CN114751754B - Preparation method of silicon nitride ceramic substrate biscuit - Google Patents

Preparation method of silicon nitride ceramic substrate biscuit Download PDF

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CN114751754B
CN114751754B CN202210568487.8A CN202210568487A CN114751754B CN 114751754 B CN114751754 B CN 114751754B CN 202210568487 A CN202210568487 A CN 202210568487A CN 114751754 B CN114751754 B CN 114751754B
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silicon nitride
biscuit
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陈明
郭天枫
陈玉衡
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Jiangsu Fangda Zhengyuan Electronic Material Technology Co ltd
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Abstract

The invention provides a preparation method of a silicon nitride ceramic substrate biscuit, which comprises the following steps: s1: will market the alpha-Si 3 N 4 Pretreating the powder and the rare earth oxide; s2: preparing micro-nano slurry: n is a radical of hydrogen 2 Respectively adding the pretreated commercial alpha-Si under protection 3 N 4 Mixing the powder and the rare earth oxide in a mixer in proportion to generate S 0 (ii) a Addition of polysiloxanes to commercially available dispersants to form L 1 Mixing a nonaqueous plasticizer and a wetting agent to obtain a mixture L 2 (ii) a Adding a nonaqueous binder and an organic solvent in N 2 Fully stirring and dissolving under the protection to prepare liquid solution L 3 (ii) a Will S 0 、L 1 、L 2 And L 3 Mixing and sanding to prepare micro-nano slurry J 0 And S3: preparing a casting sheet; s4: preparing a biscuit; s5: the prepared rough substrate of the silicon nitride substrate has the measurement performance, the measured thermal conductivity of the rough substrate of the biscuit prepared by the invention is over 85W/(m.K), the thermal conductivity is obviously improved compared with the thermal conductivity of the silicon nitride substrate prepared by the prior art, and the measured fracture toughness is 6.5MPa/m 2 As described above.

Description

Preparation method of silicon nitride ceramic substrate biscuit
Technical Field
The invention relates to the technical field of a preparation process of a commercialized silicon nitride ceramic substrate, in particular to a preparation method of a biscuit of a silicon nitride ceramic substrate.
Background
In recent years, the miniaturization of electronic components and the rapid development of large-scale integrated circuits have made higher demands on ceramic insulating substrates used for them. In certain fields, it is required that the ceramic substrate should have not only a high thermal conductivity but also sufficient toughness.
The existing preparation methods of the silicon nitride ceramic substrate mainly comprise two methods: one is to sinter a silicon nitride ceramic block and then cut it into silicon nitride substrates of the desired thickness, but the cost of preparing silicon nitride ceramic substrates by this method is high. The other method is to prepare a silicon nitride blank sheet with the required thickness by a tape casting method, and then prepare the silicon nitride ceramic substrate by proper binder removal and sintering processes. This method is clearly of great advantage for reducing production costs compared to the former preparation method.
Although casting techniques are well established for industrial production, there are still many problems with the casting of silicon nitride ceramic substrates: firstly, the thermal conductivity and mechanical properties of the silicon nitride ceramic substrate prepared by the prior art are not uniform, so that the ceramic substrate has poor performances such as thermal conductivity, strength and toughness; secondly, the thermal conductivity of the ceramic substrate prepared by tape casting is poor and is lower than 70W/(m.k), and thirdly, slurry needs to be prepared in the tape casting process, and the slurry prepared by the existing preparation method is difficult to exhaust, so that the time consumed in the defoaming process is long; fourth, the prior art may cause oxidation reaction when preparing the tape casting slurry, affecting the performance and quality of the prepared substrate.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method of a silicon nitride ceramic substrate biscuit.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a biscuit of a silicon nitride ceramic substrate is characterized by comprising the following steps: the method comprises the following steps:
s1: commercially available alpha-Si is added 3 N 4 Pretreating the powder and the rare earth oxide: high temperature N 2 Para alpha-Si 3 N 4 Drying the powder and the rare earth oxide and discharging oxygen; at N 2 para-alpha-Si under protection 3 N 4 The powder and the rare earth oxide are pretreated for drying and oxygen discharging to ensure alpha-Si 3 N 4 Purity of powder and rare earth oxide, avoiding alpha-Si 3 N 4 The powder and the rare earth oxide are oxidized, which causes the quality and performance of the prepared ceramic substrate to be poor.
