CN115557777A - Preparation method of spontaneous solidification formed alumina ceramic material and ceramic substrate - Google Patents
Preparation method of spontaneous solidification formed alumina ceramic material and ceramic substrate Download PDFInfo
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- CN115557777A CN115557777A CN202211223046.0A CN202211223046A CN115557777A CN 115557777 A CN115557777 A CN 115557777A CN 202211223046 A CN202211223046 A CN 202211223046A CN 115557777 A CN115557777 A CN 115557777A
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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 61
- 239000000758 substrate Substances 0.000 title claims abstract description 52
- 238000007711 solidification Methods 0.000 title claims abstract description 25
- 230000008023 solidification Effects 0.000 title claims abstract description 25
- 230000002269 spontaneous effect Effects 0.000 title claims abstract description 25
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000002002 slurry Substances 0.000 claims abstract description 52
- 239000001509 sodium citrate Substances 0.000 claims abstract description 27
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000003349 gelling agent Substances 0.000 claims abstract description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 29
- 238000000498 ball milling Methods 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 18
- 239000000499 gel Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000741 silica gel Substances 0.000 claims description 15
- 229910002027 silica gel Inorganic materials 0.000 claims description 15
- 238000000465 moulding Methods 0.000 claims description 13
- 238000010304 firing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims 1
- 239000003566 sealing material Substances 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 11
- 239000001993 wax Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000000429 assembly Methods 0.000 description 3
- 230000000712 assembly Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- -1 ammonium carboxylate Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical group [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
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- 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
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- 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
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/34—Moulds, cores, or mandrels of special material, e.g. destructible 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
- 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
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Abstract
The invention relates to a ceramic material, in particular to a method for preparing a self-solidifying and forming alumina ceramic material and a ceramic substrate. The alumina ceramic material formed by spontaneous solidification comprises alumina powder, a gelling agent, a dispersing agent and a defoaming agent; the gel is ISOBAM104, and the content of the gel is 0.3-0.5%; the dispersant is sodium citrate, and the content of the dispersant is 0.1-0.3%; the content of the defoaming agent is not more than 0.1%; the rest is alumina powder. The alumina ceramic material formed by spontaneous solidification provided by the invention does not need expensive equipment, and the shape and the thickness of the prepared substrate are controllable. The dispersant sodium citrate added in the spontaneous solidification process plays a good role in dispersion, pH does not need to be adjusted in the slurry, the content of the additive in the whole system is low, and the prepared ceramic substrate has high volume density and high breaking strength.
Description
Technical Field
The invention relates to a ceramic material, in particular to a method for preparing a self-solidifying and forming alumina ceramic material and a ceramic substrate.
Background
The alumina ceramic substrate is widely applied to solar panel assemblies, aerospace and military electronic assemblies, intelligent power assemblies and high-power semiconductor modules due to high strength, high mechanical stress, high thermal conductivity, high insulativity and corrosion resistance. The alumina substrate on the market at present is mainly a 96 alumina substrate, and since the substrate with high alumina content has higher thermal conductivity and bending strength, in order to realize low loss, the alumina substrate with high purity (more than 99.9%) needs to be prepared.
The preparation method of the high-purity alumina ceramic substrate mainly comprises dry pressing molding, injection molding and tape casting molding. The large-size ceramic substrate prepared by dry pressing is easy to crack, deform and other defects; more organic additives are added in the injection molding process, so that the performance of the ceramic substrate is influenced to a certain extent; expensive casting machines are required for casting, and the used additives have certain toxicity, harm to human health and damage to the environment.
The spontaneous solidification molding is developed after dry pressing molding, injection molding and tape casting molding and is a net size molding process. Isodam is used as a gel, a small amount of additive is added to prepare high-solid-phase-content slurry with good fluidity, and the alumina ceramic substrate is prepared by spontaneous solidification and molding. Generally, a dispersant is required to be added into alumina powder, the dispersant is ammonium citrate, and the pH of the slurry is adjusted by adding alkali, so that the strength of the prepared alumina ceramic is not high. The problems of cracking, warping, difficult demoulding and the like exist in the gel curing process.
