Electronic ceramic slurry and preparation method thereof

Abstract

The invention discloses electronic ceramic slurry and a preparation method thereof, and relates to the technical field of electronic ceramic processing. Comprising the following steps: step 1, preparing sol: S1.1, preparing silicon nitride powder, lauryl sodium sulfate, modified polyvinyl alcohol, polyethylene glycol-400, a sintering aid and an ethanol water solution as materials; s1.2, in a nitrogen atmosphere, sequentially putting the materials into a mixing tank, and homogenizing to obtain a glue solution; step 2, ball milling and defoaming: transferring the glue solution into a ball milling tank, grinding and pulping, defoaming after the granularity requirement and the blade coating requirement are met, and finally filtering and deironing to obtain the electronic ceramic slurry. The automatic continuous preparation method of the electronic ceramic slurry provided by the invention has the beneficial effects that the adhesive polyvinyl alcohol is correspondingly modified in the process; meanwhile, in order to improve the dispersion effect of the sintering aid, the surface of the diatomite is chemically modified, so that the diatomite is used as a carrier of the sintering aid, and the product quality is effectively improved.

Description

Technical Field

[0001] The invention relates to the technical field of electronic ceramic processing, in particular to an electronic ceramic slurry and a preparation method thereof. Background Art

[0002] With the development of the third-generation semiconductor technology, packaging technology accounts for an increasingly higher proportion in the entire semiconductor industry. Electronic ceramics are a very important packaging material. Electronic ceramics mainly include: silicon nitride, aluminum nitride, aluminum oxide, and zirconium oxide. Its front-end process uses the tape casting method. The prerequisite for obtaining a good green body is the preparation of high-quality slurry.

[0003] The commonly used electronic ceramic preparation process currently includes sol-gel-ball milling-degassing: these three steps are limited by the requirements for slurry quality and are currently operated in an independent and intermittent manner. The current problems are as follows: there are high requirements for personnel's on-site handling capabilities and operational proficiency: personnel training normally takes 30-60 days, and the training cycle is long, which is not conducive to expanded mass production; the material weighing accuracy and the degree of control of the material flow process basically depend on human behavior: it is impossible to obtain a standard slurry with controllable performance indicators, and the quality control risk factor is high; the glue preparation process is in an open state: the glue is prone to crusting, easy to contaminate, and the discharge time is too long; the pulping process is a semi-closed system, and there is a risk of pollution: it is not conducive to the stable preparation of high-precision ceramic products, nor is it conducive to the expanded mass production of products; the slurry needs to be transferred a certain distance after degassing: the slurry is in a shaking state during this process, affecting the stability of the slurry.

[0004] Therefore, in order to solve the above problems, the present invention prepares an electronic ceramic slurry. Summary of the invention

[0005] The object of the present invention is to provide an electronic ceramic slurry and a preparation method thereof to solve the problems raised in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing an electronic ceramic slurry comprises the following steps:

[0008] Step 1: Sol:

[0009] S1.1: prepare silicon nitride powder, sodium dodecyl sulfate, modified polyvinyl alcohol, polyethylene glycol-400, sintering aid, and ethanol aqueous solution as materials; S1.2: under nitrogen atmosphere, place the materials in a mixing tank in turn for homogenization to obtain a glue solution;

[0010] Step 2: Ball milling and degassing:

[0011] The glue solution is transferred to a ball mill, ground and slurried to meet the particle size requirements and coating requirements, degassed, and finally filtered and iron-removed to obtain electronic ceramic slurry.

[0012] More optimally, in step 1, the specific process of S1.2 is: under a nitrogen atmosphere, the materials are gradually added to the mixing tank. During this process, the parameters are first set to a stirring rate of 8-12 r / min and a dispersion rate of 250-300 r / min, and maintained for 8-12 min, and then the parameters are set to a stirring rate of 15-20 r / min and a dispersion rate of 700-800 r / min, and maintained for 15-20 min; after all the materials are introduced, the parameters are set to a stirring rate of 30 r / min, a dispersion rate of 1500 r / min, a vacuum degree of -0.01 to -0.03 MPa, and a water heating cycle with a mold temperature controller of 45 to 50°C, and maintained for 9 to 10 hours to obtain a glue solution.

