CN116639985B - High-thermal-conductivity silicon nitride ceramic substrate and application thereof - Google Patents
High-thermal-conductivity silicon nitride ceramic substrate and application thereof Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 58
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 49
- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical class [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 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 abstract description 12
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 12
- 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 abstract description 12
- 229940117972 triolein Drugs 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- JZHRGBKQPQTREL-UHFFFAOYSA-N 2-(4-phenylbutoxycarbonyl)benzoic acid Chemical compound OC(=O)C1=CC=CC=C1C(=O)OCCCCC1=CC=CC=C1 JZHRGBKQPQTREL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000011863 silicon-based powder Substances 0.000 claims description 16
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 14
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000010345 tape casting Methods 0.000 claims description 10
- KOFGAQNZWLWHCK-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-thiol Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)S KOFGAQNZWLWHCK-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 244000028419 Styrax benzoin Species 0.000 claims description 7
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 7
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 7
- 229960002130 benzoin Drugs 0.000 claims description 7
- 235000019382 gum benzoic Nutrition 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 5
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 5
- 239000013078 crystal Substances 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000007373 indentation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910021426 porous silicon Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- DJADIOIWLJDZAQ-UHFFFAOYSA-N C1(=CC=CC=C1)C.C(C=1C(C(=O)O)=CC=CC1)(=O)OCCCC Chemical compound C1(=CC=CC=C1)C.C(C=1C(C(=O)O)=CC=CC1)(=O)OCCCC DJADIOIWLJDZAQ-UHFFFAOYSA-N 0.000 description 1
- 238000007545 Vickers hardness test Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The application discloses a high-thermal-conductivity silicon nitride ceramic substrate and application thereof, and relates to the technical field of silicon nitride ceramics. The silicon nitride ceramic substrate comprises the following raw materials in parts by weight: 60 parts of modified silicon powder, 2.5-10 parts of sintering aid, 0.5-5 parts of triolein, 50-200 parts of solvent, 5-20 parts of polyvinyl butyral and 3-20 parts of phenylbutyl phthalate. The silicon nitride ceramic substrate prepared by the application has high heat conduction performance and excellent mechanical property.
Description
Technical Field
The invention relates to the technical field of silicon nitride ceramics, in particular to a high-heat-conductivity silicon nitride ceramic substrate and application thereof.
Background
In recent years, semiconductor devices have been rapidly developed in the direction of power enhancement, high frequency enhancement, and integration. The semiconductor process and microelectronic technology required for supporting the development of the semiconductor chip are also rapidly developed, and for example, the integrated circuits are more and more integrated, the flat cable density is more and more high, and the heat rejection problem of the electronic package substrate is also caused. The heat generated by the operation of the semiconductor device is a critical factor in causing the failure of the semiconductor device, and the thermal conductivity of the insulating substrate is a critical factor in affecting the heat dissipation of the overall semiconductor device. If the substrate cannot effectively discharge heat of components on the integrated circuit in time, a large amount of heat is accumulated on the integrated circuit, and finally the components are damaged. The problem of substrate heat dissipation can be solved by improving the heat conductivity of the substrate and reducing the thickness of the substrate, however, considering that the substrate needs to have higher requirements on mechanical properties in the use environment, the substrate material needs to have high heat conductivity and excellent mechanical properties at the same time.
Silicon nitride ceramic is a structural ceramic material with the best comprehensive performance, and the theoretical thermal conductivity of single crystal silicon nitride can reach more than 400 W.m -1·K-1, so that the silicon nitride ceramic has the potential of becoming a high-thermal-conductivity substrate. However, silicon nitride belongs to a strong covalent bond compound, and has a complex crystal structure, low self-diffusion coefficient of silicon atoms and nitrogen atoms, small sintering driving force of silicon nitride powder, and difficult sintering, and usually an oxide sintering aid is added to generate a liquid phase at high temperature, so that sintering is promoted through particle rearrangement, dissolution and precipitation processes. In the sintering process, a small amount of sintering additive is added, and the densification sintering is realized by forming a liquid phase with a silicon dioxide layer formed on the surface of the silicon nitride powder through the sintering additive, so that the purpose of obtaining sintered dense silicon nitride ceramics at a lower temperature is achieved, and the effect of improving the heat conductivity is realized. Impurity oxygen is dissolved into the silicon nitride crystal lattice to form silicon vacancies, and the silicon nitride is influenced by factors such as self crystal lattice defects and the like, so that the actual thermal conductivity of the silicon nitride is greatly different from the theoretical value. If the thermal conductivity needs to be improved, long-time heat preservation is needed to promote oxygen in crystal lattices to diffuse out, and the mechanical property of the material is necessarily affected.