Disclosure of Invention
In order to solve the problems, the invention provides a self-solidifying and forming alumina ceramic material which is used for preparing a substrate, has controllable shape and thickness, is not easy to crack and warp and is easy to demould, and the specific technical scheme is as follows:
the alumina ceramic material formed by spontaneous solidification comprises alumina powder, a gelling agent, a dispersing agent and a defoaming agent; the gel is ISOBAM104, and the content of the gel is 0.3-0.5%; the dispersant is sodium citrate, and the content of the dispersant is 0.1-0.3%; the content of the defoaming agent is not more than 0.1%; the remainder is alumina powder.
The alumina ceramic substrate is prepared by spontaneous solidification by taking ISOBAM104 as a gelling agent and sodium citrate as a dispersing agent.
Preferably, the addition amount of the gel ISOBAM104 is 0.3-0.5%, and the addition amount of the sodium citrate is 0.1-0.3%.
Preferably, the preparation method of the alumina ceramic substrate comprises the following steps:
(1) Adding ISOBAM104 and sodium citrate into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2), adding 0.1wt% of defoaming agent, and continuing ball milling;
(4) Pouring the slurry obtained in the step (3) into a mold coated with a release agent, vibrating to exhaust, and flattening into a substrate blank;
(5) Sealing the substrate blank in the step (4), standing, solidifying and molding;
(6) Putting the blank body obtained in the step (5) and the mould into an oven for drying;
(7) Demoulding, wherein the maximum firing temperature at one time is 1150-1250 ℃;
(8) Polishing, wherein the secondary maximum firing temperature is 1580-1610 ℃.
Preferably, the fineness of the alumina powder in the step (2) is 0.4-0.6 μm.
Preferably, the mold in the step (4) is a silica gel mold, and the release agent is glycerol; the silica gel mold is sealed on a glass plate by paraffin, and the softening temperature of the paraffin is 40-60 ℃.
Preferably, the material used for sealing in the step (5) is one or two of paper or a porous plate.
Preferably, the antifoaming agent in step (3) is NXZ.
Preferably, the oven drying temperature curve in the step (6) is 8-16h at 30 ℃, 10-24h at 60 ℃, 5-8h at 80 ℃ and 2h at 100 ℃.
Preferably, the volume density of the ceramic substrate is 3.9 to 3.92g/cm 3 The flexural strength is 269-337 MPa.
Compared with the prior art, the invention has the following beneficial effects:
the alumina ceramic material formed by spontaneous solidification provided by the invention does not need expensive equipment, and the shape and the thickness of the prepared substrate are controllable. The dispersant sodium citrate added in the spontaneous solidification process plays a good role in dispersion, the pH does not need to be adjusted in the slurry, the content of the additive in the whole system is low, and the prepared ceramic substrate has high volume density and high breaking strength.
The used mold is made of silica gel, the glycerol is smeared to play a role of a mold release agent, and the silica gel mold is soft and cannot move in a spontaneous solidification process and can generate buckling deformation in a drying process of a substrate blank. Because the used low-temperature wax is put into the oven to be heated to more than 60 ℃, the glass plate can be separated from the silica gel grinding tool, and the blank also has certain strength.
Paper or a porous plate is adopted for sealing, so that the slurry has a stable environment in the gel curing process, and meanwhile, the phenomenon that water drops are formed in the water evaporation process to drip to influence the appearance of a blank body and even cause cracking is avoided.
The spontaneous solidification molding needs few additives ISOBAM-104, ISOBAM-104 is in solution for a long time, amide groups and carboxylic acid groups in molecular chains form firm seven-membered rings through hydrogen bonds, ammonium carboxylate is promoted to ionize NH4+, and then the bonding is carried out with-COO-on long chains, so that the performance of ISOBAM-104 is changed, hydrophobic molecular chains are polymerized to form van der Waals force, a certain amount of ISOBAM-104 is uniformly dispersed on the surfaces of alumina particles, and finally slurry gel is solidified. Adding ISOBAM104 with the mass fraction of 0.3-0.5 wt% into alumina slurry with the solid content of 70-75 wt%, standing for 12-18h to form a gel structure of Q bomb, but cracking can occur in the drying process due to low solid content.
The sodium citrate as dispersant is ionized into ion and adsorbed onto the surface of alumina particle to form one kind of double electric layer structure on the surface of the alumina particle, so as to raise the surface charge density, overcome the van der Waals attraction between alumina particles and realize the dispersing effect. Adding ISOBAM104 with the mass fraction of 0.3-0.5 wt% into slurry with the solid phase content of 75wt%, and under the condition of not adding sodium citrate, stirring the viscosity of the slurry at a low speed to reach 28000-30000mPa & s, adding 0.1-0.3 wt% of sodium citrate, and stirring at the same speed, so that the viscosity of the slurry is reduced to 1750mPa & s-2000mPa & s.
