CN117105640A - Alumina ceramic substrate and preparation method thereof - Google Patents
Alumina ceramic substrate and preparation method thereof Download PDFInfo
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- CN117105640A CN117105640A CN202311072331.1A CN202311072331A CN117105640A CN 117105640 A CN117105640 A CN 117105640A CN 202311072331 A CN202311072331 A CN 202311072331A CN 117105640 A CN117105640 A CN 117105640A
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- 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 130
- 239000000758 substrate Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000002002 slurry Substances 0.000 claims abstract description 35
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 34
- 239000011029 spinel Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000000853 adhesive Substances 0.000 claims abstract description 27
- 230000001070 adhesive effect Effects 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 29
- 239000003822 epoxy resin Substances 0.000 claims description 28
- 229920000647 polyepoxide Polymers 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 239000001307 helium Substances 0.000 claims description 19
- 229910052734 helium Inorganic materials 0.000 claims description 19
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 19
- 239000011858 nanopowder Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 13
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 239000004848 polyfunctional curative Substances 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 10
- 229920000058 polyacrylate Polymers 0.000 claims description 10
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical class [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 8
- 239000011268 mixed slurry Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 5
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 4
- GIXXQTYGFOHYPT-UHFFFAOYSA-N Bisphenol P Chemical compound C=1C=C(C(C)(C)C=2C=CC(O)=CC=2)C=CC=1C(C)(C)C1=CC=C(O)C=C1 GIXXQTYGFOHYPT-UHFFFAOYSA-N 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- GKXVJHDEWHKBFH-UHFFFAOYSA-N [2-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC=C1CN GKXVJHDEWHKBFH-UHFFFAOYSA-N 0.000 claims description 3
- GKQPCPXONLDCMU-CCEZHUSRSA-N lacidipine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C1=CC=CC=C1\C=C\C(=O)OC(C)(C)C GKQPCPXONLDCMU-CCEZHUSRSA-N 0.000 claims description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 2
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000395 magnesium oxide Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000005329 float glass Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005336 cracking Methods 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000002159 abnormal effect Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000695274 Processa Species 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 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
- 238000009831 deintercalation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- -1 yttrium compound Chemical class 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Classifications
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- 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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- 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
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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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
- C04B35/634—Polymers
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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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention provides an alumina ceramic substrate and a preparation method thereof, wherein the alumina ceramic substrate comprises the following raw materials: alumina, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent, wherein the mass ratio of the components is as follows: (50-70): (0.05-0.5): (2-10): (0.1-1): (1-3). The preparation method comprises the following steps: respectively weighing aluminum oxide, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent according to stoichiometric proportions; adding alumina and magnesia alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill to obtain slurry; removing bubbles from the slurry, adding a hardening agent into the slurry after removing the bubbles, uniformly mixing, casting into a die, curing at room temperature for a certain time, drying the cured green tape in a humidity environment for a certain time, and drying at room temperature for a certain time; and respectively presintering and sintering the dried green tapes to obtain the alumina ceramic substrate.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to an alumina ceramic substrate and a preparation method thereof.
Background
The alumina ceramic substrate is the most stable substance in oxide, has the characteristics of high mechanical strength, high hardness, wear resistance, high temperature resistance, corrosion resistance, high electrical insulation, low dielectric loss and the like, is a ceramic material which has earlier development, lower cost and the most wide application, and is very widely applied in the fields of aerospace, aviation, wear resistance, microwave dielectric and the like. In microcosmic, the alumina ceramic substrate is a material formed by combining covalent bonds and ionic bonds, and the material has the defects of high brittleness and low toughness due to the directionality of the combined valence bonds, so that the material breaks at extremely low strain values, and the working reliability and the use safety of ceramic parts are affected, thereby greatly limiting the wide application of the alumina ceramic substrate, and therefore, how to improve the strength of alumina is the focus of the research of the alumina ceramic substrate industry.