S2: preparing micro-nano slurry:
N 2 respectively adding the pretreated commercial alpha-Si under protection 3 N 4 Mixing the powder and the rare earth oxide in a mixer in proportion to generate S 0 (ii) a The ceramic substrate is fully and uniformly mixed through the mixer, so that the phenomenon that the ceramic substrate manufactured in the prior art is uneven in heat conductivity and mechanical property is prevented. Addition of a polysiloxane to a commercially available dispersant to form L 1 Mixing a non-aqueous plasticizer and a wetting agent in a certain proportion to form L 2 (ii) a Adding a non-aqueous binder and a certain amount of organic solvent in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 (ii) a Will S 0 、L 1 、L 2 And L 3 Mixing the raw materials in proportion, grinding the mixture in a sand mill to prepare micro-nano slurry J 0 Through N 2 Fully stirring and dissolving under the protection to prepare liquid solution L 3 Preventing oxygen charging, while S 0 The oxygen is discharged through pretreatment, and S is 0 、L 1 、L 2 And L 3 Mixing the raw materials in proportion, grinding the mixture in a sand mill to prepare micro-nano slurry J 0 The low oxygen content in the slurry is ensured, so that the oxygen content in the prepared biscuit is relatively low, the O/N ratio in the substrate is relatively low, and the thermal conductivity of the substrate is increased.
S3: preparing a casting sheet: mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1 (ii) a Slurry J 0 The oxygen content in the slurry is low, so that part of gas remaining in the slurry is easily foamed and discharged in the defoaming process, the exhaust is convenient, the oxygen content in the slurry is further reduced through secondary defoaming treatment, the O/N ratio is reduced, and the thermal conductivity of the generated substrate is improved.
S4: preparing a biscuit: a plurality of pieces P 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing to form a biscuit P 2 (ii) a Prevention of biscuit P formation 2 With blistering or delamination, ensuring a biscuit P 2 Of the mass of (c).
S5: preparing a silicon nitride substrate blank: the biscuit P is put 2 After the glue is discharged, the silicon nitride substrate rough plate is sintered in a vacuum pressure sintering furnace at 1850-1950 ℃ to obtain the silicon nitride substrate rough plate. The thermal conductivity and mechanical toughness of the silicon nitride substrate blank were measured by preparing the silicon nitride substrate blank.
Preferably, the ratio of dispersant to polysiloxane in S2 = 100; plasticizer, humectant = 1-100; binder organic solvent =100, and the above ratio is a weight ratio.
Preferably, the rare earth oxide comprises MgF 2 CaO and Y 2 O 3 ,N 2 Respectively adding pretreated commercial alpha-Si under protection 3 N 4 Powder, mgF 2 、CaO and Y 2 O 3 Respectively preparing micro-nano powder S from equal rare earth oxides 1 、S 2 、S 3 And S 4 Then, the S is 1 、S 2 、S 3 And S 4 Mixing in a mixer according to a certain proportion, and fully mixing to generate S 0 . At N 2 Commercial alpha-Si to be pretreated under protection 3 N 4 Powder, mgF 2 CaO and Y 2 O 3 Respectively grinding the rare earth oxide to obtain micro-nano powder, and preventing the rare earth oxide or alpha-Si from being oxidized during the process of preparing the micro-nano powder 3 N 4 The powder contacts with oxygen in the air to generate oxidation reaction, resulting in rare earth oxide or alpha-Si 3 N 4 The purity of the powder is reduced, which affects the quality of the finally manufactured substrate; simultaneous rare earth oxide powder and alpha-Si 3 N 4 The powder is micro-nano powder, the particle size of the powder is ensured to be nano-scale fine particles, and S is mixed by a mixer 1 、S 2 、S 3 And S 4 Can be fully mixed, and the phenomenon of uneven thermal conductivity and mechanical property is avoided, so that the thermal conductivity and mechanical property of the prepared silicon nitride substrate are improved.
