stress of the green body, setting parameters, and controlling the frequency to be 40Hz and the temperature to be 40 ℃ for 30min; taking out the green body, orderly stacking 30-40 layers, separating each layer by using a PET film, pressing a piece of toughened glass with the weight of 200g on the top layer, then placing the toughened glass in a resistance wire heating furnace, setting the slow heating speed to be 0.5 ℃/min, and keeping the temperature at 80 ℃ for 4 hours; finally, rapidly placing the green sheet in the heating furnace in a vacuum condensing chamber for quenching treatment; then carrying out powder coating process, and naturally standing for 12 hours for waiting to burn after lamination placement;
4) Discharging glue from the green sheet through a box furnace at 450 ℃, and preserving heat for 5 hours; and sintering at 1500-1580deg.C for 4-6 h to obtain 4-inch and 0.12-1.0 mm thick high-purity aluminum oxide ceramic substrate, with the appearance of green body and sintered body shown in the figure.
Table 1 shows the properties of the as-fired high-purity alumina ceramic substrates prepared in examples 1 to 5
| Numbering device | Substrate size (mm) | Roughness (um) | Bulk Density (g/cm) 3 ) | Flexural strength (Mpa) | Warp degree (mm) |
| Example 1 | 4 inch | A：0.12～0.16 | 3.75 | 250～300 | 0.8 |
| Example 2 | 4 inch | A：0.08～0.12 | 3.82 | 350～400 | 0.3 |
| Example 3 | 4 inch | A：0.1～0.14 | 3.78 | 280～300 | 0.5 |
| Example 4 | 4 inch | A：0.06～0.1 | 3.88 | 450～500 | 0.15 |
| Example 5 | 4 inch | A：0.04～0.08 | 3.92 | 550～600 | 0.08 |
Claims (10)
1. The preparation method for the instant-firing high-purity alumina ceramic substrate is characterized by comprising the following steps of: the preparation method comprises the steps of preparing slurry in a synchronous circulation and double dispersion way, preparing a green body through hot press molding, eliminating residual stress in the green body through aging treatment, discharging glue, sintering to prepare the ready-to-burn high-purity alumina ceramic substrate,
wherein, when the slurry is prepared by synchronous circulation and double dispersion, the ultrasonic dispersion circulation system arranged on the mechanical dispersion equipment and the mechanical dispersion equipment synchronously and circularly operate, the materials added into the mechanical dispersion equipment are subjected to double dispersion to obtain fully dispersed slurry,
when the aging treatment is carried out to eliminate the residual stress in the green body, the green body is subjected to ultrasonic oscillation, resistance wire heating, pressurizing and quenching treatment and then naturally standing, so as to obtain the green body with the residual stress eliminated fully; before the aging treatment eliminates the residual stress in the green body, the cast green body is subjected to hot pressing with improved volume density and fracture toughness,
the prepared instant-firing high-purity alumina ceramic substrate has the warp less than 0.1mm, the flexural strength more than or equal to 550Mpa and the volume density more than or equal to 3.88g/cm 3 And has no cracking and breakage and excellent surface state.
2. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 1, wherein: the device for the hot-pressing process with the improved volume density and fracture toughness comprises a hot-pressing die, a hydraulic press, a hydraulic pump, a heating device, a pressure gauge and a thermometer; during hot pressing, a hot pressing die is used as a green body to position opposite sides; the hydraulic press adopts unidirectional pressure application, and the pressure range is 0-200 Mpa; the inner diameter of the hydraulic pump is 150mm, and the precision is 5Mpa; the heating device is a bottom plate heating resistor, and the temperature range is 0-150 ℃.
3. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 2, wherein: when the green body with the internal residual stress eliminated is subjected to glue discharging and sintering, the glue discharging temperature is 450 ℃ and the heat preservation time is 5 hours; sintering is high-temperature sintering, the sintering temperature is 1500-1580 ℃, and the sintering time is 4-6 h.