[0013] More optimally, in step 2, vertical stirring is adopted during the grinding and pulping process; the grinding includes four stages of pre-dispersion, auxiliary agent mixing stage, grinding and rubber grinding, wherein the speed of pre-dispersion is 50-55r / min, and the time is 30-40min; the speed of the auxiliary agent mixing stage is 80-90r / min, and the time is 1-2h; the grinding is first at 90-95r / min, maintained for 1-2h, and then at 60-65r / min, maintained for 330-350min; the speed of rubber grinding is 70-75r / min, and the time is 4-5h.

[0014] More optimally, in step 2, degassing is performed by online continuous degassing, at room temperature, vacuum degree -50 to -60 KPa, rotation speed frequency 50 to 55 Hz, and time 1.5 to 2 h.

[0015] More optimally, the particle size requirement is that the D50 control range is 0.6±0.2μm; the scraping requirement is that the number of surface convex points is ≤6.

[0016] More optimally, the materials of the electronic ceramic slurry include the following substances: by weight mass fraction, 40-50% silicon nitride powder, 1-2% sodium dodecyl sulfate, 5-10% modified polyvinyl alcohol, 1-2% polyethylene glycol-400, 10-12% sintering aid, and the rest is 10-15% by volume ethanol aqueous solution.

[0017] More optimally, the preparation process of the modified polyvinyl alcohol is:

[0018] S1: Glycidyl methacrylate, N,N-dimethylethanolamine, triethylamine and tetrahydrofuran are mixed, stirred evenly, heated to 85-95°C, reacted for 4-8h, cooled to room temperature, extracted with ethyl acetate, dried, and concentrated to obtain tertiary aminated methacrylate;

[0019] S2: Mix tertiary aminated methacrylate, polyvinyl alcohol and deionized water, adjust the pH value to acidic, stir evenly at high speed, add ammonium cerium nitrate solution, heat to 50-60°C, react for 8-10 hours, cool to room temperature, then add 1,3-propane sultone solution, continue to heat to 40-50°C, react for 1-2 hours, filter, wash and dry after cooling to obtain modified polyvinyl alcohol.

[0020] More optimally, the raw materials of the tertiary aminated methacrylate include the following substances: by weight, 16 to 18 parts of glycidyl methacrylate, 10 to 12 parts of N,N-dimethylethanolamine, 0.1 to 0.2 parts of triethylamine, and 100 to 150 parts of tetrahydrofuran;

[0021] The modified polyvinyl alcohol raw material comprises the following substances: by weight, 4-5 parts of tertiary aminated methacrylate, 8-10 parts of polyvinyl alcohol, 110-120 parts of deionized water, 0.5-0.8 parts of cerium ammonium nitrate solution, and 1-2 parts of 1,3-propane sultone solution.

[0022] More optimally, the preparation process of the sintering aid is as follows: in a nitrogen atmosphere, mercapto diatomite, tertiary aminated methacrylate, and isopropanol are mixed, azobisisobutyronitrile is added, the temperature is raised to 50-60° C., the reaction is carried out under light for 1-2 hours, the mixture is cooled to room temperature, washed, and transferred to acetone after drying, 1,3-propane sultone solution is added, the temperature is continued to be raised to 40-50° C., and the reaction is carried out for 1-2 hours to obtain modified diatomite; the modified diatomite, magnesium oxide, chlorine oxide, yttrium oxide, and isopropanol are mixed, and stirred for 3-4 hours to obtain a sintering aid;