In facing the above problems, researchers have invented a number of toughening methods, among which phase change toughening, whisker and particle toughening, fiber toughening, nanowire or nanotube toughening, and the like are common. But the phase change, whisker and particle toughening effects are not particularly pronounced; the operation engineering of fiber toughening is complex, and the density of the product is poor; carbon nanowires or nanotubes are generally used for toughening the nanowires or nanotubes, and are easily reacted with a matrix material at high temperature, so that the toughening effect is reduced. In order to obtain good toughening effect, researchers try to adopt more than two toughening methods, and Chinese patent document CN101948325A discloses a synergic toughening alumina ceramic substrate and a preparation method thereof. The technology adopts phase change toughening and whisker toughening, and improves the toughness of the alumina ceramic substrate.
The silicon compound, the zirconium compound and the yttrium compound adopted in the process of preparing the alumina ceramic substrate are dissolved in the solvent, so that a large amount of solvent volatilizes in the subsequent drying process, and the volatilized solvent easily causes cracking of the alumina ceramic substrate, so that the alumina ceramic substrate has high porosity and is difficult to form a compact structure; furthermore, the binder is also largely volatilized during the discharge of the paste, and voids are formed in the ceramic. The hardness and strength of the alumina ceramic substrate are seriously affected by the above conditions.
Disclosure of Invention
In view of the above, the present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides an alumina ceramic substrate and a preparation method thereof. The alumina ceramic substrate provided by the invention has novel and unique structure, shortens the pore canal of sodium ion deintercalation, improves the ion diffusion speed of the material, and has good electrochemical performance and multiplying power performance. Meanwhile, the preparation method has simple process flow and is suitable for large-scale industrial production.
To this end, in a first aspect, an embodiment of the present invention provides an alumina ceramic substrate, where the alumina ceramic substrate preparation raw materials include the following components: alumina, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent, wherein the mass ratio of the components is as follows: (50-70): (0.05-0.5): (2-10): (0.1-1): (1-3).
Preferably, the alumina is high-purity alumina nano powder, the purity of the alumina nano powder is more than 99.9 percent, and the specific surface area is 10-20m 2 /g, median particle size of 0.1 μm to 0.3 μm; the magnesia-alumina spinel is magnesia-alumina spinel nano powder, and the specific surface area is 25-35m 2 /g。
Preferably, the adhesive is a mixture of epoxy resin and ethylene glycol diglycidyl ether; wherein the mass ratio of the epoxy resin to the ethylene glycol diglycidyl ether is (2-3): (7-8), wherein the epoxy resin is one or a mixture of a plurality of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin and bisphenol P epoxy resin.
Preferably, the dispersing agent is a mixture of sodium polyacrylate and ammonium polyacrylate, and the mass ratio of the sodium polyacrylate to the ammonium polyacrylate is (3-4): (6-7); the hardener is one or more of dipropylenetriamine, ethylenediamine, diethylenetriamine, triethylenetetramine and xylylenediamine.
In a second aspect, an embodiment of the present invention provides a method for preparing an alumina ceramic substrate, the method comprising weighing alumina, magnesia-alumina spinel, an adhesive, a dispersant, and a hardener, respectively, according to a stoichiometric ratio; adding the weighed alumina and magnesia-alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill to obtain slurry; placing the obtained slurry into a defoaming machine for defoaming, and then adding the weighed hardening agent into the defoamed slurry and uniformly mixing; casting the uniformly mixed slurry in a mould, curing for a certain time at room temperature, drying the cured green tape for a certain time in a humidity environment, and drying for a certain time at room temperature; presintering the dried green tape to obtain a presintered green tape; and sintering the pre-sintered green tape to obtain the alumina ceramic substrate.
Preferably, the mixing time is 20-24h, the slurry particle diameter D50 is 0.4-0.6 mu m, the viscosity is 1000-5000Pa.s, and the solid load rate is 42% -45%.
Preferably, the bubble removal time is 20-30min and the bubble removal pressure is 0.8-1kPa.
Preferably, the curing time is 2-4 hours; the drying time under the humidity environment is 24-48h, wherein the humidity environment is an environment with humidity higher than 98%; the drying time is 24-48h under the room temperature condition.