Preferably, said S 1 、S 2 、S 3 And S 4 Respectively alpha-Si with purity of more than 99.99 percent 3 N 4 Powder and chemically pure MgF 2 CaO and Y 2 O 3 (ii) a Ensuring alpha-Si 3 N 4 Powder, mgF 2 CaO and Y 2 O 3 By alpha-Si with a purity of more than 99.99% 3 N 4 Powder reduction of alpha-Si 3 N 4 beta-Si contained in the powder 3 N 4 Amount of powder, avoiding beta-Si 3 N 4 The powder causes low thermal conductivity of the generated silicon nitride substrate; s is 1 、S 2 、S 3 And S 4 Respectively weight of m 1 、m 2 、m 3 And m 4 In a ratio of m 1 :m 2 :m 3 :m 4 =100:0.1~10:0.1~10:0.1~10,m 1 +m 2 +m 3 +m 4 =m 0
Preferably, the dispersant is one or a mixture of several of castor oil, fatty acid (glycerol trioleate), natural fish oil, synthetic surfactant, benzene sulfonic acid, fish oil, oleic acid and methyl octadiene;
the non-aqueous plasticizer comprises one or a mixture of a plurality of polyethylene glycol, tricresyl phosphate and phthalate ester mixture;
the non-aqueous binder is one or a mixture of more of nitrocellulose, petroleum resin, polyethylene, polyacrylate, polymethacrylic acid, polyvinyl alcohol, vinyl chloride, polymethacrylate and ethyl cellulose;
the wetting agent is polyoxyethylene ester;
the solvent is one or a mixture of a plurality of acetone, ethanol, benzene, butanol, diacetone, methyl isobutyl ketone, xylene and trichloroethylene.
Preferably, one kind of slurry J 0 Is composed of S 0 、L 1 、L 2 And L 3 The micro-nano-scale slurry obtained by grinding through the sand mill after mixing according to the proportion is ground to generate the micro-nano-scale slurry, so that all components in the slurry are uniformly mixed, the probability of generating air holes or layering in the tape-casting sheet can be reduced through the micro-nano-scale slurry, the quality of the tape-casting sheet is improved, and meanwhile, the phenomenon of agglomeration is not easy to occur in the tape-casting process. S 0 :L 1 :L 2 :L 3 =100:0.1~5:0.1~10:30~70。
Preferably, the condition of the warm isostatic pressing in S4 is that the isostatic pressing machine carries out static pressing for 20-50 min under the pressure condition of 30-40 MPa. Casting sheet P by isostatic pressing machine 1 Pressing to reduce the biscuit P 2 Casting sheet P of (1) 1 The phenomenon of layering or air bubbles appears between the two parts, and the biscuit P is ensured 2 Thereby improving the thermal conductivity and mechanical properties of the resulting silicon nitride substrate.
Preferably, said casting sheet P 1 The drying temperature of (2) is not more than 40 ℃. Prevent too high temperature of stoving from leading to liquid drying rate too fast, cause and flowExtension sheet P 1 Cracks, breaks or voids are generated inside, thereby reducing the quality of the finished cast sheet.
Preferably, said casting sheet P 1 The thickness of (2) is 10 mu m to 10 cm. In real life, because the silicon nitride substrate has different requirements on thickness according to different requirements, the invention adopts the casting sheet P 1 To meet the thickness requirement of the silicon nitride substrate to be produced.
Compared with the prior art, the invention has the beneficial effects that: (1) The invention passes through N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 Preventing oxygen charging, while S 0 Performing oxygen discharge through pretreatment, and discharging S 0 、L 1 、L 2 And L 3 Mixing the raw materials in proportion, grinding the mixture in a sand mill to prepare micro-nano slurry J 0 The low oxygen content in the slurry is ensured, so that the oxygen content in the prepared biscuit is relatively low, and the O/N ratio in the substrate is relatively low, thereby increasing the thermal conductivity of the substrate; the thermal conductivity measured by the substrate rough plate prepared by the biscuit is more than 85W/(m.K), the highest thermal conductivity in the embodiment can reach 92.6W/(m.K), and compared with the thermal conductivity of the silicon nitride substrate prepared in the prior art, the thermal conductivity is obviously improved. (2) The invention firstly carries out the reaction on the commercial alpha-Si 3 N 4 Pretreating the powder and the rare earth oxide: high temperature N 2 Para alpha-Si 3 N 4 Drying the powder and rare earth oxide and discharging oxygen to avoid