Electronic ceramic slurry and preparation method thereof

Abstract

The present invention discloses an electronic ceramic slurry and a preparation method thereof, and relates to the field of electronic ceramic processing technology. The method comprises the following steps: Step 1: Sol: S1.1: Prepare silicon nitride powder, sodium lauryl sulfate, modified polyvinyl alcohol, polyethylene glycol-400, sintering aid, and ethanol aqueous solution as materials; S1.2: Under a nitrogen atmosphere, place the materials in a mixing tank in sequence for homogenization to obtain a glue solution; Step 2: Ball milling and degassing: Transfer the glue solution to a ball mill, grind and slurry, meet the particle size requirements and scraping requirements, degas, and finally filter and remove iron to obtain an electronic ceramic slurry. Advantages: 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 the diatomaceous earth is chemically modified so that it acts as a carrier of the sintering aid, effectively improving the quality of the product.

Description

Technical Field

[0001] The present 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 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 casting method. The prerequisite for obtaining a good green body is high-quality slurry preparation.

[0003] The currently commonly used electronic ceramic preparation process 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 easy to form a skin, easy to be contaminated, 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, which affects 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 lauryl sulfate, modified polyvinyl alcohol, polyethylene glycol-400, sintering aid, and ethanol aqueous solution as materials; S1.2: Under a nitrogen atmosphere, place the materials in a mixing tank in sequence and homogenize them to obtain a glue solution;

[0010] Step 2: Ball milling and degassing:

[0011] The glue solution is transferred to a ball mill, ground into a slurry, and after reaching the particle size requirements and coating requirements, it is degassed and finally filtered and iron-removed to obtain the 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. 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 mold temperature controller temperature of 45-50°C for water heating circulation, and maintained for 9-10 hours to obtain a glue solution.

[0013] More optimally, in step 2, a vertical stirring method is adopted during the grinding and pulping process; the grinding includes four stages: pre-dispersion, auxiliary agent mixing stage, grinding and rubber grinding, wherein the speed of the 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 the rubber grinding is 70-75r / min, and the time is 4-5h.

[0014] More optimally, in step 2, degassing adopts online continuous degassing, temperature is room temperature, vacuum degree is -50~-60Kpa, rotation speed frequency is 50~55Hz, and time is 1.5~2h.

[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 lauryl sulfate, 5-10% modified polyvinyl alcohol, 1-2% polyethylene glycol-400, 10-12% sintering aid, and the rest is 10-15% volume fraction of 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 were mixed and stirred uniformly, and then heated to 85-95°C for reaction for 4-8 hours. The mixture was cooled to room temperature, and the product was extracted with ethyl acetate, dried, and concentrated to obtain tertiary aminated methacrylate.

[0019] S2: Mix tertiary ammonium methacrylate, polyvinyl alcohol, and deionized water, adjust the pH value to acidic, stir 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, cool, filter, wash, and dry to obtain modified polyvinyl alcohol.

[0020] More optimally, the raw materials of the tertiary aminated methacrylate include the following substances: 16 to 18 parts by weight 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 includes the following substances: by weight, 4 to 5 parts of tertiary amine methacrylate, 8 to 10 parts of polyvinyl alcohol, 110 to 120 parts of deionized water, 0.5 to 0.8 parts of cerium ammonium nitrate solution, and 1 to 2 parts of 1,3-propane sultone solution.

[0022] More optimally, the preparation process of the sintering aid is as follows: under a nitrogen atmosphere, mercaptolated diatomaceous earth, 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 diatomaceous earth; the modified diatomaceous earth, 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: 20 to 25 parts by weight of mercaptolated diatomaceous earth, 10 to 12 parts of tertiary amine methacrylate, 100 to 120 parts of isopropyl alcohol, 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 includes 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 fluorine oxide, 1 to 2 parts of yttrium oxide, and 50 to 60 parts of isopropyl alcohol.

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

[0026] The present invention provides an automated continuous preparation method for electronic ceramic slurry. During this process, the binder polyvinyl alcohol is modified accordingly. At the same time, to improve the dispersion effect of the sintering aid, the surface of diatomaceous earth is chemically modified so that it acts as a carrier for 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, significantly improving production efficiency. It 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. The slurry particle size control is more precise, the scraping surface is almost free of protrusions, the iron content is significantly reduced, and the uniformity, stability, and purity of the slurry are significantly improved.