[0023] The modified diatomaceous earth comprises the following components: by weight, 20 to 25 parts of mercapto diatomaceous earth, 10 to 12 parts of tertiary aminated methacrylate, 100 to 120 parts of isopropanol, 0.1 to 0.2 parts of azobisisobutyronitrile, 60 to 70 parts of acetone, and 1 to 2 parts of 1,3-propane sultone solution;

[0024] The sintering aid comprises the following components: by weight, 4 to 5 parts of modified diatomaceous earth, 1 to 2 parts of magnesium oxide, 1 to 2 parts of chlorine oxide, 1 to 2 parts of yttrium oxide, and 50 to 60 parts of isopropanol.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The present invention provides an automated continuous preparation method for electronic ceramic slurry, during which the adhesive polyvinyl alcohol is modified accordingly; at the same time, in order to improve the dispersion effect of the sintering aid, the surface of diatomite is chemically modified so that it acts as a carrier of the sintering aid, effectively improving the quality of the product. The details are as follows:

[0027] First, the present invention optimizes the traditional intermittent operation mode into continuous production through an automated continuous pulping process, thereby significantly improving production efficiency; the invention adopts technologies such as nitrogen replacement, online centrifugal degassing and strong magnetic iron removal filtration to avoid crusting and contamination caused by contact between the slurry and air, and the particle size control of the slurry is more precise, the scraping surface has almost no protrusions, the iron content is significantly reduced, and the uniformity, stability and purity of the slurry are significantly improved;

[0028] Second, the invention introduces zwitterionic chain segments into the polyvinyl alcohol molecular chain, which not only breaks the regularity of the molecular chain and reduces its crystallinity, but also can well adjust the viscosity and fluidity of the slurry and reduce the use of plasticizers; and the zwitterionic chain segments have the characteristics of coexistence of positive and negative charges, and can interact with the solid particles in the slurry through electrostatic action to prevent particle agglomeration;

[0029] Third: By chemically modifying the surface of diatomite with zwitterionic segments; magnesium oxide, chlorine oxide, and yttrium oxide can combine with its surface through chemical bonds or physical adsorption, so that the additives are evenly distributed on the surface of diatomite, avoiding the agglomeration of the additives, ensuring that they play a role evenly during the sintering process, and improving the mechanical strength of the sintered ceramic material. DETAILED DESCRIPTION

[0030] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work shall fall within the scope of protection of the present invention.

[0031] It should be noted that the following parts are parts by weight, and the purchase manufacturers of all raw materials involved in the present invention are not subject to any special restrictions and are exemplified as follows: In the following embodiments, glycidyl methacrylate CAS is 106-91-2, N,N-dimethylethanolamine CAS is 108-01-0, and 1,3-propane sultone CAS is 1120-71-4.

[0032] The preparation process of modified polyvinyl alcohol is:

[0033] S1: 16 parts of glycidyl methacrylate, 10 parts of N,N-dimethylethanolamine, 0.1 parts of triethylamine and 100 parts of tetrahydrofuran were mixed, stirred evenly, heated to 85°C, reacted for 4 hours, cooled to room temperature, extracted the product with ethyl acetate, dried, and concentrated to obtain tertiary aminated methacrylate;

[0034] S2: Mix 4 parts of tertiary aminated methacrylate, 8 parts of polyvinyl alcohol, and 110 parts of deionized water, adjust the pH value to acidic, stir evenly at high speed, add 0.5 parts of ammonium cerium nitrate solution, heat to 50°C, react for 8 hours, cool to room temperature, then add 1 part of 1,3-propane sultone solution, continue to heat to 40°C, react for 1 hour, filter, wash, and dry after cooling to obtain modified polyvinyl alcohol.