The content of the gel ISOBAM104 is 0.3-0.5%; the content of the sodium citrate serving as a dispersant is 0.1-0.3%, the content of a solid phase can reach 80-85 wt%, and the defoaming agent with the content not more than 0.1% is added, so that the slurry can be poured out and spread out for forming.
Detailed Description
The present invention will now be further described with reference to examples.
The alumina ceramic material formed by spontaneous solidification comprises alumina powder, a gelling agent, a dispersing agent and a defoaming agent; the gel is ISOBAM104, and the content of the gel is 0.3-0.5%; the dispersant is sodium citrate, and the content of the dispersant is 0.1 to 0.3 percent; the defoaming agent is NXZ, and the content of the defoaming agent is not more than 0.1%; the rest is alumina powder.
A method for preparing a spontaneously solidified and molded alumina ceramic substrate is characterized in that the alumina ceramic substrate is prepared by spontaneous solidification by taking ISOBAM104 as a gelling agent and sodium citrate as a dispersing agent.
The addition amount of the gel ISOBAM104 is 0.3 to 0.5 percent, and the addition amount of the sodium citrate is 0.1 to 0.3 percent.
The preparation method of the alumina ceramic substrate formed by spontaneous solidification comprises the following steps:
(1) Adding ISOBAM104 and sodium citrate into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2) for 10-16h, adding 0.1wt% of defoaming agent, and continuing ball milling for 5min;
(4) Pouring the slurry obtained in the step (3) into a mold coated with a release agent, vibrating and exhausting, and flattening into a substrate blank with the thickness of 2-3 mm;
(5) Sealing the substrate blank in the step (4), standing for 24-72h, and solidifying and molding;
(6) Putting the blank body obtained in the step (5) and the mould into an oven for drying;
(7) Demoulding, wherein the one-time highest firing temperature is 1150-1250 ℃;
(8) Polishing, wherein the secondary maximum firing temperature is 1580-1610 ℃;
the fineness D50 of the alumina powder in the step (2) is 0.4-0.6 μm.
The mold in the step (4) is a silica gel mold, and the release agent is glycerol.
The silica gel mould is sealed on the glass plate by paraffin wax, and the softening temperature of the paraffin wax is 40-60 ℃.
And (3) sealing in the step (5) by using one or two of paper and a porous plate.
The defoaming agent in the step (3) is NXZ.
The drying temperature curve of the oven in the step (6) is 8-16h at 30 ℃, 10-24h at 60 ℃, 10-18h at 80 ℃ and 2-3h at 100 ℃.
The volume density of the ceramic substrate is 3.9-3.92 g cm-3, and the flexural strength is 269-337 MPa.
Example 1:
step one, adding ISOBAM104 with solid content of 0.3wt% and sodium citrate with solid content of 0.2wt% into 50g of deionized water for complete dissolution;
adding alumina powder into the solution obtained in the step one to prepare slurry with high solid content of 83 wt%;
step three, performing ball milling dispersion on the slurry obtained in the step two for 13 hours, adding 0.1wt% of defoaming agent NXZ, and performing ball milling for 5 minutes to obtain slurry with good fluidity;
step four, pouring a layer of molten low-temperature wax on the surface of the glass uniformly, wherein the softening temperature is 50 ℃, adhering the silica gel mold on the glass, and coating a proper amount of glycerol on the surface of the silica gel mold;
pouring the slurry obtained in the third step into a glycerol-coated mould obtained in the fourth step, vibrating, exhausting gas, and flattening into substrate blank slurry with the thickness of 2.5 mm;
step six, sealing the base plate blank slurry mould in the step five with paper, standing for 48h, and solidifying and forming;
step seven, putting the blank body in the step six and the mould into an oven, 12h at 30 ℃, 12h at 60 ℃, 12h at 80 ℃ and 3h at 100 DEG C
Step eight, demolding, wherein the one-time highest firing temperature is 1200 ℃;
step nine, polishing, keeping the temperature for 5 hours at the maximum secondary firing temperature of 1600 ℃, and adopting a multi-layer sintering mode to obtain the ceramic substrate with the thickness of 1.5mm and the volume density of 3.91g/cm 3 The breaking strength is 337MPa.