Preferably, the pre-sintering step is performed on the dried green tape: heating from room temperature to 700-900 ℃ at a heating rate of 0.5-1.5 ℃/min, and preserving heat for 2-4h; wherein the presintered sintering atmosphere comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
Preferably, the sintering step of the pre-sintered green tape is as follows: heating to 1450-1550 ℃ at a heating rate of 1-3 ℃/min, and preserving heat for 2-4h; wherein the sintering atmosphere for sintering comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
The relative density of the alumina ceramic substrate prepared by the preparation method provided by the embodiment of the invention reaches more than 99.5%, and the density is more than 3.98g/cm 3 The bending strength can reach more than 600 MPa. In addition, the preparation method of the alumina ceramic substrate provided by the invention has the advantages that the adhesive with low viscosity is added in the preparation process, so that the slurry with low viscosity and high load can be obtained; in addition, the alumina ceramic substrate is prepared by adopting a casting method, and the slurry is dried for 2 hours in an environment with the humidity of 98 percent after being solidified4-48h, and drying for 24-48h at room temperature, so as to effectively prevent the occurrence of cracking and deformation of the green belt caused by too high drying rate; magnesia-alumina spinel is added into the raw materials, so that the sintering process is enhanced, abnormal growth of crystal grains is restrained, and the alumina ceramic substrate with high strength is prepared. Meanwhile, the preparation method has simple process flow and is suitable for large-scale industrial production.
Drawings
Fig. 1 is a flowchart of a preparation method of an alumina ceramic substrate according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
The following disclosure provides many different embodiments, or examples, for implementing different structures of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the applicability of other processes and/or the use of other materials.
The invention aims to provide an alumina ceramic substrate and a preparation method thereof, the alumina ceramic substrate provided by the invention is a high-strength alumina ceramic substrate with the thickness of 0.02-0.2mm, the relative density of the alumina ceramic substrate is more than 99.5%, and the density is more than 3.98g/cm 3 And the bending strength can reach more than 600 MPa. The preparation method of the alumina ceramic substrate provided by the invention can obtain low-viscosity and high-negative adhesive by adding the low-viscosity adhesive in the preparation processA supported slurry; in addition, the alumina ceramic substrate is prepared by adopting a casting method, the slurry is dried for 24-48 hours in an environment with the humidity of 98% after being solidified, and then is dried for 24-48 hours at room temperature, so that the occurrence of belt cracking and deformation caused by too high drying rate is effectively prevented; magnesia-alumina spinel is added into the raw materials, so that the sintering process is enhanced, abnormal growth of crystal grains is restrained, and the alumina ceramic substrate with high strength is prepared. Meanwhile, the preparation method has simple process flow and is suitable for large-scale industrial production.
The embodiment of the first aspect of the invention provides an alumina ceramic substrate, wherein the alumina ceramic substrate preparation raw materials comprise the following components: alumina, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent, wherein the mass ratio of the components is as follows: (50-70): (0.05-0.5): (2-10): (0.1-1): (1-3).
Wherein the alumina is high-purity alumina nano powder, the purity of the alumina nano powder is more than 99.9%, and the specific surface area is 10-20m 2 /g, preferably 15m 2 And/g, the median particle diameter is 0.1 μm to 0.3 μm. The magnesia-alumina spinel is magnesia-alumina spinel nano powder, and the specific surface area is 25-35m 2 /g, preferably 30m 2 /g。
The adhesive is a mixture of epoxy resin and ethylene glycol diglycidyl ether. Wherein the mass ratio of the epoxy resin to the ethylene glycol diglycidyl ether is (2-3): (7-8), the epoxy resin may be one or more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, bisphenol P type epoxy resin, etc.
The dispersant is sodium polyacrylate (molecular weight Mw=1800-2300 g.mol) -1 ) And a mixture of ammonium polyacrylate salts (molecular weight mw=3300-3600 g·mol) -1 ) The mass ratio of the two is (3-4): (6-7). The hardener can be one or more of dipropylenetriamine, ethylenediamine, diethylenetriamine, triethylenetetramine, xylylenediamine and the like.
