CN113773091A - Aluminum nitride ceramic tape-casting slurry, aluminum nitride ceramic substrate and preparation method - Google Patents
Aluminum nitride ceramic tape-casting slurry, aluminum nitride ceramic substrate and preparation method Download PDFInfo
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- CN113773091A CN113773091A CN202110920742.6A CN202110920742A CN113773091A CN 113773091 A CN113773091 A CN 113773091A CN 202110920742 A CN202110920742 A CN 202110920742A CN 113773091 A CN113773091 A CN 113773091A
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- aluminum nitride
- nitride ceramic
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- casting slurry
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 77
- 239000000919 ceramic Substances 0.000 title claims abstract description 72
- 239000002002 slurry Substances 0.000 title claims abstract description 37
- 239000000758 substrate Substances 0.000 title claims abstract description 28
- 238000010345 tape casting Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 51
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 15
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 12
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 10
- 239000004014 plasticizer Substances 0.000 claims abstract description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000292 calcium oxide Substances 0.000 claims abstract description 8
- 229910001954 samarium oxide Inorganic materials 0.000 claims abstract description 7
- 229940075630 samarium oxide Drugs 0.000 claims abstract description 7
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 33
- 238000005266 casting Methods 0.000 claims description 32
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 13
- 238000004080 punching Methods 0.000 claims description 11
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims description 7
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims description 7
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 5
- 229940117972 triolein Drugs 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- 238000001816 cooling Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003292 glue Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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Abstract
The invention discloses aluminum nitride ceramic tape-casting slurry which is prepared from the following raw materials in parts by mass: 100 parts of aluminum nitride powder, 3-10 parts of a sintering aid, 1-6 parts of a dispersing agent, 50-100 parts of an organic solvent, 10-50 parts of a binder, 1-15 parts of a plasticizer and 0.5-2 parts of a defoaming agent. The sintering aid consists of a component A and a component B, wherein the component A is at least one of yttrium oxide and calcium oxide, and the component B is at least one of niobium pentoxide, cerium oxide and samarium oxide. Therefore, the sintering temperature of the aluminum nitride ceramic substrate is not more than 1800 ℃, the sintering temperature rise rate is higher than 5 ℃/min, the sintering heat preservation time can be lower than 3 hours, the efficiency of the preparation process is improved, and the performance of the ceramic is not reduced.
Description
Technical Field
The invention belongs to the technical field of electronic ceramics, and particularly relates to aluminum nitride ceramic tape-casting slurry, an aluminum nitride ceramic substrate and a preparation method thereof
Background
The aluminum nitride ceramic has high thermal conductivity (close to silicon carbide and beryllium oxide which is 5-10 times of that of aluminum oxide), low dielectric constant and dielectric loss, good electrical insulation property and thermal expansion coefficient matched with silicon and gallium arsenide, and is an ideal electronic packaging material.
In the preparation process of the aluminum nitride ceramic substrate for electronic assembly, the casting slurry is the key. In order to control the sintering temperature and improve the performance of the finished product, oxides, fluorides, carbonates or silicates of metal elements such as calcium, yttrium, lanthanum, samarium and the like are usually added into the aluminum nitride ceramic tape casting slurry as a multi-element sintering aid (sintering aid), so that the sintering temperature is between 1800 and 1900 ℃.
The existing aluminum nitride ceramic low-temperature sintering aid contains lithium oxide or lithium carbonate, reduces the sintering temperature or sintering time, but has adverse effect on the thermal conductivity or mechanical property of a finished product.
Disclosure of Invention
The invention aims to solve the technical problem of improving the sintering process of the aluminum nitride ceramic substrate on the premise of not influencing the main performance.
The invention provides aluminum nitride ceramic tape-casting slurry which is prepared from the following raw materials in parts by mass: 100 parts of aluminum nitride powder, 3-10 parts of a sintering aid, 1-6 parts of a dispersing agent, 50-100 parts of an organic solvent, 10-50 parts of a binder, 1-15 parts of a plasticizer and 0.5-2 parts of a defoaming agent; the sintering aid consists of a component A and a component B, wherein the component A is at least one of yttrium oxide and calcium oxide, and the component B is at least one of niobium pentoxide, cerium oxide and samarium oxide. The sintering aid is adopted, wherein the covalent property of oxide chemical bonds: the yttrium oxide and the niobium pentoxide are centered, the calcium oxide is strongest, the cerium oxide and the samarium oxide are weakest, and the melting points of the yttrium oxide, the niobium pentoxide and the samarium oxide are all higher than 2000 ℃. The great or similar degree of the covalency difference is beneficial to the co-melting, thereby reducing the sintering temperature of the aluminum nitride ceramic.