alpha-Si 3 N 4 The powder and the rare earth oxide are oxidized to reduce the oxygen content, N, in the powder 2 Fully stirring and dissolving under the protection to prepare liquid solution L 3 The method has the advantages that oxygen is prevented from being filled, the oxygen content in the slurry is ensured to be low, the oxygen content in the prepared biscuit is lower, in the defoaming process, part of residual gas in the biscuit is easily foamed and discharged, the exhaust is convenient, the exhaust time is short, and the production efficiency of the slurry is improved. (3) N of the invention 2 Respectively adding pretreated commercial alpha-Si under protection 3 N 4 Mixing the powder and the rare earth oxide in proportion in a mixer to generate S 0 (ii) a And before mixingNeed to be in N 2 Respectively adding the pretreated commercial alpha-Si under protection 3 N 4 Powder of MgF 2 CaO and Y 2 O 3 Respectively preparing the rare earth oxides into micro-nano powder, ensuring the particle size of the powder to be nano-scale fine particles, fully and uniformly mixing the powder by a mixer, and avoiding the phenomenon of non-uniform heat conductivity and mechanical properties, thereby improving the heat conductivity and mechanical toughness of the prepared silicon nitride substrate, wherein the fracture toughness measured by the silicon nitride substrate blank prepared by the biscuit prepared by the method is 6.5MPa/m 2 As described above. (4) The alpha-Si 3N4 powder and the rare earth oxide of the invention are all in N 2 Pretreating to remove oxygen under protection, grinding into micro-nano powder, mixing, and avoiding the rare earth oxide or alpha-Si due to oxidation reaction caused by introducing oxygen into the prepared slurry 3 N 4 The purity of the powder is reduced, affecting the quality of the final substrate.
Drawings
FIG. 1 is a table 1 of the present invention: the properties of the silicon nitride substrate blanks obtained in examples 1 to 4.
Detailed Description
In order to further understand the objects, structures, features and functions of the present invention, the following embodiments are described in detail.
Firstly, to the commercial alpha-Si 3 N 4 Pretreating the powder and the rare earth oxide: high temperature N 2 Para alpha-Si 3 N 4 Powder of MgF 2 CaO and Y 2 O 3 And drying and oxygen discharging operation. alpha-Si 3 N 4 The purity of the powder is better than 99.99 percent, and MgF 2 CaO and Y 2 O 3 Are all chemically pure. Then at N 2 Respectively adding the pretreated commercial alpha-Si under protection 3 N 4 Powder of MgF 2 CaO and Y 2 O 3 Respectively preparing micro-nano powder S 1 、S 2 、S 3 And S 4
Example 1:
weighing S 1 Is 100g, S 2 5.0g of S in the amount of 3 3.0g of S in the total amount 4 Is 2.0g, under the protection of N2Fully mixing the materials in a mixer to generate S with the mass of 110g 0
Addition of a certain amount of a polysiloxane to a commercially available dispersant to form L 1 Wherein the weight ratio of the dispersant to the polysiloxane is 100.
A nonaqueous plasticizer and a wetting agent were mixed at a ratio of 100.5 to produce L 2
Adding a non-aqueous binder and a certain amount of organic solvent in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 Wherein, the binder is organic solvent = 100.0;
then weighing 100 parts of S by weight respectively 0 2.1 parts by weight of L 1 1 part by weight of L 2 50 parts by weight of L 3 Mixing, grinding in a sand mill to prepare micro-nano slurry J 0 Mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing 32 pieces of P1 to form a biscuit P 2 From P to P 2 After the binder removal, the silicon nitride substrate blank is sintered at 1900 ℃ in a vacuum pressure sintering furnace to obtain the silicon nitride substrate blank for performance measurement, and the measurement results are shown in table 1. As is clear from Table 1, the thermal conductivity of example 1 was as high as 92.6W/(m.K), and the fracture toughness was 7.2MPa/m 2
Example 2:
weighing S 1 Is 100g, S 2 Is 5.5g of 3 Is 2.0g in S 4 1.5g of the mixture is placed in a blender to be fully mixed under the protection of N2 to generate S with the mass of 109g 0
Addition of a certain amount of a polysiloxane to a commercially available dispersant to form L 1 Wherein the weight ratio of the dispersant to the polysiloxane is 100.