According to the alumina ceramic substrate, the magnesia-alumina spinel and the low-viscosity adhesive are added into the raw materials, so that the high-strength alumina ceramic substrate can be obtained, and the relative density of the alumina ceramic substrate reaches99.5% or more, density > 3.98g/cm 3 The bending strength can reach more than 600 MPa.
An embodiment of the second aspect of the present invention provides a method for preparing an alumina ceramic substrate, as shown in fig. 1, the method comprising the steps of:
step S1: respectively weighing aluminum oxide, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent according to stoichiometric proportions;
wherein, the mass ratio of the alumina, the magnesia-alumina spinel, the adhesive and the dispersing agent is as follows: (50-70): (0.05-0.5): (2-10): (0.1-1): (1-3).
In the embodiment of the invention, the alumina is high-purity alumina nano powder, the purity of the alumina nano powder is more than 99.9%, and the specific surface area is 15m 2 And/g, the median particle diameter is 0.1 μm to 0.3 μm. The magnesia-alumina spinel is magnesia-alumina spinel nano powder, and the specific surface area is 30m 2 /g。
The adhesive is a mixture of epoxy resin and ethylene glycol diglycidyl ether. Wherein the mass ratio of the epoxy resin to the ethylene glycol diglycidyl ether is (2-3): (7-8), the epoxy resin may be one or a mixture of a bisphenol A type epoxy resin, a bisphenol F type epoxy resin, a bisphenol S type epoxy resin, a bisphenol P type epoxy resin, etc. The dispersant is sodium polyacrylate (molecular weight Mw=1800-2300 g.mol) -1 ) And a mixture of ammonium polyacrylate salts (molecular weight mw=3300-3600 g·mol) -1 ) The mass ratio of the two is (3-4): (6-7).
Step S2: adding the weighed alumina and magnesia-alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill to obtain slurry;
wherein the mixing time can be 20-24h, the grain diameter D50 of the obtained slurry is 0.4-0.6 mu m, the viscosity is 1000-5000Pa.s, and the solid load rate is 42-45%.
Step S3: placing the obtained slurry into a defoaming machine for defoaming, and then adding the weighed hardening agent into the defoamed slurry and uniformly mixing;
wherein the bubble removal time can be 20-30min, and the bubble removal pressure can be 0.8-1kPa.
Step S4: casting the uniformly mixed slurry in a mould, curing for a certain time at room temperature, drying the cured green tape for a certain time in a humidity environment, and drying for a certain time at room temperature;
in an embodiment of the present invention, the mold may be a float glass mold, and preferably, the float glass mold is cleaned with a mixture of ethanol and hydrochloric acid before use. The curing time may be 2 to 4 hours; the drying time under the humidity environment can be 24-48h, wherein the humidity environment refers to an environment with humidity of more than 98%; the drying time at room temperature may be 24-48 hours.
Step S5: presintering the dried green tape to obtain a presintered green tape;
specifically, the pre-sintering step of the dried green tape may be: heating from room temperature to 700-900 ℃ at a heating rate of 0.5-1.5 ℃/min, and preserving heat for 2-4h. Wherein the presintered sintering atmosphere comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
Step S6: and sintering the pre-sintered green tape to obtain the alumina ceramic substrate.
Specifically, the sintering step of the pre-sintered green tape may be: heating to 1450-1550 ℃ at a heating rate of 1-3 ℃/min, and preserving heat for 2-4h. Wherein the sintering atmosphere for sintering comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
According to the preparation method of the alumina ceramic substrate, provided by the embodiment of the invention, the low-viscosity adhesive is added in the preparation process, so that the slurry with low viscosity and high load can be obtained; in addition, the alumina ceramic substrate is prepared by adopting a casting method, the slurry is dried for 24-48 hours in an environment with the humidity of 98% after being solidified, and then is dried for 24-48 hours at room temperature, so that the occurrence of belt cracking and deformation caused by too high drying rate is effectively prevented; magnesia-alumina spinel is added into the raw materials, so that the sintering process is enhanced, abnormal growth of crystal grains is restrained, and the alumina ceramic substrate with high strength is prepared. Meanwhile, the preparation method has simple process flow and is suitable for large-scale industrial production.
