CN116768609A - Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics - Google Patents

Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics Download PDF

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CN116768609A
CN116768609A CN202310738706.7A CN202310738706A CN116768609A CN 116768609 A CN116768609 A CN 116768609A CN 202310738706 A CN202310738706 A CN 202310738706A CN 116768609 A CN116768609 A CN 116768609A
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powder
ball milling
alumina
ceramic
product
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请求不公布姓名
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Suzhou Ruicer New Material Technology Co ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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Abstract

The invention discloses an application of cast-molded green ceramic in preparing electronic ceramics, which comprises the following raw materials: 30-60 parts of alumina powder, 20-40 parts of white corundum powder, 2-20 parts of acrylic adhesive, 10-40 parts of solvent, and the granularity D of the alumina powder and the white corundum powder 50 The addition amount of the acrylic adhesive is 15% -30% of the total addition amount of the alumina powder and the white corundum powder, wherein the addition amount of the acrylic adhesive is 30-80 mu m respectively; when in use, the firing-supporting raw porcelainThe sintering temperature of (2) is less than or equal to 1650 ℃; the sintering-bearing raw porcelain can be used as a supporting plate and a covering plate in the sintering process of the raw porcelain of a product, and the raw porcelain of the product is clamped in the middle to separate and prevent impurities in a sintering furnace from adhering to the surface of the sintered product, and meanwhile, the warping degree of the sintered product can be reduced.

Description

Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics
The invention relates to a firing-bearing raw porcelain, which is a divisional application of Chinese invention patent application with the application date of 2022, 07, 29, the application number of 2022109031796 and the name of 'a preparation method and application'.
Technical Field
The invention relates to the field of electronic ceramics, in particular to application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics.
Background
Electronic ceramics can be usually formed by sintering raw ceramic tiles (generally obtained by casting alumina slurry) after operations such as punching, printing with metalized slurry and the like, wherein the sintering operation is generally performed in a high-temperature furnace, however, the conditions of volatilization, carbonization, decomposition and the like of a binder and a solvent can occur in the sintering process, so that the environment in the furnace is dirty, particularly dirt in a glue discharging area below 500 ℃ is more, the dirt can often adhere to products, poor products are caused, and meanwhile, the products warp during sintering in the furnace due to the difference of shrinkage rates of the alumina slurry adopted by the raw ceramic and the metalized slurry adopted by printing, and certain negative effects are caused on the quality of the products.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art, and provides application of a novel cast-molded green ceramic in preparing electronic ceramics, wherein the green ceramic can be used as a supporting plate and a cover plate in the sintering process of the green ceramic, and the green ceramic can be clamped between the supporting plate and the cover plate to separate and prevent impurities in a sintering furnace from adhering to the surface of a sintered product, and meanwhile, the warping degree of the sintered product can be reduced.
In order to achieve the above purpose, the invention adopts a technical scheme that: the application of the tape casting formed green ceramic in preparing the electronic ceramic is characterized in that the raw materials of the green ceramic comprise the following components in parts by weight: 30-60 parts of alumina powder, 20-40 parts of white corundum powder, 2-20 parts of acrylic adhesive and 10-40 parts of solvent;
wherein the particle size D of the alumina powder 50 The granularity D of the white corundum powder is 30-80 mu m 50 30-80 μm;
in the raw materials of the firing ceramic, the addition amount of the acrylic adhesive accounts for 15-30% of the total addition amount of the alumina powder and the white corundum powder;
the sintering temperature of the green ceramic is less than or equal to 1650 ℃ when the green ceramic is used.
The invention provides another technical scheme that: the raw material of the ceramic comprises the following components in parts by weight:
wherein the particle size D of the alumina powder 50 The granularity D of the white corundum powder is 30-80 mu m 50 30-80 μm;
in the raw materials of the firing ceramic, the addition amount of the acrylic adhesive accounts for 15-30% of the total addition amount of the alumina powder and the white corundum powder.