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

[0029] Third: By chemically modifying the diatomite surface 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 diatomite surface, 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 by weight, and all raw materials involved in the present invention are purchased from manufacturers without any special restrictions. Examples include: In the following examples, 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 and stirred uniformly. The mixture was heated to 85°C and reacted for 4 hours. The mixture was cooled to room temperature, and the product was extracted with ethyl acetate, dried, and concentrated to obtain tertiary aminated methacrylate.

[0034] S2: Mix 4 parts of tertiary amine methacrylate, 8 parts of polyvinyl alcohol, and 110 parts of deionized water, adjust the pH value to acidic, stir 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, cool, filter, wash, and dry to obtain modified polyvinyl alcohol.

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

[0036] (1) Under nitrogen, 25 parts of mercapto-diatomaceous earth, 12 parts of tertiary amine methyl acrylate, and 120 parts of isopropanol were mixed, 0.2 parts of azobisisobutyronitrile were added, the temperature was raised to 50 ° C, and 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, and the temperature was continued to be raised to 40 ° C. The mixture was reacted for 1 hour to obtain modified diatomaceous earth; 5 parts of modified diatomaceous earth, 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] Example 1: A method for preparing an electronic ceramic slurry, comprising 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 lauryl 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 a nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10 r / min, then increase the speed to 800 r / min and disperse for 20 minutes; after all the materials are added, heat in a water bath to 50°C, stir at 30 r / min at -0.03 MPa, then increase the speed to 1500 r / min and disperse for 10 hours to obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0040] Step 2: The glue solution in step 1 is transferred to a ball mill by air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, powder grinding and glue grinding; wherein the pre-dispersion speed is 50r / min, and the time is 30min; the speed of the additive mixing stage is 80r / min, and the time is 1h; the powder grinding is first at 90r / min, maintained for 1h, and then at 60r / min, maintained for 330min; the speed of the glue grinding 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 deironing treatment, a slurry product is obtained; the viscosity of the slurry product is 20000cp.

[0041] Example 2: A method for preparing an electronic ceramic slurry, comprising 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 lauryl 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 a nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10 r / min, then increase the speed to 800 r / min and disperse for 20 minutes; after all the materials are added, heat in a water bath to 50°C, stir at 30 r / min at -0.03 MPa, then increase the speed to 1500 r / min and disperse for 10 hours to obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0044] Step 2: The glue solution in step 1 is transferred to a ball mill by air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding 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 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 deironing 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 lauryl 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 a nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10 r / min, then increase the speed to 800 r / min and disperse for 20 minutes; after all the materials are added, heat in a water bath to 50°C, stir at 30 r / min at -0.03 MPa, then increase the speed to 1500 r / min and disperse for 10 hours to 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 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 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, 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 was not modified, and the rest was 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 lauryl sulfate, 5% polyvinyl alcohol, 1% polyethylene glycol-400, 10% sintering aid, and the rest is 10% ethanol aqueous solution by volume; S1.2: Under a nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10 r / min, then increase the speed to 800 r / min and disperse for 20 minutes; after all the materials are added, heat in a water bath to 50°C, stir at 30 r / min at -0.03 MPa, then increase the speed to 1500 r / min and disperse for 10 hours to obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0052] Step 2: The glue solution in step 1 is transferred to a ball mill by air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding 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 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 deironing 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 lauryl sulfate, 5% modified polyvinyl alcohol, 1% polyethylene glycol-400, 2% magnesium oxide, 2% chlorine oxide, 6% yttrium oxide, and the rest is 10% volume fraction of ethanol aqueous solution; S1.2: Under a nitrogen atmosphere, gradually add the materials to the reaction vessel. During this process, stir at 10 r / min, then increase the speed to 800 r / min and disperse for 20 minutes; after all the materials are added, heat the water bath to 50°C, stir at 30 r / min at -0.03 MPa, then increase the speed to 1500 r / min, disperse for 10 hours to obtain a uniform glue; the viscosity of the glue here is 6000cp;