Optionally, the mass ratio of the component a to the component B is 1: 2 to 3. The proportion of the yttrium oxide and the calcium oxide in the sintering aid is controlled, so that the two components can be reduced from mixing into aluminum nitride crystal lattices, and the reduction of the heat conductivity of ceramic finished products is inhibited.
Optionally, the component B is 2-4 parts of niobium pentoxide. The sintering aid is adopted, wherein the covalent property of niobium pentoxide is similar to that of yttrium oxide, and the melting point of the niobium pentoxide is lower than 1500 ℃, so that the sintering temperature of the aluminum nitride ceramic can be reduced.
Optionally, the purity of the aluminum nitride powder is greater than 99.0%, and the average particle size of the aluminum nitride powder is 1-2 μm.
Optionally, the organic solvent is a mixed solution of isopropanol and ethyl acetate, and the mass ratio of the isopropanol to the ethyl acetate is 2:1, the mass part of the organic solvent is 50-100. The mixed solvent of isopropanol and ethyl acetate is adopted, the dispersibility of other organic components is good, and the mixed solvent has a lower boiling range temperature when the mass ratio of the isopropanol to the ethyl acetate is 2: 1.
Optionally, the dispersant is selected from at least one of triolein, triethyl phosphate, sodium polyacrylate, and castor oil.
Optionally, the dispersing agent is 4-6 parts of triolein.
Optionally, the plasticizer is dibutyl phthalate 5-12 parts, the binder is polyvinyl butyral 10-20 parts, and the defoaming agent is octanol 1-2 parts.
The invention also provides an aluminum nitride ceramic substrate prepared by using the aluminum nitride ceramic casting slurry.
The invention also provides a preparation method of the aluminum nitride ceramic substrate, which comprises the following steps:
s10, tape casting: feeding the aluminum nitride ceramic casting slurry into a casting machine, flatly paving on a film belt, and then drying to obtain a casting sheet;
s20, punching: feeding the casting sheet into a sheet punching machine, and punching to obtain a green sheet with a preset shape;
s30, rubber discharging: feeding the green body sheet into a binder removal furnace, raising the temperature to 450-550 ℃ at a heating rate of 0.5-2 ℃/min, preserving the temperature for 60-120 min, and removing the organic solvent, the dispersing agent, the binder, the plasticizer and the defoaming agent to obtain a binder removal green body sheet;
s40, sintering: and (3) sending the rubber discharge blank sheet into a sintering furnace, heating to 1650-1800 ℃ at a heating rate of 2-8 ℃/min in a nitrogen or inert atmosphere, and preserving heat for 2.5-5 hours.
Alternatively, in the casting step of S10, the base film for casting is peeled finally. Depending on the base film material used.
Optionally, after the step of die cutting at S20 and before the step of glue discharging at S30, a lamination press is performed: and overlapping 4-12 layers of the green sheets obtained in the step of punching by S20, and pressing for 1-5 min under the conditions that the temperature is 100-150 ℃ and the pressure is 8-20 Mpa. Thereby further improving the density of the prepared aluminum nitride ceramic substrate.
The technical effects of the technical scheme of the invention are as follows: (1) the adopted sintering aid consists of a component A and a component B, wherein the component A is at least one of yttrium oxide and calcium oxide, and the component B is at least one of niobium pentoxide, cerium oxide and samarium oxide. Therefore, the sintering temperature of the aluminum nitride ceramic substrate is not more than 1800 ℃, the sintering temperature rise rate can reach 8 ℃/min, the sintering heat preservation time can be as low as 2.5 hours, the efficiency of the preparation process is improved, and the performance of the ceramic is not reduced; (2) the method adopts a mixed solvent of isopropanol and ethyl acetate, and the mass ratio of the isopropanol to the ethyl acetate is 2:1, the boiling range with lower temperature is provided, so that the effects of airing and removing glue after tape casting are better, and the glue removing temperature is not more than 550 ℃.