A nonaqueous plasticizer and a wetting agent were mixed at a ratio of 100 2
Adding a non-aqueous binder and a certain amount of organic solvent in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 Wherein, the binder is organic solvent = 100;
then respectively weighing100 parts by weight of S 0 1.8 parts by weight of L 1 2 parts by weight of L 2 50 parts by weight of L 3 Mixing, grinding in a sand mill to obtain micro-nano slurry J 0 Mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing 32 pieces of P1 to form a biscuit P 2 A 1 is to P 2 After the binder removal, the silicon nitride substrate blank is sintered at 1900 ℃ in a vacuum pressure sintering furnace to obtain the silicon nitride substrate blank for performance measurement, and the measurement results are shown in table 1. As is clear from Table 1, the thermal conductivity of example 2 was 87.6W/(m.K), and the fracture toughness was 6.8MPa/m 2
Example 3:
weighing S 1 Is 100g, S 2 7.0g of S was contained in the total amount 3 Is 2.2g, S 4 2.5g of the mixture is placed in a blender to be fully mixed under the protection of N2 to generate S with the mass of 111.7g 0
Addition of a certain amount of a polysiloxane to a commercially available dispersant to form L 1 Wherein the weight ratio of the dispersing agent to the polysiloxane is 100.
A nonaqueous plasticizer and a wetting agent were mixed at a ratio of 100 2
Adding a non-aqueous binder and a certain amount of organic solvent in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 Wherein, the binder is organic solvent = 100.0;
then weighing 100 parts of S by weight respectively 0 0.9 parts by weight of L 1 3 parts by weight of L 2 50 parts by weight of L 3 Mixing, grinding in a sand mill to prepare micro-nano slurry J 0 Mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing 32 pieces of P1 to form a biscuit P 2 From P to P 2 After the binder removal, the silicon nitride substrate blank is sintered at 1900 ℃ in a vacuum pressure sintering furnace to obtain the silicon nitride substrate blank for performance measurement, and the measurement results are shown in table 1. As is clear from Table 1, the thermal conductivity of example 3 was as high as 85.4W/(mK)) The fracture toughness is 7.5MPa/m 2
Example 4:
weighing S 1 Is 100g, S 2 Is 3.5g of 3 Is 3.8g of S 4 3.1g, and the mixture is placed in a mixer under the protection of N2 to be fully mixed to generate S with the mass of 110.4g 0
Addition of a certain amount of a polysiloxane to a commercially available dispersant to form L 1 Wherein the weight ratio of the dispersant to the polysiloxane is 100.
A nonaqueous plasticizer and a wetting agent were mixed at a ratio of 100.0 to produce L 2
Adding a non-aqueous binder and a certain amount of organic solvent in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 Wherein, the binder is organic solvent = 100.0;
then weighing 100 parts of S by weight respectively 0 2.4 parts by weight of L 1 4 parts by weight of L 2 50 parts by weight of L 3 Mixing, grinding in a sand mill to prepare micro-nano slurry J 0 Mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing 32 pieces of P1 to form a biscuit P 2 A 1 is to P 2 After the binder removal, the silicon nitride substrate blank was sintered at 1900 ℃ in a vacuum pressure sintering furnace to obtain silicon nitride substrate blanks for performance measurement, and the measurement results are shown in table 1. As is clear from Table 1, the thermal conductivity of example 4 was 88.6W/(m.K), and the fracture toughness was 7.4MPa/m 2
Casting sheet P obtained in examples 1 to 4 1 0.01 cm thick, prepared tape casting sheet P 1 All dried at 35-37 ℃, cut, screened, laminated and sealed, and then placed in an isostatic press to be statically pressed for 50min under the pressure condition of 30MPa, thereby ensuring that the biscuit P prepared in the examples 1-4 2 The production conditions of (1) were the same, and the dispersant used in the experiments of examples 1 to 4 was castor oil, and the nonaqueous plasticizer was polyethylene glycol; the non-aqueous binder is butylene acetate cellulose, the wetting agent is allyl polyether alcohol, and the organic solvent is ethanol.
As can be seen from Table 1, the thermal conductivity of example 1 can reach 92.6W/(m.K) at most, the thermal conductivity of examples 2 to 4 is poorer than that of example 1, but the thermal conductivity of the examples is more than 85W/(m.K), the thermal conductivity is remarkably improved compared with that of the silicon nitride substrate prepared in the prior art, and the fracture toughness measured by the substrate rough plates prepared by the biscuit of examples 1 to 4 of the invention is 6.5MPa/m 2 As described above, the toughness is high, and the requirement for the toughness of the silicon nitride substrate is satisfied.