[0056] Step 2: The glue solution in step 1 is transferred to a ball mill by air pressure, and a ball milling aid is added for grinding. The grinding includes four stages: pre-dispersion, additive mixing stage, grinding and grinding 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 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 deironing 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-glue coating and tensile strength, and the obtained data are shown in the following table:

[0061] project Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Scrape before gluing 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 slurrying process, Examples 1-2 significantly reduced preparation time from 60 hours to 24-25 hours, increasing production capacity by 1.6 times. Furthermore, particle size control was more precise, particle dispersion was more uniform, and slurry quality was significantly improved. Furthermore, compared to Comparative Example 1, Examples 1-2 exhibited a wider viscosity range, making them suitable for different process requirements. In tensile strength and pre-squeeze coating experiments, the modified polyvinyl alcohol and special treatment of the sintering aid resulted in optimized rheological properties and improved mechanical strength.

[0064] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are 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 will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection 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 lauryl sulfate, modified polyvinyl alcohol, polyethylene glycol-400, sintering aid, and ethanol aqueous solution as materials; S1.2: Under a nitrogen atmosphere, place the materials in a mixing tank in sequence and homogenize them 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; The preparation process of the modified polyvinyl alcohol is as follows: S1: glycidyl methacrylate, N,N-dimethylethanolamine, triethylamine, and tetrahydrofuran are mixed, stirred evenly, heated to 85-95° C., reacted for 4-8 hours, cooled to room temperature, extracted with ethyl acetate, dried, and concentrated to obtain tertiary ammonium methacrylate; S2: tertiary ammonium methacrylate, polyvinyl alcohol, and deionized water are mixed, the pH value is adjusted to acidic, stirred evenly at high speed, ammonium cerium nitrate solution is added, heated to 50-60° C., reacted for 8-10 hours, cooled to room temperature, and then 1,3-propane sultone solution is added, the temperature is further heated to 40-50° C., reacted for 1-2 hours, cooled, filtered, washed, and dried to obtain the modified polyvinyl alcohol; The preparation process of the sintering aid is as follows: under a nitrogen atmosphere, mercaptolated diatomaceous earth, tertiary aminated methacrylate, and isopropyl alcohol 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., the mixture is reacted for 1-2 hours to obtain modified diatomaceous earth; and the modified diatomaceous earth, magnesium oxide, chlorine oxide, yttrium oxide, and isopropyl alcohol are mixed and stirred for 3-4 hours to obtain the sintering aid.

2. The method for preparing an electronic ceramic slurry according to claim 1, wherein: 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 minutes. 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 minutes. 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, wherein: In step 2, a vertical stirring method is adopted during the grinding and pulping process; the grinding includes four stages: pre-dispersion, auxiliary agent mixing stage, grinding and rubber grinding, wherein the speed of the 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 the 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, wherein: In step 2, degassing adopts online continuous degassing, temperature is room temperature, vacuum degree is -50~-60KPa, rotation speed frequency is 50~55Hz, and time is 1.5~2h.

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

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

7. The method for preparing an electronic ceramic slurry according to claim 1, wherein: The raw materials of the tertiary aminated methacrylate include the following substances: 16 to 18 parts by weight 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 includes the following substances: by weight, 4 to 5 parts of tertiary amine methacrylate, 8 to 10 parts of polyvinyl alcohol, 110 to 120 parts of deionized water, 0.5 to 0.8 parts of cerium ammonium nitrate solution, and 1 to 2 parts of 1,3-propane sultone solution.

8. The method for preparing an electronic ceramic slurry according to claim 1, wherein: The modified diatomaceous earth comprises the following components: by weight, 20 to 25 parts of mercaptolated diatomaceous earth, 10 to 12 parts of tertiary amine methacrylate, 100 to 120 parts of isopropyl alcohol, 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 includes 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 fluorine oxide, 1 to 2 parts of yttrium oxide, and 50 to 60 parts of isopropyl alcohol.

9. A finished slurry product obtained by the method for preparing an electronic ceramic slurry according to any one of claims 1 to 8.

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