Disclosure of Invention
The invention aims to provide a high-heat-conductivity silicon nitride ceramic substrate and application thereof, which solve the following technical problems:
The prior silicon nitride ceramic substrate is doped with oxygen impurities due to the addition of oxygen-containing sintering auxiliary agent and the like in the preparation process, so that the thermal conductivity of the prepared silicon nitride ceramic substrate is far lower than the theoretical thermal conductivity of monocrystalline silicon nitride.
The aim of the invention can be achieved by the following technical scheme:
The silicon nitride ceramic substrate with high thermal conductivity comprises the following raw materials in parts by weight: 60 parts of modified silicon powder, 2.5-10 parts of sintering aid, 0.5-5 parts of triolein, 50-200 parts of solvent, 5-20 parts of polyvinyl butyral and 3-20 parts of phenylbutyl phthalate.
As a further aspect of the invention: the preparation method of the high-heat-conductivity silicon nitride ceramic substrate comprises the following steps:
a1: mixing triolein and a solvent, continuously adding modified silicon powder and a sintering aid, and ball milling to obtain slurry;
A2: continuously adding tolylbutyl phthalate and polyvinyl butyral into the slurry prepared in the step A1, and performing ball milling to obtain modified slurry;
A3: defoaming the modified slurry, and carrying out tape casting molding to obtain a silicon tape casting film;
A4: cutting and laminating the silicon casting film obtained in the step A3, and sintering in a vacuum furnace to obtain a substrate;
A5: heating the substrate obtained in the step A4 to 1300-1400 ℃ in a nitrogen atmosphere to obtain a nitrided substrate;
A6: and (3) heating the nitriding substrate obtained in the step A5 to 1800-1900 ℃ under the nitrogen pressure of 0.5-0.7MPa, and preserving heat for 1-12h to obtain the high-heat-conductivity silicon nitride ceramic substrate.
As a further aspect of the invention: the preparation method of the modified silicon powder comprises the following steps:
s1: adding deionized water and vinyl trimethoxy silane into a reaction bottle, uniformly stirring, adding silicon powder, heating to 70-80 ℃, and preserving heat for 1-2h to obtain silane coupling agent modified silicon powder;
S2: in nitrogen atmosphere, adding ethyl acetate, perfluorooctanethiol and benzoin dimethyl ether into a reaction kettle, uniformly stirring, adding silane coupling agent modified silicon powder into the reaction kettle, and reacting for 0.5-1h to obtain modified silicon powder.
As a further aspect of the invention: in the S1, the mass ratio of deionized water to vinyl trimethoxy silane to silicon powder is 50-100:0.1-1:50.
As a further aspect of the invention: in S2, the mass ratio of the ethyl acetate to the perfluorooctanethiol to the benzoin dimethyl ether to the silane coupling agent modified silicon powder is 500-1000:5-10:0.1-1:100.
As a further aspect of the invention: the sintering aid is Y 2S i4N6 C with the mass ratio of 4:1-2: mixing MgO to obtain the product.
As a further aspect of the invention: the volume ratio of the solvent is 1:1 and butanone.
An application of a silicon nitride ceramic substrate with high thermal conductivity in the field of electronic components.
The invention has the beneficial effects that:
(1) According to the application, silicon powder is used as a raw material, double bond groups are grafted on the surface of the silicon powder through grafting of silicon hydroxyl groups on the surface of the silicon powder and vinyl silane coupling agents, mercapto groups of perfluorooctanethiol are utilized to react with double bonds on the surface of the silicon powder, and perfluoroalkyl groups are grafted on the surface of the silicon powder, so that modified silicon powder is obtained. The modification of the application effectively reduces the oxygen content of the surface of the silicon powder, and in the sintering process, the perfluor alkane grafted on the surface of the modified silicon powder and the sintering aid synergistically enhance, so that oxygen impurities in silicon nitride crystals can be effectively removed, silicon vacancies caused by oxygen solid solution of impurities into the silicon nitride crystal lattice can be effectively avoided, crystal grains are purified, the growth of the crystal grains is promoted, the density of the silicon nitride is improved, and the thermal conductivity of the silicon nitride is further improved.