The present invention has been described in relation to the above embodiments, which are only exemplary of the implementation of the present invention. It should be noted that the disclosed embodiments do not limit the scope of the invention. Rather, it is intended that all such modifications and variations be included within the spirit and scope of this invention.

Claims (4)

1. A preparation method of a silicon nitride ceramic substrate biscuit is characterized by comprising the following steps: the method comprises the following steps:
s1: will market the alpha-Si 3 N 4 Pretreating the powder and the rare earth oxide: high temperature N 2 Para alpha-Si 3 N 4 Drying the powder and the rare earth oxide and discharging oxygen;
s2: preparing micro-nano slurry:
N 2 respectively adding pretreated commercial alpha-Si under protection 3 N 4 Mixing the powder and the rare earth oxide in proportion in a mixer to generate S 0 (ii) a Addition of a polysiloxane to a commercially available dispersant to form L 1 Mixing a non-aqueous plasticizer and a wetting agent in a certain proportion to produce L 2 (ii) a A non-aqueous binder and a certain amount of organic solvent are added in N 2 Fully stirring and dissolving under protection to prepare liquid solution L 3 (ii) a Will S 0 、L 1 、L 2 And L 3 Proportionally mixing, grinding in sand mill to obtain micro-nano slurry J 0
S3: preparing a casting sheet: mixing the slurry J 0 Casting into casting sheet P after secondary defoaming 1
S4: preparing a biscuit: a plurality of pieces P 1 Drying, cutting, screening, laminating, sealing and warm isostatic pressing to form a biscuit P 2
S5: preparing a silicon nitride substrate blank: a biscuit P is put 2 After the glue is discharged, sintering the blank in a vacuum pressure sintering furnace to obtain a silicon nitride substrate blank;
the rare earth oxide comprises MgF 2 CaO and Y 2 O 3 ,N 2 Respectively adding pretreated commercial alpha-Si under protection 3 N 4 Powder, mgF 2 CaO and Y 2 O 3 Respectively preparing micro-nano powder S 1 、S 2 、S 3 And S 4 Then, the S is 1 、S 2 、S 3 And S 4 Mixing the raw materials in a mixer in proportion to generate S 0 (ii) a The ratio of the dispersing agent to the polysiloxane in S2 is = 100; plasticizer, wetting agent = 1-100; binder, organic solvent = 100; s is 1 、S 2 、S 3 And S 4 Respectively alpha-Si with purity of more than 99.99 percent 3 N 4 Powder and chemically pure MgF 2 CaO and Y 2 O 3 (ii) a S is 1 、S 2 、S 3 And S 4 Respectively weight of m 1 、m 2 、m 3 And m 4 In a ratio of m 1 :m 2 :m 3 :m 4 =100:0.1~10:0.1~10:0.1~10,m 1 +m 2 +m 3 +m 4 =m 0 (ii) a The dispersing agent is one or a mixture of a plurality of castor oil, fatty acid, benzene sulfonic acid, fish oil, oleic acid and methyl octadiene;
the non-aqueous plasticizer comprises one or a mixture of a plurality of polyethylene glycol, tricresyl phosphate and phthalate ester mixture;
the non-aqueous binder is one or a mixture of more of nitrocellulose, petroleum resin, polyethylene, polyacrylate, polymethacrylene, polyvinyl alcohol, chloroethylene, polymethacrylate and ethyl cellulose;
the wetting agent is polyoxyethylene ester;
the organic solvent is one or a mixture of a plurality of acetone, ethanol, benzene, butanol, diacetone, methyl isobutyl ketone, xylene and trichloroethylene; the slurry J 0 Is formed by S 0 、L 1 、L 2 And L 3 Mixing the raw materials in proportion, grinding the mixture by a sand mill to obtain micro-nano slurry S 0 :L 1 :L 2 :L 3 =100:0.1~5:0.1~10:30~70。
2. The method of making a silicon nitride ceramic substrate biscuit of claim 1, wherein: and the condition of the medium temperature isostatic pressing in the S4 is that the isostatic pressing machine carries out hydrostatic pressing for 20-50 min under the pressure condition of 30-40 MPa.
3. The method of making a silicon nitride ceramic substrate biscuit of claim 1 wherein: the casting sheet P 1 The drying temperature of (A) is not more than 40 ℃.
4. The method of making a silicon nitride ceramic substrate biscuit of claim 1 wherein: the casting sheet P 1 The thickness of (2) is 10 mu m to 10 cm.
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