Detailed Description
In order that those skilled in the art will fully understand the present invention, embodiments of the present invention are described below.
In the following description, parts of all components are parts by mass, min represents minutes, and h represents hours.
The aluminum nitride ceramic casting slurry in the embodiment of the invention is prepared from the raw materials listed in the table 1:
TABLE 1 composition of raw materials (in parts by mass) of aluminum nitride ceramic tape-casting slurry
| Aluminum nitride powder | 100 |
| Sintering aid | 3～10 |
| Dispersing agent | 1～6 |
| Organic solvent | 50～100 |
| Binder | 10～50 |
| Plasticizer | 1～15 |
| Defoaming agent | 0.5～2 |
The sintering aid comprises a component A and a component B, wherein the component A is at least one of yttrium oxide (for short, yttrium oxide) and calcium oxide, and the component B is at least one of niobium pentoxide (for short, niobium oxide), cerium oxide and samarium oxide.
Specifically, the mass ratio of the component A to the component B is 1: 2 to 3.
Specifically, the component B is 2-4 parts of niobium pentoxide.
Specifically, the purity of the aluminum nitride powder is more than 99.0%, and the average particle size of the aluminum nitride powder is 1-2 μm. The organic solvent is a mixed solution of isopropanol and ethyl acetate, and the mass ratio of the isopropanol to the ethyl acetate is 2:1, the mass part of the organic solvent is 50-100.
Specifically, the dispersant is selected from at least one of triolein, triethyl phosphate, sodium polyacrylate, and castor oil. More specifically, the dispersing agent is 4-6 parts of glycerol trioleate, the plasticizer is 5-12 parts of dibutyl phthalate, the binder is 10-20 parts of polyvinyl butyral, and the defoaming agent is 1-2 parts of octanol.
Specifically, the preparation method of the aluminum nitride ceramic casting slurry comprises the following steps:
s01, primary ball milling: adding 100 parts of aluminum nitride powder, 3-10 parts of sintering aid, 1-6 parts of dispersing agent and 50-100 parts of organic solvent into a ball mill for ball milling for 6-8 h.
S02, secondary ball milling: and S01, adding 10-50 parts of binder and 1-15 parts of plasticizer into the materials obtained by the processing, and continuing ball milling for 4-6 hours.
S03, defoaming: and S02, adding 0.5-2 parts of defoaming agent into the material obtained by the treatment, and stirring for 30-50 min in vacuum to obtain slurry which is uniformly dispersed and has proper and stable viscosity.
The aluminum nitride ceramic substrate in the embodiment of the invention is prepared from the aluminum nitride ceramic casting slurry.
The preparation method of the aluminum nitride ceramic substrate in the embodiment of the invention comprises the steps of casting, binder removal, sintering and the like of the aluminum nitride ceramic casting slurry. Compared with the existing preparation method of the aluminum nitride ceramic, the sintering temperature is not more than 1800 ℃, the sintering temperature rise rate can reach 8 ℃/min, the sintering heat preservation time can be as low as 2.5 hours, the efficiency of the preparation process is improved, and the performance of the ceramic cannot be reduced.
The following describes the details of the embodiments of the present invention.
Example 1
Firstly, preparing aluminum nitride ceramic tape-casting slurry, wherein the raw materials and parts are listed in a table 2, and the following steps are adopted:
s01, primary ball milling: 100 parts of aluminum nitride powder with the purity of 99.9 percent, 2 parts of yttrium oxide, 0.5 part of calcium oxide, 4 parts of niobium oxide, 6 parts of triolein, 33.5 parts of isopropanol and 16.5 parts of ethyl acetate are added into a ball mill to be ball-milled for 8 hours.
S02, secondary ball milling: and S01, adding 10 parts of polyvinyl butyral and 5 parts of dibutyl phthalate into the obtained material, and continuing to perform ball milling for 6 hours.
S03, defoaming: and S02, adding 1.5 parts of octanol into the mixture, and stirring the mixture in vacuum for 30min to prepare slurry which is uniformly dispersed and has proper and stable viscosity.