(2) According to the application, the surface of the silicon powder is subjected to organic treatment to obtain the modified silicon powder, and the triolein is added as the dispersing agent, so that the agglomeration of powder in the slurry is effectively reduced, and the improvement of the solid content of the slurry and the improvement of the flow property of the slurry are facilitated. And the intensity and toughness of the casting film in the preparation process of the silicon nitride ceramic substrate are improved by adding polyvinyl butyral and toluene butyl phthalate. The compact of silicon composed of modified silicon powder and sintering aid is heated in nitrogen atmosphere, silicon nitride is converted into porous silicon nitride sintered body, then the silicon nitride sintered body is further heated to higher temperature, so that the porous silicon nitride is sintered into compact silicon nitride ceramic, the sintering aid introduces nitrogen and promotes elimination of silicon dioxide, a higher nitrogen-oxygen ratio is formed in the second phase, so that particles in the compact silicon nitride sample are increased, the oxygen content in crystal lattice is reduced, the intermolecular continuity of silicon nitride is increased, and the thermal conductivity is increased.
Detailed Description
The following description will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the modified silicon powder comprises the following steps:
S1: adding 100mL of deionized water and 0.2g of vinyl trimethoxy silane into a reaction bottle, uniformly stirring, adding 100g of silicon powder, heating to 70 ℃, and preserving heat for 1h to obtain silane coupling agent modified silicon powder;
S2: in a nitrogen atmosphere, adding 500g of ethyl acetate, 5g of perfluorooctanethiol and 0.1g of benzoin dimethyl ether into a reaction kettle, uniformly stirring, adding 100g of silane coupling agent modified silicon powder into the reaction kettle, and reacting for 0.5h to obtain modified silicon powder.
Example 2
The preparation method of the modified silicon powder comprises the following steps:
s1: adding 100mL of deionized water and 1g of vinyl trimethoxy silane into a reaction bottle, uniformly stirring, adding 100g of silicon powder, heating to 70 ℃, and preserving heat for 2 hours to obtain silane coupling agent modified silicon powder;
s2: in a nitrogen atmosphere, adding 500g of ethyl acetate, 5g of perfluorooctanethiol and 1g of benzoin dimethyl ether into a reaction kettle, uniformly stirring, adding 100g of silane coupling agent modified silicon powder into the reaction kettle, and reacting for 1h to obtain the modified silicon powder.
Example 3
The preparation method of the modified silicon powder comprises the following steps:
s1: 200mL of deionized water and 2g of vinyl trimethoxy silane are added into a reaction bottle, uniformly stirred, 100g of silicon powder is added, the temperature is raised to 80 ℃, and the temperature is kept for 2 hours, so as to obtain silane coupling agent modified silicon powder;
S2: in a nitrogen atmosphere, 1000g of ethyl acetate, 10g of perfluorooctanethiol and 1g of benzoin dimethyl ether are added into a reaction kettle, and are uniformly stirred, 100g of silane coupling agent modified silicon powder is added into the reaction kettle, and the reaction is carried out for 1h, so as to obtain the modified silicon powder.
Example 4
The preparation method of the silicon nitride ceramic substrate with high thermal conductivity comprises the following steps:
a1: weighing the following raw materials in parts by weight: 60 parts of modified silicon powder prepared in example 1, 4 parts of Y 2Si4N6 C, 1 part of MgO, 0.5 part of triolein, 100 parts of solvent, 10 parts of polyvinyl butyral and 5 parts of phenylbutyl phthalate; the volume ratio of the solvent is 1:1, mixing ethanol and butanone;
a2: mixing triolein and a solvent, continuously adding modified silicon powder and a sintering aid, and ball milling to obtain slurry;
a3: continuously adding tolylbutyl phthalate and polyvinyl butyral into the slurry prepared in the step A2, and performing ball milling to obtain modified slurry;
a4: defoaming the modified slurry, and carrying out tape casting molding to obtain a silicon tape casting film;
A5: cutting and laminating the silicon casting film obtained in the step A4, and sintering in a vacuum furnace to obtain a substrate;
A6: heating the substrate obtained in the step A5 to 1300-1400 ℃ in a nitrogen atmosphere to obtain a nitrided substrate;
a7: and (3) heating the nitriding substrate obtained in the step A6 to 1800-1900 ℃ under the nitrogen pressure of 0.5-0.7MPa, and preserving heat for 1-12h to obtain the high-heat-conductivity silicon nitride ceramic substrate.