The following describes in further detail the specific procedures and effects of the preparation method of the alumina ceramic substrate according to the present invention with reference to some specific examples, but is not limited to the scope of the present invention.
Example 1
The embodiment provides a preparation method of an alumina ceramic substrate, which comprises the following steps:
step S1: 1200g (specific surface area 15 m) of high-purity alumina nano powder is weighed 2 4g (specific surface area 30 m) of magnesia-alumina spinel nano powder 2 Per g), 120g of ethylene glycol diglycidyl ether of epoxy resin, 8g of sodium polyacrylate (molecular weight mw=2100 g mol) -1 ) 12g of ammonium polyacrylate salt (molecular weight Mw=3500 g.mol) -1 ) 596g of deionized water and 60g of hardener;
step S2: adding aluminum oxide and magnesia alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill for 24 hours to obtain slurry with the particle size D50 of 0.53 mu m, the viscosity of 3000Pa.s and the solid loading rate of 43.8%;
step S3: placing the obtained slurry in a bubble removing machine for bubble removal for 30min, wherein the bubble removing pressure is 0.8kPa, adding the weighed hardener into the bubble removed slurry, and uniformly mixing;
step S4: cleaning a float glass mold by using a mixture of ethanol and hydrochloric acid, casting the uniformly mixed slurry into the float glass mold, curing for 4 hours at room temperature, peeling the cured green belt from the mold after curing, drying for 40 hours in an environment with the humidity of 98%, and drying for 48 hours at room temperature;
step S5: presintering the dried green tape, heating the green tape from room temperature to 900 ℃ at a heating rate of 1 ℃/min under helium atmosphere, and preserving heat for 4 hours;
step S6: sintering the pre-sintered green tape, heating to 1500 ℃ at a heating rate of 1 ℃/min under helium atmosphere, and preserving heat for 2 hours to obtain the alumina ceramic substrate.
Example 2
The embodiment provides a preparation method of an alumina ceramic substrate, which comprises the following steps:
step S1: 1200g (specific surface area 15 m) of high-purity alumina nano powder is weighed 2 4g (specific surface area 30 m) of magnesia-alumina spinel nano powder 2 Per g), 160g of ethylene glycol diglycidyl ether of epoxy resin, 8g of sodium polyacrylate (molecular weight Mw=2100 g. Mol) -1 ) 12g of ammonium polyacrylate salt (molecular weight Mw=3500 g.mol) -1 ) 556g of deionized water and 60g of hardener;
step S2: adding aluminum oxide and magnesia-alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill for 24 hours to obtain slurry with the particle size D50 of 0.55 mu m, the viscosity of 3280Pa.s and the solid loading rate of 44.2%;
step S3: placing the obtained slurry in a bubble removing machine for bubble removal for 30min, wherein the bubble removing pressure is 0.8kPa, adding the weighed hardener into the bubble removed slurry, and uniformly mixing;
step S4: cleaning a float glass mold by using a mixture of ethanol and hydrochloric acid, casting the uniformly mixed slurry into the float glass mold, curing for 4 hours at room temperature, peeling the cured green belt from the mold after curing, drying for 40 hours in an environment with the humidity of 98%, and drying for 48 hours at room temperature;
step S5: presintering the dried green tape, heating the green tape from room temperature to 900 ℃ at a heating rate of 1 ℃/min under helium atmosphere, and preserving heat for 4 hours;
step S6: sintering the pre-sintered green tape, heating to 1500 ℃ at a heating rate of 1.5 ℃/min under helium atmosphere, and preserving heat for 3 hours to obtain the alumina ceramic substrate.
