CN114538935A - Forming method of high-thermal-conductivity silicon nitride substrate - Google Patents
Forming method of high-thermal-conductivity silicon nitride substrate Download PDFInfo
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- CN114538935A CN114538935A CN202210267457.3A CN202210267457A CN114538935A CN 114538935 A CN114538935 A CN 114538935A CN 202210267457 A CN202210267457 A CN 202210267457A CN 114538935 A CN114538935 A CN 114538935A
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- Prior art keywords
- silicon nitride
- casting
- sheet
- ball milling
- drying
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 36
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000758 substrate Substances 0.000 title claims abstract description 12
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Abstract
The invention discloses a method for molding a high-thermal-conductivity silicon nitride substrate, which comprises the following molding process steps: s1: material preparation and ball milling: adding an organic monomer and a cross-linking agent into a solvent to prepare a premixed solution, and then mixing the premixed solution, a dispersing agent, silicon nitride and auxiliary ceramic powder for ball milling; s2: and a plasticizer is added to increase the flexibility of the silicon nitride sheet after tape casting. Then carrying out secondary ball milling for 4-30 h; s3: removing bubbles in vacuum, namely removing bubbles in vacuum in the slurry obtained by secondary ball milling, and adding an initiator for stirring; s4: performing gel casting, namely performing casting operation on the slurry obtained by vacuum defoaming; s5: drying the sheet, wherein the sheet has certain strength and toughness after being solidified for certain time, and drying. The invention adopts the technology of combining gel and tape casting, integrates the advantages of two types of molding, reduces the production cost and the environmental pollution, and realizes the preparation of the high-performance silicon nitride ceramic substrate.
Description
Technical Field
The invention relates to the technical field of ceramic forming, in particular to a forming method of a high-thermal-conductivity silicon nitride substrate.
Background
The silicon nitride ceramic has the advantages of high thermal conductivity, high dielectric strength, thermal expansion coefficient matching with Si, SiC, GaN and the like, and becomes an ideal heat dissipation and packaging material for a new generation of large-scale integrated circuits, semiconductor module circuits and high-power devices.
Currently, the main method for preparing silicon nitride ceramic substrates is tape casting, and most of them are organic solvent tape casting. Although the tape casting technology has been applied to industrial production after decades of development, there are still many problems, such as the use of organic solvents (benzene, toluene, xylene, acetone, butanone, etc.) with certain toxicity has high toxicity, high production cost, environmental friendliness and harm to health; the introduction of a large amount of organic matters in the slurry leads to low density of the biscuit, and the biscuit is easy to crack and deform in the glue discharging process; the ceramic powder is settled in the drying process, and the upper surface and the lower surface of the blank form density gradient, which can cause cracks, pits, peeling and the like on the upper surface.
The gel casting is a method of combining the traditional ceramic process with organic polymerization chemistry and flexibly introducing the method of polymerizing high molecular monomers into the ceramic forming process. The basic principle of the process is that organic monomers are added into slurry with low viscosity and high solid content, under the action of a catalyst and an initiator, the organic monomers in the slurry are subjected to cross-linking polymerization to form a three-dimensional network structure, the slurry is subjected to in-situ curing and molding, and then demolding, drying, organic matter removal and sintering are carried out, so that the required ceramic part can be obtained.
The gel casting process combines the characteristics of gel and casting molding, and utilizes the polymerization principle of organic monomers to carry out casting molding, the method is to disperse ceramic powder in a solution containing the organic monomers and a cross-linking agent to prepare a suspension with low viscosity and high solid phase volume fraction, then an initiator and a catalyst are added to initiate the polymerization of the organic monomers under a certain temperature condition, so that the viscosity of the suspension is increased, and the in-situ solidification molding is caused, and the ceramic powder is uniformly distributed in a three-dimensional network structure formed by high polymers. Therefore, the prepared green body has uniform structure, high density and certain strength and can be machined. The slurry used for gel casting is prepared from ceramic powder, organic monomer, cross-linking agent, solvent, dispersant, plasticizer and the like. The gel casting process has the advantages of greatly reducing the use amount of organic matters in the slurry, improving the solid content of the slurry, improving the density and strength of the biscuit, greatly reducing environmental pollution and obviously reducing production cost.