Example 5
The preparation method of the silicon nitride ceramic substrate with high thermal conductivity comprises the following steps:
a1: weighing the following raw materials in parts by weight: 60 parts of modified silicon powder prepared in example 2, 4 parts of Y 2Si4N6 C, 1 part of MgO, 0.5 part of triolein, 100 parts of solvent, 10 parts of polyvinyl butyral and 5 parts of phenylbutyl phthalate; the volume ratio of the solvent is 1:1, mixing ethanol and butanone;
a2: mixing triolein and a solvent, continuously adding modified silicon powder and a sintering aid, and ball milling to obtain slurry;
a3: continuously adding tolylbutyl phthalate and polyvinyl butyral into the slurry prepared in the step A2, and performing ball milling to obtain modified slurry;
a4: defoaming the modified slurry, and carrying out tape casting molding to obtain a silicon tape casting film;
A5: cutting and laminating the silicon casting film obtained in the step A4, and sintering in a vacuum furnace to obtain a substrate;
A6: heating the substrate obtained in the step A5 to 1300-1400 ℃ in a nitrogen atmosphere to obtain a nitrided substrate;
a7: and (3) heating the nitriding substrate obtained in the step A6 to 1800-1900 ℃ under the nitrogen pressure of 0.5-0.7MPa, and preserving heat for 1-12h to obtain the high-heat-conductivity silicon nitride ceramic substrate.
Example 6
The preparation method of the silicon nitride ceramic substrate with high thermal conductivity comprises the following steps:
a1: weighing the following raw materials in parts by weight: 60 parts of modified silicon powder prepared in example 3,4 parts of Y 2Si4N6 C, 1 part of MgO, 0.5 part of triolein, 100 parts of solvent, 10 parts of polyvinyl butyral and 5 parts of phenylbutyl phthalate; the volume ratio of the solvent is 1:1, mixing ethanol and butanone;
a2: mixing triolein and a solvent, continuously adding modified silicon powder and a sintering aid, and ball milling to obtain slurry;
a3: continuously adding tolylbutyl phthalate and polyvinyl butyral into the slurry prepared in the step A2, and performing ball milling to obtain modified slurry;
a4: defoaming the modified slurry, and carrying out tape casting molding to obtain a silicon tape casting film;
A5: cutting and laminating the silicon casting film obtained in the step A4, and sintering in a vacuum furnace to obtain a substrate;
A6: heating the substrate obtained in the step A5 to 1300-1400 ℃ in a nitrogen atmosphere to obtain a nitrided substrate;
a7: and (3) heating the nitriding substrate obtained in the step A6 to 1800-1900 ℃ under the nitrogen pressure of 0.5-0.7MPa, and preserving heat for 1-12h to obtain the high-heat-conductivity silicon nitride ceramic substrate.
Comparative example 1
The preparation method of the modified silicon powder comprises the following steps:
S1: 100mL of deionized water and 0.2g of vinyl trimethoxy silane are added into a reaction bottle, the mixture is stirred uniformly, 100g of silicon powder is added, the temperature is raised to 70 ℃, and the temperature is kept for 1h, so that modified silicon powder is obtained.
Comparative example 2
Compared with example 4, only the modified silicon powder prepared in example 1 used in example 4 was replaced by the modified silicon powder prepared in comparative example 1 in equal amount, and the remaining components and steps were completely identical.
Comparative example 3
Compared with example 4, only the modified silicon powder prepared in example 1 used in example 4 was replaced with silicon powder in equal amount, and the remaining components and steps were completely identical.