TABLE 2 raw material composition (parts by mass) of casting pastes in examples and comparative examples
Then preparing an aluminum nitride ceramic substrate by adopting the following steps:
s10, tape casting: feeding the aluminum nitride ceramic casting slurry obtained in the step S03 into a casting machine, flatly paving on a film belt, and then drying to obtain a casting sheet;
s20, punching: feeding the casting sheet obtained in the step S10 into a sheet punching machine, and punching to obtain a green sheet with a preset shape;
s30, rubber discharging: sending the green sheet obtained in the step S20 into a binder removal furnace, raising the temperature to 500 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 120min, and removing the organic solvent, the dispersing agent, the binder, the plasticizer and the defoaming agent to obtain a binder removal green sheet;
s40, sintering: and (4) sending the discharged rubber blank sheet obtained in the step S30 into a sintering furnace, heating to 1760 ℃ at the heating rate of 5 ℃/min in the atmosphere of high-purity nitrogen, preserving heat for 2.5h, and naturally cooling to obtain the aluminum nitride ceramic substrate. In other embodiments, the sintering protective gas may be a mixture of nitrogen and hydrogen, or other chemically inert gases.
Example 2
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the primary ball milling time is 8 hours, the secondary ball milling time is 6 hours, and the defoaming time is 30 min.
S30, rubber discharging: raising the temperature to 550 ℃ at the heating rate of 1.5 ℃/min, and preserving the heat for 120 min;
s40, sintering: heating to 1680 ℃ at the heating rate of 6 ℃/min, preserving the temperature for 3h, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 3
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the primary ball milling time is 6 hours, the secondary ball milling time is 5 hours, and the defoaming time is 50 min.
S30, rubber discharging: heating to 510 ℃ at the heating rate of 1.5 ℃/min, and keeping the temperature for 60 min;
s40, sintering: heating to 1650 ℃ at the heating rate of 5.5 ℃/min, preserving the heat for 3.5h, and naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 4
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the secondary ball milling time is 5h, and the defoaming time is 40 min.
S30, rubber discharging: raising the temperature to 530 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 120 min;
s40, sintering: heating to 1800 ℃ at the heating rate of 7 ℃/min, preserving the heat for 2.5 hours, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 5
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the primary ball milling time is 8.5h, and the defoaming time is 35 min.
S30, rubber discharging: heating to 540 deg.C at a rate of 2 deg.C/min, and maintaining for 120 min;
s40, sintering: heating to 1675 ℃ at the heating rate of 4 ℃/min, preserving the heat for 3h, and naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 6
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the secondary ball milling time is 5.5h, and the defoaming time is 40 min.
S30, rubber discharging: heating to 480 ℃ at a heating rate of 1.8 ℃/min, and keeping the temperature for 80 min;
s40, sintering: heating to 1700 ℃ at the heating rate of 3 ℃/min, preserving the heat for 2.5h, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 7
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials are fed according to the parts shown in Table 2, the primary ball milling time is 7.5h, the secondary ball milling time is 5.5h, and the defoaming time is 30 min.
S30, rubber discharging: heating to 450 deg.C at a rate of 1.2 deg.C/min, and maintaining for 120 min;
s40, sintering: raising the temperature to 1750 ℃ at the heating rate of 2 ℃/min, preserving the temperature for 3h, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
Example 8
The procedure used was essentially identical to that of example 1, with the following differences:
in the casting step of S10, the base film for casting is peeled off finally;
after the die cutting step of S20 and before the glue discharging step of S30, laminate pressing is performed: the green sheet obtained in the punching step of S20 was laminated by 8 layers and pressed at a temperature of 120 ℃ and a pressure of 14MPa for 3 min.
In other embodiments, the green sheets may be stacked in 4, 6, 10 or 12 layers, controlled at a temperature of 100, 110, 130, 140 or 150 ℃, a pressing pressure of 8, 12, 16 or 20MPa, and a pressing time of 1, 2, 4 or 5 minutes.
Comparative example 1
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials were charged in the parts shown in Table 2, and the defoaming time was 30 min.
S30, rubber discharging: heating to 500 deg.C at a rate of 1 deg.C/min, and maintaining for 120 min;
s40, sintering: raising the temperature to 1760 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2.5h, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
Comparative example 2
The procedure used was essentially identical to that of example 1, with the following differences:
preparing aluminum nitride ceramic tape-casting slurry: the raw materials were charged in the parts shown in Table 2, and the defoaming time was 30 min.