Example 2
Step one, adding ISOBAM104 with solid content of 0.4wt% and sodium citrate with solid content of 0.1wt% into 50g of deionized water for complete dissolution;
adding alumina powder into the solution obtained in the step one to prepare slurry with high solid content of 80 wt%;
step three, performing ball milling dispersion on the slurry obtained in the step two for 10 hours, adding 0.1wt% of defoaming agent NXZ, and performing ball milling for 5 minutes to obtain slurry with good fluidity;
step four, pouring a layer of molten low-temperature wax on the surface of the glass uniformly, wherein the softening temperature of the wax is 60 ℃, adhering the silica gel mold on the glass, and coating a proper amount of glycerol on the surface of the silica gel mold;
pouring the slurry obtained in the third step into the mould coated with the glycerol obtained in the fourth step, vibrating and exhausting, and flattening the slurry into substrate blank slurry with the thickness of 2 mm;
step six, sealing the base plate blank slurry mould in the step five by using a porous plate, standing for 72 hours, and solidifying and molding;
step seven, putting the blank body in the step six and the mould into an oven, wherein the temperature is 30 ℃ 16h,60 ℃ 24h,80 ℃ 18h and 100 ℃ 3h
Step eight, demolding, wherein the one-time highest firing temperature is 1250 ℃;
step nine, polishing, keeping the temperature for 5h at the maximum secondary firing temperature of 1610 ℃, and adopting a multi-layer sintering mode to obtain the ceramic substrate with the thickness of 1mm and the volume density of 3.92g/cm 3 The breaking strength is 322MPa.
Example 3
Step one, adding ISOBAM104 with solid content of 0.5wt% and sodium citrate with solid content of 0.3wt% into 50g of deionized water for complete dissolution;
adding alumina powder into the solution obtained in the step one to prepare slurry with high solid content of 85 wt%;
step three, performing ball milling dispersion on the slurry obtained in the step two for 16 hours, adding 0.1wt% of defoaming agent NXZ, and performing ball milling for 5 minutes to obtain slurry with good fluidity;
step four, pouring a layer of molten low-temperature wax on the surface of the glass uniformly, wherein the softening temperature of the wax is 40 ℃, adhering the silica gel mold on the glass, and coating a proper amount of glycerol on the surface of the silica gel mold;
pouring the slurry obtained in the third step into a glycerol-coated mould obtained in the fourth step, vibrating, exhausting air, and flattening the slurry into substrate blank slurry with the thickness of 3 mm;
step six, sealing the base plate blank slurry mould in the step five by using a porous plate or paper, standing for 24 hours, and solidifying and forming;
step seven, putting the blank body in the step six and the mould into an oven, wherein the temperature is respectively 8h at 30 ℃, 10h at 60 ℃, 5h at 80 ℃ and 2h at 100 DEG C
Step eight, demolding, wherein the one-time highest firing temperature is 1150 ℃;
step nine, polishing, keeping the temperature for 5h at the maximum secondary firing temperature of 1580 ℃, and adopting a multi-layer sintering mode to obtain the ceramic substrate with the thickness of 2mm and the volume density of 3.90g/cm 3 The breaking strength is 269MPa.
Comparative example:
1. the solution without the use of gelling agent;
(1) Adding sodium citrate into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2) for 10-16h, adding 0.1wt% of defoaming agent, and continuing ball milling for 5min;
(4) Pouring the slurry obtained in the step (3) into a mold coated with a release agent, vibrating to exhaust, and flattening into a substrate blank with the thickness of 2-3 mm;
(5) Sealing the substrate blank in the step (4), and standing for 24-72h;
and (3) test results: during standing, the blank cracks into many small pieces due to stress caused by shrinkage.
2. The scheme of not adopting a dispersing agent is adopted,
(1) Adding ISOBAM104 into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) And (3) performing ball milling dispersion on the slurry obtained in the step (2) for 10-16h.
And (3) test results: the powder is adhered to the wall of the ball milling tank, has no flowability and is not uniform.
3. Other gelling agents the sodium citrate complexing protocol of the present invention,
other gels have more addition and some have certain toxicity.