Performance detection
(1) Hardness: and (3) a Vickers indentation method is adopted, and after a sample is ground and polished, the sample is pressed by a diamond pressing head of an HBV30A type hardness machine. The pressing pressure was 49N, and the diagonal lengths d1 and d2 were measured after 15 seconds of holding the pressure. To ensure accuracy, 7 points per sample were taken and averaged. The vickers hardness of the sample was calculated by the vickers hardness calculation formula:
H＝(1.8544F/d2)×10-3
wherein: H-Vickers hardness, GPa; f-pressure, N; d-average value mm of indentation diagonal lengths d1, d 2; the detection results are shown in Table 1;
(2) Fracture toughness: the toughness of the sample is tested by adopting an indentation method, the crack diagonal length c of the indentation is measured, and the fracture toughness of the sample is calculated by the following formula:
KIC＝0.02325×P×c-3/2
Wherein: k IC -fracture toughness, MPa.m 1/2; p-load magnitude, kgf; c-diagonal length of indentation crack, mm; the detection results are shown in Table 1;
(3) Flexural strength: the bending strength of the sample was tested by a three-point bending method. The sample has a specification size of 3mm×4mm×36mm, and after polishing, the sample was tested for flexural strength by a universal tester (Mode 5569, company I nstron, U.S.) with a span of 30mm and a ram loading rate of 0.5 mm/min. The flexural strength of the sample was calculated by the formula:
R＝(3FL)/(2bh)2
Wherein: r-flexural strength, MPa; f-experiment loading load, N; l-span between fulcrums, mm; b-width of sample, mm; d-sample thickness in the loading direction, mm; the detection results are shown in Table 1;
(4) Thermal conductivity: the thermal conductivity of the LFA-427 laser thermoconductor samples was tested. The method is characterized in that after the thermal diffusivity of the sample ceramic is calculated, the thermal conductivity formula of the sample ceramic is calculated according to the following formula:
λ＝ραCp
wherein: λ—thermal conductivity, W/(m·k); ρ -sample density, g/cm 3; alpha-thermal diffusivity, mm 2; cp-specific heat capacity, J.g -1·K-1; the detection results are shown in Table 1;
table 1: examples 4-6, comparative examples 2-3 Performance test data statistics
As can be seen from Table 1, the silicon nitride ceramic substrate prepared by the present application has excellent mechanical properties and high thermal conductivity.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (6)
1. The silicon nitride ceramic substrate with high thermal conductivity is characterized by comprising the following raw materials in parts by weight: 60 parts of modified silicon powder, 2.5-10 parts of sintering aid, 0.5-5 parts of triolein, 50-200 parts of solvent, 5-20 parts of polyvinyl butyral and 3-20 parts of phenylbutyl phthalate;
the preparation method of the high-heat-conductivity silicon nitride ceramic substrate comprises the following steps:
a1: mixing triolein and a solvent, continuously adding modified silicon powder and a sintering aid, and ball milling to obtain slurry;
A2: continuously adding tolylbutyl phthalate and polyvinyl butyral into the slurry prepared in the step A1, and performing ball milling to obtain modified slurry;
A3: defoaming the modified slurry, and carrying out tape casting molding to obtain a silicon tape casting film;
A4: cutting and laminating the silicon casting film obtained in the step A3, and sintering in a vacuum furnace to obtain a substrate;
A5: heating the substrate obtained in the step A4 to 1300-1400 ℃ in a nitrogen atmosphere to obtain a nitrided substrate;
a6: heating the nitriding substrate obtained in the step A5 to 1800-1900 ℃ under the nitrogen pressure of 0.5-0.7MPa, and preserving heat for 1-12h to obtain a high-heat-conductivity silicon nitride ceramic substrate;
the preparation method of the modified silicon powder comprises the following steps:
s1: adding deionized water and vinyl trimethoxy silane into a reaction bottle, uniformly stirring, adding silicon powder, heating to 70-80 ℃, and preserving heat for 1-2h to obtain silane coupling agent modified silicon powder;
S2: in nitrogen atmosphere, adding ethyl acetate, perfluorooctanethiol and benzoin dimethyl ether into a reaction kettle, uniformly stirring, adding silane coupling agent modified silicon powder into the reaction kettle, and reacting for 0.5-1h to obtain modified silicon powder.
2. The high thermal conductivity silicon nitride ceramic substrate according to claim 1, wherein the mass ratio of deionized water, vinyltrimethoxysilane and silicon powder in S1 is 50-100:0.1-1:50.
3. The high-thermal-conductivity silicon nitride ceramic substrate according to claim 1, wherein the mass ratio of ethyl acetate, perfluorooctanethiol, benzoin dimethyl ether and silane coupling agent modified silicon powder in S2 is 500-1000:5-10:0.1-1:100.
4. The high thermal conductivity silicon nitride ceramic substrate according to claim 1, wherein the sintering aid is Y 2Si 4N6 C with a mass ratio of 4:1-2: mixing MgO to obtain the product.
5. The high thermal conductivity silicon nitride ceramic substrate according to claim 1, wherein the solvent has a volume ratio of 1:1 and butanone.
6. The use of a high thermal conductivity silicon nitride ceramic substrate according to claim 1 in the field of electronic components.
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