S30, rubber discharging: raising the temperature to 550 ℃ at the heating rate of 1.5 ℃/min, and preserving the heat for 120 min;
s40, sintering: heating to 1780 ℃ at the heating rate of 6 ℃/min, preserving the heat for 3h, and then naturally cooling to obtain the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrates obtained in the above 8 examples and two comparative examples were subjected to the density test of the sample by the archimedes drainage method, the bending strength test of the sample by the three-point bending test, the thermal conductivity test of the sample by the laser flash method, and the microhardness test of the sample by the microhardness test. The test results are shown in Table 3.
As can be seen from Table 3, in 8 examples, the density, flexural strength, microhardness and thermal conductivity of the aluminum nitride ceramic substrate are all equivalent to those of the aluminum nitride ceramic electronic substrate in the prior art, and can meet the technical requirements of the electronic industry. Example 8 has improved density, flexural strength and thermal conductivity compared to example 1.
TABLE 3 test results of ceramic substrates in examples and comparative examples
Comparative example 1 corresponds to example 1 and comparative example 2 corresponds to example 2, in both of which the sintering aid does not contain component B but is replaced by an equal mass of component a. The finished samples of the comparative examples had low flexural strength and low thermal conductivity under the same sintering process. If better test results are to be obtained, the sintering temperature is increased, the sintering temperature rise rate is reduced or the sintering heat preservation time is prolonged, so that the structure of the ceramic crystal is more complete.
The above examples are only preferred embodiments of the present invention, which are used for illustrating the content of the present invention and do not constitute any limitation to the scope of the present invention. It should be understood by those skilled in the art that the equivalent components, equivalent flow transformations, or direct applications of the present disclosure to other related arts are included within the scope of the present disclosure.
Claims (10)
1. The aluminum nitride ceramic tape-casting slurry is characterized by being prepared from the following raw materials in parts by mass:
the sintering aid consists of a component A and a component B, wherein the component A is at least one of yttrium oxide and calcium oxide, and the component B is at least one of niobium pentoxide, cerium oxide and samarium oxide.
2. The aluminum nitride ceramic casting slurry according to claim 1, wherein the mass ratio of the component a to the component B is 1: 2 to 3.
3. The aluminum nitride ceramic casting slurry according to claim 1, wherein the component B is 2 to 4 parts of niobium pentoxide.
4. The aluminum nitride ceramic casting slurry according to claim 1, wherein the purity of the aluminum nitride powder is more than 99.0%, and the average particle diameter of the aluminum nitride powder is 1 to 2 μm.
5. The aluminum nitride ceramic casting slurry of claim 1, wherein the organic solvent is a mixture of isopropanol and ethyl acetate, and the mass ratio of isopropanol to ethyl acetate is 2:1, the mass part of the organic solvent is 50-100.
6. The aluminum nitride ceramic casting slurry of claim 5, wherein the dispersant is selected from at least one of triolein, triethyl phosphate, sodium polyacrylate, and castor oil.
7. The aluminum nitride ceramic casting slurry according to claim 6, wherein the dispersant is 4 to 6 parts of glycerol trioleate.
8. The aluminum nitride ceramic casting slurry according to claim 7, wherein the plasticizer is dibutyl phthalate in an amount of 5 to 12 parts, the binder is polyvinyl butyral in an amount of 10 to 20 parts, and the defoaming agent is octanol in an amount of 1 to 2 parts.
9. An aluminum nitride ceramic substrate produced by using the aluminum nitride ceramic casting slurry according to any one of claims 1 to 8.
10. A preparation method of an aluminum nitride ceramic substrate comprises the following steps:
s10, tape casting: feeding the aluminum nitride ceramic casting slurry of any one of claims 1 to 8 into a casting machine, spreading the slurry on a film belt, and then drying to obtain a casting sheet;
s20, punching: feeding the casting sheet into a sheet punching machine, and punching to obtain a green sheet with a preset shape;
s30, rubber discharging: feeding the green body sheet into a binder removal furnace, raising the temperature to 450-550 ℃ at a heating rate of 0.5-2 ℃/min, preserving the temperature for 60-120 min, and removing the organic solvent, the dispersing agent, the binder, the plasticizer and the defoaming agent to obtain a binder removal green body sheet;
s40, sintering: and (3) sending the rubber discharge blank sheet into a sintering furnace, heating to 1650-1800 ℃ at a heating rate of 2-8 ℃/min in a nitrogen or inert atmosphere, and preserving heat for 2.5-5 hours.
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