[0035] The preparation process of the sintering aid is:

[0036] (1) Under nitrogen, 25 parts of mercapto diatomite, 12 parts of tertiary aminated methacrylate, and 120 parts of isopropanol were mixed, 0.2 parts of azobisisobutyronitrile were added, the temperature was raised to 50°C, the mixture was reacted under light for 1-2 hours, the mixture was cooled to room temperature, washed, dried, and then transferred to 70 parts of acetone, 2 parts of 1,3-propane sultone solution were added, the temperature was further raised to 40°C, and the mixture was reacted for 1 hour to obtain modified diatomite; 5 parts of modified diatomite, 2 parts of magnesium oxide, 2 parts of chlorine oxide, 2 parts of yttrium oxide, and 60 parts of isopropanol were mixed and stirred for 3 hours to obtain a sintering aid.

[0037] Embodiment 1: A method for preparing an electronic ceramic slurry comprises the following steps:

[0038] Step 1: Sol:

[0039] S1.1: Prepare silicon nitride powder, triolein, modified polyvinyl alcohol, dibutyl phthalate, sintering aid, and ethanol aqueous solution as materials; the mass fraction of the materials is: 40% silicon nitride powder, 1% sodium dodecyl sulfate, 5% modified polyvinyl alcohol, 1% polyethylene glycol-400, 10% sintering aid, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10r / min, then increase the speed to 800r / min, and disperse for 20min; after all the materials are added, heat the water bath to 50℃, stir at 30r / min at -0.03MPa, then increase the speed to 1500r / min, disperse for 10h, and obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0040] Step 2: The glue solution of step 1 is transferred to a ball mill through air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding of glue; wherein the speed of the pre-dispersion is 50r / min, and the time is 30min; the speed of the additive mixing stage is 80r / min, and the time is 1h; the grinding is first at 90r / min, maintained for 1h, and then at 60r / min, maintained for 330min; the speed of the grinding of glue is 70r / min for 4h; after meeting the particle size requirements and scraping requirements, it is transferred to a degassing device for centrifugal degassing; wherein, the centrifugal degassing adopts a centrifugal accelerated online continuous degassing method, the temperature is room temperature, the vacuum degree is -50~-60Kpa, the speed frequency is 50Hz, the time is 1.5h, and finally, after filtration and iron removal treatment, a slurry product is obtained; the viscosity of the slurry product is 20000cp.

[0041] Embodiment 2: A method for preparing an electronic ceramic slurry comprises the following steps:

[0042] Step 1: Sol:

[0043] S1.1: Prepare silicon nitride powder, triolein, modified polyvinyl alcohol, dibutyl phthalate, sintering aid, and ethanol aqueous solution as materials; the mass fraction of the materials is: 40% silicon nitride powder, 1% sodium dodecyl sulfate, 5% modified polyvinyl alcohol, 1% polyethylene glycol-400, 10% sintering aid, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10r / min, then increase the speed to 800r / min, and disperse for 20min; after all the materials are added, heat the water bath to 50℃, stir at 30r / min at -0.03MPa, then increase the speed to 1500r / min, disperse for 10h, and obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0044] Step 2: The glue solution of step 1 is transferred to a ball mill through air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding of glue; wherein the speed of the pre-dispersion is 50r / min, and the time is 30min; the speed of the additive mixing stage is 80r / min, and the time is 1h; the grinding is first at 90r / min, maintained for 1h, and then at 60r / min, maintained for 330min; the speed of the grinding of glue is 70r / min for 4h; after meeting the particle size requirements and scraping requirements, it is transferred to a degassing device for centrifugal degassing; wherein, the centrifugal degassing adopts a centrifugal accelerated online continuous degassing method, the temperature is room temperature, the vacuum degree is -50 to -60Kpa, the speed frequency is 50Hz, the time is 1.5h, and finally, after filtration and iron removal treatment, a slurry product is obtained; the viscosity of the slurry product is 100000cp.