Example 3
The embodiment provides a preparation method of an alumina ceramic substrate, which comprises the following steps:
step S1: 1200g (specific surface area 15 m) of high-purity alumina nano powder is weighed 2 4g (specific surface area 30 m) of magnesia-alumina spinel nano powder 2 Per g), 200g of ethylene glycol diglycidyl ether of epoxy resin, 8g of sodium polyacrylate (min)Molecular weight Mw=2100 g & mol -1 ) 12g of ammonium polyacrylate salt (molecular weight Mw=3500 g.mol) -1 ) 516g of deionized water and 60g of hardener;
step S2: adding aluminum oxide and magnesia alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill for 24 hours to obtain slurry with the particle size D50 of 0.58 mu m, the viscosity of 4210Pa.s and the solid loading rate of 44.8%;
step S3: placing the obtained slurry in a bubble removing machine for bubble removal for 30min, wherein the bubble removing pressure is 0.8kPa, adding the weighed hardener into the bubble removed slurry, and uniformly mixing;
step S4: cleaning a float glass mold by using a mixture of ethanol and hydrochloric acid, casting the uniformly mixed slurry into the float glass mold, curing for 4 hours at room temperature, peeling the cured green belt from the mold after curing, drying for 40 hours in an environment with the humidity of 98%, and drying for 48 hours at room temperature;
step S5: presintering the dried green tape, heating the green tape from room temperature to 900 ℃ at a heating rate of 1 ℃/min under helium atmosphere, and preserving heat for 4 hours;
step S6: sintering the pre-sintered green tape, heating to 1500 ℃ at a heating rate of 2.0 ℃/min under helium atmosphere, and preserving heat for 3 hours to obtain the alumina ceramic substrate.
Comparative example 1
The embodiment provides a preparation method of an alumina ceramic substrate, which comprises the following steps:
step S1: 1200g (specific surface area 15 m) of high-purity alumina nano powder is weighed 2 4g (specific surface area 30 m) of magnesia-alumina spinel nano powder 2 Per g), epoxy resin ethylene glycol diglycidyl ether 36g, sodium polyacrylate 8g (molecular weight mw=2100 g mol -1 ) 12g of ammonium polyacrylate salt (molecular weight Mw=3500 g.mol) -1 ) 680g of deionized water and 60g of hardener;
step S2: adding aluminum oxide and magnesia alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill for 24 hours to obtain slurry with the particle size D50 of 0.51 mu m, the viscosity of 2280Pa.s and the solid loading rate of 36.2%;
step S3: placing the obtained slurry in a bubble removing machine for bubble removal for 30min, wherein the bubble removing pressure is 0.8kPa, adding the weighed hardener into the bubble removed slurry, and uniformly mixing;
step S4: cleaning a float glass mold by using a mixture of ethanol and hydrochloric acid, casting the uniformly mixed slurry into the float glass mold, curing for 4 hours at room temperature, peeling the cured green belt from the mold after curing, drying for 40 hours in an environment with the humidity of 98%, and drying for 48 hours at room temperature;
step S5: sintering the dried green tape, heating the green tape from room temperature to 1500 ℃ at a heating rate of 1.5 ℃/min under helium atmosphere, and preserving heat for 5 hours to obtain the alumina ceramic substrate
In order to verify the quality of the alumina ceramic substrate finished product prepared by the preparation method of the alumina ceramic substrate provided by the embodiment of the present invention, the alumina ceramic substrates prepared in the above-mentioned examples 1 to 3 and comparative example 1 were tested, and the test results are shown in table 1.
Table 1, test items and test results of examples 1-3 and comparative example 1
| Examples numbering | Flexural Strength (MPa) | Relative density of |
| Example 1 | 612 | 3.982 |
| Example 2 | 628 | 3.985 |
| Example 3 | 618 | 3.983 |
| Comparative example 1 | 506 | 3.935 |
According to the above examples and comparative examples and the comparison of the test results obtained by testing them, the flexural strength and the relative density of the alumina ceramic substrates in examples 1 to 3 are greatly improved compared with comparative example 1, and it can be seen that the alumina ceramic substrate prepared by the preparation method of the present invention has better flexural strength and relative density.