4. Scheme for matching gel with other dispersing agents
(1) Adding ISOBAM104 and sodium polyacrylate into deionized water for complete dissolution;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2) for 10-16h, adding 0.1wt% of defoaming agent, and continuing ball milling for 5min;
experiment results show that under the condition of the ammonium polyacrylate and the sodium citrate with the same proportion, slurry added with the sodium citrate has flowability, because the ammonium polyacrylate and the ISOBAM104 are added with the same amount, the slurry is stuck on a ball milling tank, the flowability is extremely poor, the ISOBAM104 and the dispersant ammonium polyacrylate can react, and the dispersion is not facilitated.
5. Non-drying scheme
(1) Adding ISOBAM104 and sodium citrate into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2) for 10-16h, adding 0.1wt% of defoaming agent, and continuing ball milling for 5min;
(4) Pouring the slurry obtained in the step (3) into a mold coated with a release agent, vibrating to exhaust, and flattening into a substrate blank with the thickness of 2-3 mm;
(5) Standing the blank in the step (4) for 24-72h, and solidifying and molding;
and (3) test results: during the drying process, because the blank of the gel is soft and is not sealed, the evaporation speed of the edge is high, the blank is dried and hardened firstly to generate shrinkage stress, and the middle blank is soft and can generate cracking.
Claims (10)
1. The alumina ceramic material formed by spontaneous solidification is characterized by comprising alumina powder, a gelling agent, a dispersing agent and a defoaming agent;
the gel is ISOBAM104, and the content of the gel is 0.3-0.5%;
the dispersant is sodium citrate, and the content of the dispersant is 0.1 to 0.3 percent;
the content of the defoaming agent is not more than 0.1%;
the rest is alumina powder.
2. The preparation method of the alumina ceramic substrate formed by spontaneous solidification is characterized in that the alumina ceramic substrate is prepared by spontaneous solidification by taking ISOBAM104 as a gelling agent and sodium citrate as a dispersing agent.
3. The method for preparing the alumina ceramic substrate formed by spontaneous solidification according to claim 1, wherein the addition amount of the gelling agent ISOBAM104 is 0.3-0.5%, and the addition amount of the sodium citrate is 0.1-0.3%.
4. The method for preparing the alumina ceramic substrate formed by spontaneous solidification according to claim 2, wherein the method for preparing the alumina ceramic substrate comprises:
(1) Adding ISOBAM104 and sodium citrate into deionized water to be completely dissolved;
(2) Adding alumina powder into the solution obtained in the step (1) to prepare 80-85 wt% of slurry with high solid content;
(3) Performing ball milling dispersion on the slurry obtained in the step (2), adding 0.1wt% of defoaming agent, and continuing ball milling;
(4) Pouring the slurry obtained in the step (3) into a mold coated with a release agent, vibrating to exhaust, and flattening into a substrate blank;
(5) Sealing the substrate blank in the step (4), standing, solidifying and molding;
(6) Putting the blank body obtained in the step (5) and the mould into an oven for drying;
(7) Demoulding, wherein the maximum firing temperature at one time is 1150-1250 ℃;
(8) Polishing, wherein the secondary maximum firing temperature is 1580-1610 ℃.
5. The method for preparing the alumina ceramic substrate formed by spontaneous solidification according to claim 4, wherein the fineness of the alumina powder in the step (2) is 0.4 to 0.6 μm.
6. The method for preparing an alumina ceramic substrate formed by spontaneous solidification according to claim 4, wherein the mold in the step (4) is a silica gel mold, and the release agent is glycerin;
the silica gel mold is sealed on a glass plate by paraffin, and the softening temperature of the paraffin is 40-60 ℃.
7. The method for preparing a self-solidifying formed alumina ceramic substrate according to claim 4, wherein the sealing material in the step (5) is one or both of paper and porous plate.
8. The method for preparing an alumina ceramic substrate formed by spontaneous solidification according to claim 4, wherein the antifoaming agent in the step (3) is NXZ.
9. The method for preparing the alumina ceramic substrate formed by spontaneous solidification according to claim 4, wherein the drying temperature curve of the oven in the step (6) is 8-1697 h at 30 ℃, 10-24h at 60 ℃, 5-8h at 80 ℃ and 2h at 100 ℃.
10. The method of claim 4, wherein the bulk density of the ceramic substrate is 3.9-3.92 g/cm 3 The flexural strength is 269-337 MPa.
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| CN116023124A (en) * | 2023-03-28 | 2023-04-28 | 成都超纯应用材料有限责任公司 | Alumina ceramic based on injection molding and preparation method thereof |
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