Disclosure of Invention
The present invention is directed to a method for forming a silicon nitride substrate with high thermal conductivity, so as to solve the above problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a forming method of a high-thermal-conductivity silicon nitride substrate comprises the following steps:
s1: material preparation and ball milling: adding an organic monomer and a cross-linking agent into a solvent to prepare a premixed solution, and then mixing the premixed solution, a dispersing agent, silicon nitride and auxiliary ceramic powder for ball milling;
s2: and a plasticizer is added to increase the flexibility of the silicon nitride sheet after tape casting. Then carrying out secondary ball milling for 4-30 h;
s3: removing bubbles in vacuum, namely removing bubbles in vacuum in the slurry obtained by secondary ball milling, and adding an initiator for stirring;
s4: performing gel casting, namely performing casting operation on the slurry obtained by vacuum defoaming;
s5: drying the sheet, wherein the sheet has certain strength and toughness after being solidified for certain time, and drying.
Preferably, in S1 based on the molding process: the organic monomer is acrylamide, methacrylamide, sorbitol polyglycidyl ether or marine epoxy resin, and the like, and the adding amount of the organic monomer is 1-10% of the weight of the silicon nitride powder;
the cross-linking agent is methyl bisacrylamide, the solvent is ethanol, glycol, propanol or isopropanol and the like, and the mass ratio of the organic monomer to the cross-linking agent is 5:1-30: 1;
the dispersant is ammonium polymethacrylate, PEI, phosphate ester or ammonium polyacrylate and the like, and the addition amount of the dispersant is 0.1-2.5% of the weight of the silicon nitride powder;
the ball-material ratio in the ball-milling tank is 0.5:1-3:1, the solid content of the slurry is 20-50%, and the ball-milling time is 2-48 h;
the sintering aid is 6-12% and is oxides or fluorides of magnesium oxide, yttrium oxide, ytterbium oxide, lanthanum oxide, strontium oxide, neodymium oxide, yttrium fluoride, magnesium fluoride and the like.
Preferably, in S2 based on the molding process: the plasticizer is glycerol, polyethylene glycol, phthalate, polyether glycol and oleic acid or a mixture of the glycerol, the polyethylene glycol, the phthalate, the polyether glycol and the oleic acid, the addition amount of the plasticizer is 0.1-10% of the weight of the silicon nitride ceramic powder, and the plasticizer is adjusted according to the thickness of the tape-casting sheet.
Preferably, in S3 based on the molding process: stirring at 30-100 rpm for 5-30 min;
the initiator is azobisisobutylamidine dihydrochloride, tetraethylpentamine or 3, 3' -diaminodipropylamine and the like, and the addition amount of the initiator is 0.25-10% of that of the organic monomer.
Preferably, in S4 based on the molding process: the speed of the casting belt is 0.2m/min-5m/min, the temperature of the heating interval of the casting belt is 40-60 ℃, and the curing time is 10min-60 min; and adjusting various parameters of the casting machine according to the thickness of the casting sheet.
Preferably, in S5 based on the molding process: drying at 30-60 deg.C for 30min-4 h;
and drying the blank to a certain degree, peeling the blank sheet from the casting film, and then cutting and punching to obtain the ceramic blank sheet.