4. A method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 1, 2 or 3, characterized in that: the mechanical dispersion equipment is a vertical stirring mill, and the materials added into the vertical stirring mill comprise 65-70% by weight of high-purity alumina powder, 0.1-0.15% by weight of sintering aid, 0.2-0.3% by weight of dispersing agent and 25-30% by weight of organic solvent, and the vertical stirring mill and an ultrasonic dispersion circulation system are simultaneously started to synchronously and circularly operate for double dispersion during dispersion to prepare the ceramic dispersion slurry.
5. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 4, wherein: the preparation method comprises the steps of mixing 15-20% by weight of binder, 10-15% by weight of plasticizer and 60-70% by weight of organic solvent in a sol machine while preparing ceramic dispersion slurry, stirring and dispersing at high speed, standing for 12 hours to prepare pre-sol, and finally mixing and rolling the ceramic dispersion slurry and the pre-sol to obtain mixed ceramic slurry.
6. Root of Chinese characterThe method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 5, wherein: the high-purity alumina powder has the particle diameter D 50 Alpha-alumina with purity of not less than 99.9% and 0.4-0.5 um; the sintering aid has a particle diameter D 50 Magnesium oxide with particle diameter D between 0.3 and 0.4um 50 Mixed powder of yttrium oxide with the purity of 0.2-0.3 um, wherein the purity of the magnesium oxide and the purity of the yttrium oxide are all analytically pure; the dispersing agent is at least one of triethanolamine, polyacrylamide and polyethyleneimine with analytically pure purity; the binder is analytically pure polyvinyl butyral; the plasticizer is one of dibutyl phthalate and dioctyl phthalate with analytical purity; the organic solvent is at least one of toluene, acetone, xylene and isopropanol with industrial grade purity.
7. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 6, wherein: and filtering, vacuum defoaming, casting and drying the mixed ceramic slurry obtained by rolling ball milling to obtain a casting green body.
8. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 7, wherein: when the slurry is prepared by adopting a vertical stirring mill and an ultrasonic dispersion circulation system for synchronous circulation and double dispersion, the dispersion time is 1-2 h, and the particle size D of the slurry after dispersion 50 0.35-0.45 um; when a sol machine is adopted to prepare the pre-sol, the stirring time is 6-8 h, and the viscosity of the prepared pre-sol is 1000-1500 cps; the ball milling time is 10-15 h when the rolling ball mill is used as a glue mixing device to prepare glue mixing slurry, and the viscosity of the glue mixing slurry is 500-1000 cps; when the vacuum deaerating machine is adopted to deaerate the mixed ceramic slurry of deaerating equipment, the deaerating time is 2-3 h, and the viscosity of the deaerated slurry is 15000-20000 cps.
9. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 8, wherein: the materials added into the vertical stirring mill are sent into the grinding cavity through the upper part of the cylinder body by using a transmission device, the lower part of the cylinder body is externally connected with a slurry circulating conveying pipeline and a feed pump device, and the materials are connected with the upper part of the cylinder body in parallel to form a closed circulating dispersion system; the ultrasonic dispersion circulation system is arranged on the middle section of the circulation conveying pipe of the vertical stirring mill.
10. The method for producing a ready-to-burn high purity alumina ceramic substrate according to claim 9, wherein: the ultrasonic dispersion circulation system comprises an ultrasonic dispersion chamber, a cooling water device, a slurry inlet and outlet port, a circulation pipeline passage, an ultrasonic interface, a feed pump device, a flowmeter and a visual window; the ultrasonic dispersion chamber is a place where the slurry is subjected to ultrasonic dispersion and acoustic cavitation effects; the cooling water device is used for controlling the temperature of the slurry and preventing the quality of the slurry from being influenced by the overhigh temperature; the circulating pipeline passage is a place for slurry conveying and circulating; the ultrasonic interfaces are ultrasonic generators distributed around the dispersion chamber; the feed pump device is a circulating power device for providing solid-liquid slurry; the flowmeter displays the flow velocity and flow of the solid-liquid slurry in the circulation path of the dispersion circulation system; the visual window is used for observing the dispersion state of the slurry dispersion chamber.
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