According to some preferred aspects of the invention, the raw materials of the green ceramic comprise, in parts by weight:
according to some preferred aspects of the invention, the mass ratio of the alumina powder to the white corundum powder is 1:0.1-0.8.
According to some preferred aspects of the invention, the white corundum powder has a particle size D 50 Particle size D smaller than the alumina powder 50
According to some preferred aspects of the invention, the acrylic binder has a weight average molecular weight of 40 to 60 tens of thousands and a glass transition temperature of-10 to 30 ℃.
Further preferably, the weight average molecular weight of the acrylic adhesive is 45 to 55 tens of thousands, and the glass transition temperature is 0 to 20 ℃.
According to a specific aspect of the invention, the acrylic adhesive is KFA-440 of the interaction chemistry.
In some embodiments of the invention, the solvent is toluene.
The invention provides another technical scheme that: the preparation method of the firing-supporting raw porcelain comprises the following steps:
weighing the raw materials according to the formula, adding the alumina powder, the white corundum powder and the solvent into a ball mill, and performing ball milling for one time;
then adding an acrylic adhesive, and performing secondary ball milling;
and (5) casting after defoaming.
According to some preferred and specific aspects of the present invention, the ball milling time of the primary ball milling and the secondary ball milling is controlled to be 2-4 hours respectively.
According to some preferred and specific aspects of the present invention, in the casting machine used for casting, the temperatures of the 4 temperature zones are respectively: 55-75deg.C, 65-85deg.C, 75-95deg.C, 85-105deg.C.
The invention provides another technical scheme that: an application of the firing-supporting raw porcelain in preparing electronic ceramics, wherein the application comprises the following steps:
placing the raw porcelain of the product to be burned on the first raw porcelain to be burned, covering the upper surface of the raw porcelain of the product to be burned with the second raw porcelain to be burned to form a sequentially overlapped combination to be burned, and then placing the combination to be burned into a sintering furnace for sintering;
after sintering, the first sintering-bearing raw porcelain becomes a first sintering-bearing product, the raw porcelain of the product to be sintered becomes a ceramic product, the second sintering-bearing raw porcelain becomes a second sintering-bearing product, the first sintering-bearing product, the ceramic product and the second sintering-bearing product are sequentially overlapped, the first sintering-bearing product and the second sintering-bearing product are respectively peeled off, the ceramic product is obtained, and the ceramic product is processed into electronic ceramic;
the first and second green-ceramic are the green-ceramic.
According to the invention, in said application, the sintering temperature of said sintering is less than 1800 ℃.
Further, the sintering temperature of the sintering is 1650 ℃ or less.
In some embodiments of the present invention, the green porcelain of the product to be fired is made from an alumina slurry, which may employ formulation components commonly used in the art.
Preferably, the alumina slurry adopts the following formula components:
the alumina slurry comprises the following raw materials in percentage by mass: 45-60% of powder alumina, 2-8% of auxiliary agent powder, 0.5-5% of molybdenum powder solution, 8-20% of acrylic adhesive, 0.05-3% of plasticizer and 15-40% of first organic solvent.
Further, in the alumina slurry, 47-58% of powdery alumina, 2-7% of auxiliary agent powder, 0.8-3.5% of molybdenum powder solution, 10-18% of acrylic adhesive, 0.1-1.5% of plasticizer and 15-38% of first organic solvent.
The auxiliary powder in the present invention does not contain metallic molybdenum powder.
According to some preferred aspects of the invention, the auxiliary powder comprises silica, talc and chromia.
According to some preferred aspects of the invention, the silica, the talc and the chromia are dosed in a mass ratio of 4-5.5:1.5-3.5:1.
In some embodiments of the invention, the auxiliary powder is comprised of silica, talc and chromium oxide.
According to some preferred aspects of the present invention, the molybdenum powder solution is obtained by dispersing metallic molybdenum powder in a second organic solvent, wherein the mass fraction of the second organic solvent is 20-40%, and the second organic solvent may be isopropanol.