Compared with the prior art, the invention has the following beneficial effects:
1. the method adopts a process combining casting and casting, the ceramic powder in the slurry has high occupation ratio and uniform distribution, the drying time is shorter, the dried blank is more uniform, the defects of cracks and the like generated in the traditional casting process can be effectively reduced, the production time is shortened, and the product quality is improved;
2. the ceramic substrate with the thickness of 0.3-3mm can be directly formed by adopting a casting machine by adjusting the formula, so that the subsequent process that the thick sheet needs cold isostatic pressing in the traditional process is avoided, and the production efficiency is improved;
3. the method adopts alcohols as the solvent, successfully replaces the traditional tape casting toxic solvent, reduces the environmental pollution and reduces the production cost;
4. organic monomers and cross-linking agents are added in the gel casting, the addition amount is less, a binder for casting is not required to be added, the viscosity of the slurry is effectively reduced, the solid content is improved, and the more compact silicon nitride ceramic is obtained, which is the biggest difference between the gel casting and the casting;
5. the silicon nitride blank prepared by the gel casting has high strength but poor flexibility, and an inert gas protection device needs to be added due to the oxygen inhibition effect. The plasticizer is added in the method, so that the flexibility of the silicon nitride green body sheet can be improved, the later punching and laminating operation is facilitated, and more importantly, the oxygen inhibition effect in the polymerization process can be reduced, which is essentially different from the traditional injection-coagulation molding;
6. because the silicon nitride powder is easy to hydrolyze, the water-based gel-casting technology is difficult to popularize and apply in the field of silicon nitride ceramics, and the method can be quickly popularized in the fields of other complicated shapes of the silicon nitride ceramics. The method has simple process and high product stability, and promotes the industrial production of the silicon nitride ceramic substrate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The invention provides two embodiments:
the first embodiment is as follows:
a forming method of a high-thermal-conductivity silicon nitride substrate comprises the following steps:
s1: material preparation and ball milling: adding an organic monomer and a cross-linking agent into a solvent to prepare a premixed solution, and then mixing the premixed solution, a dispersing agent, silicon nitride and auxiliary ceramic powder for ball milling; the organic monomer is acrylamide, methacrylamide, sorbitol polyglycidyl ether or marine epoxy resin, and the like, and the adding amount of the organic monomer is 1-10% of the weight of the silicon nitride powder; the cross-linking agent is methyl bisacrylamide, the solvent is ethanol, glycol, propanol or isopropanol and the like, and the mass ratio of the organic monomer to the cross-linking agent is 5:1-30: 1; the dispersant is ammonium polymethacrylate, PEI, phosphate ester or ammonium polyacrylate and the like, and the addition amount of the dispersant is 0.1-2.5% of the weight of the silicon nitride powder; the ball-material ratio in the ball-milling tank is 0.5:1-3:1, the solid content of the slurry is 20-50%, and the ball-milling time is 2-48 h;
the sintering aid is 6-12% and is oxides or fluorides of magnesium oxide, yttrium oxide, ytterbium oxide, lanthanum oxide, strontium oxide, neodymium oxide, yttrium fluoride, magnesium fluoride and the like.
S2: and a plasticizer is added to increase the flexibility of the silicon nitride sheet after tape casting. Then carrying out secondary ball milling for 4-30 h; the plasticizer is glycerol, polyethylene glycol, phthalate, polyether glycol and oleic acid or a mixture of the glycerol, the polyethylene glycol, the phthalate, the polyether glycol and the oleic acid, the addition amount of the plasticizer is 0.1-10% of the weight of the silicon nitride ceramic powder, and the plasticizer is adjusted according to the thickness of the tape-casting sheet.
S3: removing bubbles in vacuum, namely removing bubbles in vacuum in the slurry obtained by secondary ball milling, and adding an initiator for stirring; stirring at 30-100 rpm for 5-30 min; the initiator is azobisisobutylamidine dihydrochloride, tetraethylpentamine or 3, 3' -diaminodipropylamine and the like, and the addition amount of the initiator is 0.25-10% of that of the organic monomer.
S4: performing gel casting, namely performing casting operation on the slurry obtained by vacuum defoaming; the speed of the casting belt is 0.2m/min-5m/min, the temperature of the heating interval of the casting belt is 40-60 ℃, and the curing time is 10min-60 min; and adjusting various parameters of the casting machine according to the thickness of the casting sheet.
S5: drying the sheet, wherein the sheet has certain strength and toughness after being solidified for certain time, and drying. Drying at 30-60 deg.C for 30min-4 h; and drying the blank to a certain degree, peeling the blank sheet from the casting film, and then cutting and punching to obtain the ceramic blank sheet.