[0045] Comparative Example 1: A method for preparing an electronic ceramic slurry, comprising the following steps:

[0046] Step 1: Sol:

[0047] S1.1: Prepare silicon nitride powder, triolein, modified polyvinyl alcohol, dibutyl phthalate, sintering aid, and ethanol aqueous solution as materials; the mass fraction of the materials is: 40% silicon nitride powder, 1% sodium dodecyl sulfate, 5% modified polyvinyl alcohol, 1% polyethylene glycol-400, 10% sintering aid, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10r / min, then increase the speed to 800r / min, and disperse for 20min; after all the materials are added, heat the water bath to 50℃, stir at 30r / min at -0.03MPa, then increase the speed to 1500r / min, disperse for 10h, and obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0048] Step 2: The glue solution in step 1 is transferred to a ball mill through air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding of glue; wherein the speed of pre-dispersion is 50r / min, and the time is 30min; the speed of the additive mixing stage is 50r / min, and the time is 60min; the grinding is first carried out at 50r / min, and the time is 20h; the speed of grinding of glue is 50r / min and the time is 20h; after meeting the particle size requirements and scraping requirements, it is transferred to a degassing device for centrifugal degassing; wherein the centrifugal degassing includes 5 stages, the first stage: temperature 38°C, stirring speed 3 0r / min, vacuum degree 0Kpa, time 30min; second stage: temperature 38℃, stirring speed 30r / min, vacuum degree -80Kpa, time 2h; third stage temperature 38℃, stirring speed 10r / min, vacuum degree -85Kpa, time 2h30min; fourth stage temperature 38℃, stirring speed 10r / min, vacuum degree -80Kpa, time 2h; fifth stage: temperature 38℃, stirring speed 10r / min, vacuum degree -60Kpa, time 1h; finally, after filtration and iron removal treatment, the slurry product is obtained; the viscosity of the slurry product is 10000cp.

[0049] Comparative Example 2: Compared with Example 2, polyvinyl alcohol is not modified, and the rest is the same, as follows:

[0050] Step 1: Sol:

[0051] S1.1: Prepare silicon nitride powder, triolein, modified polyvinyl alcohol, dibutyl phthalate, sintering aid, and ethanol aqueous solution as materials; the mass fraction of the materials is: 40% silicon nitride powder, 1% sodium dodecyl sulfate, 5% polyvinyl alcohol, 1% polyethylene glycol-400, 10% sintering aid, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10r / min, then increase the speed to 800r / min, and disperse for 20min; after all the materials are added, heat the water bath to 50℃, stir at 30r / min at -0.03MPa, then increase the speed to 1500r / min, disperse for 10h, and obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0052] Step 2: The glue solution of step 1 is transferred to a ball mill through air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding of glue; wherein the speed of the pre-dispersion is 50r / min, and the time is 30min; the speed of the additive mixing stage is 80r / min, and the time is 1h; the grinding is first at 90r / min, maintained for 1h, and then at 60r / min, maintained for 330min; the speed of the grinding of glue is 70r / min for 4h; after meeting the particle size requirements and scraping requirements, it is transferred to a degassing device for centrifugal degassing; wherein, the centrifugal degassing adopts a centrifugal accelerated online continuous degassing method, the temperature is room temperature, the vacuum degree is -50 to -60Kpa, the speed frequency is 50Hz, the time is 1.5h, and finally, after filtration and iron removal treatment, a slurry product is obtained; the viscosity of the slurry product is 100000cp.

[0053] Comparative Example 3: Compared with Example 2, magnesium oxide, chlorine oxide and yttrium oxide in the sintering aid are directly added, as follows:

[0054] Step 1: Sol:

[0055] S1.1: Prepare silicon nitride powder, triolein, modified polyvinyl alcohol, dibutyl phthalate, sintering aid, and ethanol aqueous solution as materials; the mass fraction of the materials is: 40% silicon nitride powder, 1% sodium dodecyl sulfate, 5% modified polyvinyl alcohol, 1% polyethylene glycol-400, 2% magnesium oxide, 2% white oxide, 6% yttrium oxide, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10r / min, then increase the speed to 800r / min, and disperse for 20min; after all the materials are added, heat the water bath to 50℃, stir at 30r / min at -0.03MPa, then increase the speed to 1500r / min, disperse for 10h, and obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0056] Step 2: The glue solution of step 1 is transferred to a ball mill through air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding of glue; wherein the speed of the pre-dispersion is 50r / min, and the time is 30min; the speed of the additive mixing stage is 80r / min, and the time is 1h; the grinding is first at 90r / min, maintained for 1h, and then at 60r / min, maintained for 330min; the speed of the grinding of glue is 70r / min for 4h; after meeting the particle size requirements and scraping requirements, it is transferred to a degassing device for centrifugal degassing; wherein, the centrifugal degassing adopts a centrifugal accelerated online continuous degassing method, the temperature is room temperature, the vacuum degree is -50 to -60Kpa, the speed frequency is 50Hz, the time is 1.5h, and finally, after filtration and iron removal treatment, a slurry product is obtained; the viscosity of the slurry product is 100000cp.

[0057] Performance test: The finished products obtained in Examples 1-2 and Comparative Example 1 were subjected to relevant tests; the obtained data are shown in the following table:

[0058]

[0059] Table 1

[0060] The finished products obtained in Examples 1-2 and Comparative Examples 1-3 were subjected to relevant tests on pre-coating and tensile strength, and the data obtained are shown in the following table:

[0061] project Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Before glue coating Almost no bulge Almost no bulge More bulges More bulges More bulges tensile strength 1.674 2.224 1.432 1.222 1.321

[0062] Table 2

[0063] Conclusion: Through the automated continuous pulping process, the preparation time of Example 1-2 is greatly shortened from 60 hours to 24-25 hours, and the production capacity is increased by 1.6 times; at the same time, the particle size control is more precise, the particle dispersion is more uniform, and the slurry quality is significantly improved; and compared with Comparative Example 1, the viscosity variation range of Example 1-2 is larger, which is suitable for different process requirements. In the tensile strength and pre-scratch coating experiments, due to the modified polyvinyl alcohol and the special treatment of the sintering aid, the rheological properties of the slurry of the sizing agent are optimized and the mechanical strength is improved.

[0064] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing an electronic ceramic slurry, characterized in that: The following steps are involved: Step 1: Sol: S1.1: prepare silicon nitride powder, sodium dodecyl sulfate, modified polyvinyl alcohol, polyethylene glycol-400, sintering aid, and ethanol aqueous solution as materials; S1.2: under nitrogen atmosphere, place the materials in a mixing tank in turn for homogenization to obtain a glue solution; Step 2: Ball milling and degassing: The glue solution is transferred to a ball mill, ground and slurried to meet the particle size requirements and coating requirements, degassed, and finally filtered and iron-removed to obtain electronic ceramic slurry.

2. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: In step 1, the specific process of S1.2 is: under a nitrogen atmosphere, the materials are gradually added to the mixing tank. During this process, the parameters are first set to a stirring rate of 8 to 12 r / min and a dispersion rate of 250 to 300 r / min, and maintained for 8 to 12 min. Then, the parameters are set to a stirring rate of 15 to 20 r / min and a dispersion rate of 700 to 800 r / min, and maintained for 15 to 20 min. After all the materials are introduced, the parameters are set to a stirring rate of 30 r / min, a dispersion rate of 1500 r / min, a vacuum degree of -0.01 to -0.03 MPa, and a water heating cycle with a mold temperature controller of 45 to 50°C, and maintained for 9 to 10 hours to obtain a glue solution.

3. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: In step 2, vertical stirring is adopted during the grinding and pulping process; the grinding includes four stages of pre-dispersion, auxiliary agent mixing stage, grinding and rubber grinding, wherein the speed of pre-dispersion is 50-55r / min, and the time is 30-40min; the speed of the auxiliary agent mixing stage is 80-90r / min, and the time is 1-2h; the grinding is first at 90-95r / min, maintained for 1-2h, and then at 60-65r / min, maintained for 330-350min; the speed of rubber grinding is 70-75r / min, and the time is 4-5h.

4. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: In step 2, degassing adopts online continuous degassing, the temperature is room temperature, the vacuum degree is -50 to -60 Kpa, the rotation frequency is 50 to 55 Hz, and the time is 1.5 to 2 hours.

5. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: The particle size requirement is that the D50 control range is 0.6±0.2μm; the scraping requirement is that the number of surface convex points is ≤6.

6. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: The electronic ceramic slurry comprises the following materials: by weight, 40-50% silicon nitride powder, 1-2% sodium dodecyl sulfate, 5-10% modified polyvinyl alcohol, 1-2% polyethylene glycol-400, 10-12% sintering aid, and the rest is 10-15% ethanol aqueous solution by volume.

7. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: The preparation process of the modified polyvinyl alcohol is: S1: Glycidyl methacrylate, N,N-dimethylethanolamine, triethylamine and tetrahydrofuran are mixed, stirred evenly, heated to 85-95°C, reacted for 4-8h, cooled to room temperature, extracted with ethyl acetate, dried, and concentrated to obtain tertiary aminated methacrylate; S2: Mix tertiary aminated methacrylate, polyvinyl alcohol and deionized water, adjust the pH value to acidic, stir evenly at high speed, add ammonium cerium nitrate solution, heat to 50-60°C, react for 8-10 hours, cool to room temperature, then add 1,3-propane sultone solution, continue to heat to 40-50°C, react for 1-2 hours, filter, wash and dry after cooling to obtain modified polyvinyl alcohol.

8. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: The raw materials of the tertiary aminated methacrylate include the following substances: by weight, 16 to 18 parts of glycidyl methacrylate, 10 to 12 parts of N,N-dimethylethanolamine, 0.1 to 0.2 parts of triethylamine, and 100 to 150 parts of tetrahydrofuran; The modified polyvinyl alcohol raw material comprises the following substances: by weight, 4-5 parts of tertiary aminated methacrylate, 8-10 parts of polyvinyl alcohol, 110-120 parts of deionized water, 0.5-0.8 parts of cerium ammonium nitrate solution, and 1-2 parts of 1,3-propane sultone solution.

9. The method for preparing an electronic ceramic slurry according to claim 1, characterized in that: The preparation process of the sintering aid is as follows: in a nitrogen atmosphere, mercaptolated diatomite, tertiary aminated methacrylate, and isopropanol are mixed, azobisisobutyronitrile is added, the temperature is raised to 50-60° C., the mixture is reacted under light for 1-2 hours, the mixture is cooled to room temperature, washed, dried, and then transferred to acetone, 1,3-propane sultone solution is added, the temperature is further raised to 40-50° C., and the mixture is reacted for 1-2 hours to obtain modified diatomite; The modified diatomaceous earth, magnesium oxide, chlorine oxide, yttrium oxide and isopropanol are mixed and stirred for 3 to 4 hours to obtain a sintering aid; The modified diatomaceous earth comprises the following components: by weight, 20 to 25 parts of mercapto diatomaceous earth, 10 to 12 parts of tertiary aminated methacrylate, 100 to 120 parts of isopropanol, 0.1 to 0.2 parts of azobisisobutyronitrile, 60 to 70 parts of acetone, and 1 to 2 parts of 1,3-propane sultone solution; The sintering aid comprises the following components: by weight, 4 to 5 parts of modified diatomaceous earth, 1 to 2 parts of magnesium oxide, 1 to 2 parts of chlorine oxide, 1 to 2 parts of yttrium oxide, and 50 to 60 parts of isopropanol.

10. A finished slurry product obtained by the method for preparing an electronic ceramic slurry according to any one of claims 1 to 9.

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