According to some preferred aspects of the invention, the plasticizer may be dibutyl phthalate.
According to some preferred aspects of the invention, the first organic solvent is an organic solvent that is poorly compatible or insoluble with water. According to a specific and preferred aspect of the present invention, the first organic solvent may be toluene.
The preparation method of the alumina slurry comprises the following steps:
(1) Respectively adding powder alumina, auxiliary agent powder, molybdenum powder solution and a first organic solvent into a ball mill, and performing first ball milling;
(2) Then adding part of acrylic adhesive into the ball mill, performing a second ball milling, and monitoring the particle size of particles in the slurry in the ball milling process;
(3) Stopping the second ball milling when the particle size reaches a preset value, adding the rest acrylic adhesive and plasticizer, and performing third ball milling to obtain alumina slurry;
wherein the part of the acrylic binder in the step (2) accounts for 0.5% -5% of the total addition amount of the acrylic binder in terms of mass percentage, the part of the acrylic binder in the step (2) accounts for 0.05% -2% of the addition amount of the powder alumina, and the time for the second ball milling accounts for more than 75% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling. In the practical process, only a small amount of proper acrylic adhesive is added to participate in the main ball milling process of the preparation of the alumina slurry, and most of acrylic adhesive and all of plasticizer are finally added.
In addition, in a large number of experimental practices, the alumina slurry is easy to gel in the initial mixing stage or the ball milling process, so that the ball milling is difficult, once the alumina slurry is formed, the alumina slurry is difficult to be used as the slurry of a casting system again, the raw porcelain cannot be prepared, and the production cost is greatly increased. Through the combination of experiments and production practices of the inventor, the analysis shows that the gelation phenomenon may occur due to the existence of water in the system, but in the practice process, even if powder raw materials such as powder alumina are subjected to certain drying treatment, the gelation phenomenon still occurs in different batches to different degrees. Later, the inventors have unexpectedly found that when other types of binders such as PVB (polyvinyl butyral) are used in organic solvent-based casting systems, gelation is substantially avoided by subjecting the powdered raw material, such as powdered alumina, to a certain drying process. The analysis after comparison shows that the invention adopts the acrylic adhesive, and the functional carboxyl contained in the acrylic adhesive can form a plurality of hydrogen bonds with water, so that the gelation phenomenon of the system can occur and is obvious under the condition of extremely low water content, but if the water is required to be completely removed, the water removal operation is long in time and high in energy consumption, which is unfavorable for reducing the cost and improving the production efficiency. According to some preferred aspects of the present invention, in step (1), the water content of the alumina powder and the auxiliary agent powder is controlled to be lower than 0.75% before the alumina powder and the auxiliary agent powder are added into the ball mill, so that the gelation phenomenon can be basically controlled, and the water removal time and the energy consumption are within reasonable ranges.
According to some preferred aspects of the present invention, the part of the acrylic adhesive in the step (2) accounts for 1% to 4% of the total addition amount of the acrylic adhesive in terms of mass%. In some embodiments of the present invention, the portion of the acrylic adhesive in step (2) is 1% -2% of the total added amount of the acrylic adhesive in terms of mass%. In some embodiments of the present invention, the portion of the acrylic adhesive in step (2) is 2% -3% of the total added amount of the acrylic adhesive in terms of mass%. In some embodiments of the present invention, the portion of the acrylic adhesive in step (2) is 3% -4% of the total added amount of the acrylic adhesive in terms of mass%.
According to some preferred aspects of the present invention, the part of the acrylic binder in step (2) accounts for 0.1% to 1.5% of the added amount of the powder alumina in terms of mass%. In some embodiments of the present invention, the portion of the acrylic binder in step (2) comprises 0.1% to 0.5% of the added amount of the powdered alumina in mass percent. In some embodiments of the invention, the portion of the acrylic binder in step (2) comprises 0.5% to 1% of the added amount of the powdered alumina in mass percent. In some embodiments of the invention, the portion of the acrylic binder in step (2) comprises 1% to 1.5% of the added amount of the powdered alumina in mass percent.