The second embodiment:
5g of acrylamide and 0.5g N, N' -methylene bisacrylamide are added into 80mL of absolute ethyl alcohol to prepare a premixed solution, then 3g of PEI dispersant, 120g of silicon nitride and auxiliary ceramic powder are added, and ball milling is carried out for 10 hours. And 6g of plasticizer glycerol is added, and the mixture is ball-milled for 10 hours again to obtain gel casting slurry. Adding 0.25g of initiator ammonium persulfate into the slurry, defoaming in vacuum at the stirring speed of 50 r/min for 25min, carrying out gel casting on a casting machine at the temperature of 50 ℃, wherein the casting belt speed is 1m/min, and then curing for 40 min. Drying at 30 deg.C for 2 hr to obtain green sheet with thickness of 0.4-1.2 mm.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. A forming method of a high-thermal-conductivity silicon nitride substrate is characterized by comprising the following steps: the molding process comprises the following steps:
s1: material preparation and ball milling: adding an organic monomer and a cross-linking agent into a solvent to prepare a premixed solution, and then mixing the premixed solution, a dispersing agent, silicon nitride and auxiliary ceramic powder for ball milling;
s2: and a plasticizer is added to increase the flexibility of the silicon nitride sheet after tape casting. Then carrying out secondary ball milling for 4-30 h;
s3: removing bubbles in vacuum, namely removing bubbles in vacuum in the slurry obtained by secondary ball milling, and adding an initiator for stirring;
s4: performing gel casting, namely performing casting operation on the slurry obtained by vacuum defoaming;
s5: drying the sheet, wherein the sheet has certain strength and toughness after being solidified for certain time, and drying.
2. The method of claim 1, wherein the method comprises: in S1 based on the molding process: the organic monomer is acrylamide, methacrylamide, sorbitol polyglycidyl ether or marine epoxy resin, and the like, and the adding amount of the organic monomer is 1-10% of the weight of the silicon nitride powder;
the cross-linking agent is methyl bisacrylamide, the solvent is ethanol, glycol, propanol or isopropanol and the like, and the mass ratio of the organic monomer to the cross-linking agent is 5:1-30: 1;
the dispersant is ammonium polymethacrylate, PEI, phosphate ester or ammonium polyacrylate, etc., and the addition amount of the dispersant is 0.1-2.5% of the weight of the silicon nitride and the auxiliary agent ceramic powder;
the ball-material ratio in the ball-milling tank is 0.5:1-3:1, the solid content of the slurry is 20-50%, and the ball-milling time is 2-48 h; the sintering aid is 6-12% and is oxides or fluorides of magnesium oxide, yttrium oxide, ytterbium oxide, lanthanum oxide, strontium oxide, neodymium oxide, yttrium fluoride, magnesium fluoride and the like.
3. The method of claim 1, wherein the method comprises: in S2 based on the molding process: the plasticizer is glycerol, polyethylene glycol, phthalate, polyether glycol and oleic acid or a mixture of the glycerol, the polyethylene glycol, the phthalate, the polyether glycol and the oleic acid, the addition amount of the plasticizer is 0.1-10% of the weight of the silicon nitride and the auxiliary agent ceramic powder, and the plasticizer is adjusted according to the thickness of the tape-casting sheet.
4. The method of claim 1, wherein the method comprises: in S3 based on the molding process: stirring at 30-100 rpm for 5-30 min;
the initiator is azobisisobutylamidine dihydrochloride, tetraethylpentamine or 3, 3' -diaminodipropylamine and the like, and the addition amount of the initiator is 0.25-10% of that of the organic monomer.
5. The method of claim 1, wherein the method comprises: in S4 based on the molding process: the speed of the casting belt is 0.2m/min-5m/min, the temperature of the heating zone of the casting belt is 40-60 ℃, and the curing time is 10min-60 min; and adjusting various parameters of the casting machine according to the thickness of the casting sheet.
6. The method of claim 1, wherein the method comprises: in S5 based on the molding process: drying at 30-60 deg.C for 30min-4 h;
and drying the blank to a certain degree, peeling the blank sheet from the casting film, and then cutting and punching to obtain the ceramic blank sheet.
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