In conclusion, the relative density of the alumina ceramic substrate prepared by the preparation method provided by the embodiment of the invention reaches more than 99.5%, and the density is more than 3.98g/cm 3 The bending strength can reach more than 600 MPa. In addition, the preparation method of the alumina ceramic substrate provided by the invention has the advantages that the adhesive with low viscosity is added in the preparation process, so that the slurry with low viscosity and high load can be obtained; in addition, the alumina ceramic substrate is prepared by adopting a casting method, the slurry is dried for 24-48 hours in an environment with the humidity of 98% after being solidified, and then is dried for 24-48 hours at room temperature, so that the occurrence of belt cracking and deformation caused by too high drying rate is effectively prevented; magnesia-alumina spinel is added into the raw materials, so that the sintering process is enhanced, abnormal growth of crystal grains is restrained, and the alumina ceramic substrate with high strength is prepared. Meanwhile, the preparation method has simple process flow and is suitable for large-scale industrial production.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A high strength alumina ceramic substrate, characterized in that: the alumina ceramic substrate preparation raw materials comprise the following components: alumina, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent, wherein the mass ratio of the components is as follows: (50-70): (0.05-0.5): (2-10): (0.1-1): (1-3).
2. The alumina ceramic substrate according to claim 1, wherein the alumina is a high purity alumina nano powder having a purity of 99.9% or more and a specific surface area of 10 to 20m 2 /g, median particle size of 0.1 μm to 0.3 μm; the magnesia-alumina spinel is magnesia-alumina spinel nano powder, and the specific surface area is 25-35m 2 /g。
3. The alumina ceramic substrate of claim 1, wherein the adhesive is a mixture of epoxy resin and ethylene glycol diglycidyl ether; wherein the mass ratio of the epoxy resin to the ethylene glycol diglycidyl ether is (2-3): (7-8), wherein the epoxy resin is one or a mixture of a plurality of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin and bisphenol P epoxy resin.
4. The alumina ceramic substrate according to claim 1, wherein the dispersant is a mixture of sodium polyacrylate salt and ammonium polyacrylate salt, and the mass ratio of the sodium polyacrylate salt to the ammonium polyacrylate salt is (3-4): (6-7); the hardener is one or more of dipropylenetriamine, ethylenediamine, diethylenetriamine, triethylenetetramine and xylylenediamine.
5. A method of preparing the alumina ceramic substrate of claim 1, comprising:
step S1: respectively weighing aluminum oxide, magnesia-alumina spinel, an adhesive, a dispersing agent and a hardening agent according to stoichiometric proportions;
step S2: adding the weighed alumina and magnesia-alumina spinel into deionized water, adding an adhesive and a dispersing agent, and mixing by a ball mill to obtain slurry;
step S3: placing the obtained slurry into a defoaming machine for defoaming, and then adding the weighed hardening agent into the defoamed slurry and uniformly mixing;
step S4: casting the uniformly mixed slurry in a mould, curing for a certain time at room temperature, drying the cured green tape for a certain time in a humidity environment, and drying for a certain time at room temperature;
step S5: presintering the dried green tape to obtain a presintered green tape;
step S6: and sintering the pre-sintered green tape to obtain the alumina ceramic substrate.
6. The method according to claim 5, wherein in the step S2, the mixing time is 20 to 24 hours, the slurry particle diameter D50 is 0.4 to 0.6 μm, the viscosity is 1000 to 5000pa.s, and the solid loading rate is 42 to 45%.
7. The method according to claim 5, wherein the bubble removal time is 20 to 30 minutes and the bubble removal pressure is 0.8 to 1kPa in the step S3.
8. The method of producing an alumina ceramic substrate according to claim 5, wherein in the step S4, the curing time is 2 to 4 hours; the drying time under the humidity environment is 24-48h, wherein the humidity environment is an environment with humidity higher than 98%; the drying time is 24-48h under the room temperature condition.
9. The method according to claim 5, wherein in the step S5, the step of pre-firing the dried green tape comprises: heating from room temperature to 700-900 ℃ at a heating rate of 0.5-1.5 ℃/min, and preserving heat for 2-4h; wherein the presintered sintering atmosphere comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
10. The method according to claim 5, wherein in the step S6, the sintering step of the green tape after the pre-sintering is performed as follows: heating to 1450-1550 ℃ at a heating rate of 1-3 ℃/min, and preserving heat for 2-4h; wherein the sintering atmosphere for sintering comprises nitrogen, argon, helium or one or more mixed atmospheres of nitrogen, argon and helium.
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