According to the invention, the preset value is: d (D) 50 1.9-2.5 μm.
According to some preferred aspects of the invention, the time taken for the first ball milling is 1% -5% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling.
In some embodiments of the invention, the time taken for the first ball milling is 2% -4% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling.
Further, the time taken for the second ball milling is 80% or more of the total ball milling time of the first ball milling, the second ball milling and the third ball milling.
In some embodiments of the present invention, the method for preparing the green porcelain for the product to be fired includes: uniformly mixing the alumina slurry, performing vacuum deaeration, removing bubbles in the slurry, then entering a casting machine to cast green ceramic, cutting according to a certain size to obtain a sheet-shaped green ceramic sheet, and printing electronic slurry for printing on the green ceramic sheet to prepare a green ceramic product to be burned;
the temperature of the 4 temperature areas of the casting machine are respectively as follows: 75.+ -. 10 ℃, 95.+ -. 10 ℃, 120.+ -. 10 ℃, 130.+ -. 10 ℃.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention innovatively provides a novel raw ceramic bearing based on the phenomena of poor surface performance, easy warping and the like in the sintering process of the raw ceramic chip of the existing product, and the raw ceramic bearing can be used as a supporting plate and a cover plate in the sintering process of the raw ceramic product to clamp the raw ceramic product in the middle so as to separate and prevent impurities in a sintering furnace from adhering to the surface of the sintered product, and meanwhile, the warping degree of the sintered product can be reduced, and in addition, the raw ceramic bearing is easy to remove after the sintering is finished, and the surface quality of the sintered product is not affected.
In particular, in the invention, the sintering temperature of the alumina is reduced by combining the alumina powder, the white corundum powder and the acrylic adhesive, because the white corundum powder is prepared by smelting industrial alumina powder at a high temperature above 2000 ℃ and cooling the industrial alumina powder, the sintering temperature of the alumina is about 1800 ℃ under the condition that no sintering aid is added, and the sintering temperature of the alumina is reduced by basically adding the sintering aid such as silicon dioxide and the like into the conventional alumina slurry, therefore, in general, the highest sintering temperature of a sintering furnace is generally 1650 ℃, in such a state, once the sintering ceramic of the invention and the ceramic of the product to be sintered are co-sintered according to the superposition mode of the invention, the intermediate ceramic of the product to be sintered can be normally sintered into ceramic, and the overall structure of the sintered ceramic is loose due to the existence of the white corundum powder, and remains as a whole under the existence of the alumina powder.
In the present invention, in the high temperature sintering furnace, the product is an organic material such as a binder at 500 ℃ or lower, a decarburized organic material at 500 to 1100 ℃ or higher, and alumina starts to sinter. Gaps appear among the degummed alumina particles, organic matters such as carbon in the product pass through the gaps among the alumina particles of the green ceramic, the gaps among the white corundum particles are slowly removed, the product starts to be sintered rapidly at about 1600 ℃, the alumina particles are slowly fused, the gaps are filled, and the sintering is successful. The sintering-supporting ceramic has relatively high sintering temperature because no sintering aid is added, so that larger gaps are kept all the time in the sintering process of the product, and organic matters are removed from the product conveniently.
Drawings
FIG. 1 is a schematic diagram showing the superposition of a to-be-fired assembly according to an embodiment of the present invention;
wherein, 1, a first raw porcelain is burned; 2. raw porcelain of the product to be burned; 3. and a second green ceramic.
Detailed Description
The above-described aspects are further described below in conjunction with specific embodiments; it should be understood that these embodiments are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the scope of the following embodiments; the implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.
All starting materials are commercially available or prepared by methods conventional in the art, not specifically described in the examples below.
Alumina powder was obtained from Meta aluminum, trade name AMB, D measured during use 50 65+ -5 μm;
the white corundum powder may be self-made or commercially available, and in the following examples, commercially available white corundum powder F180 (GB 2477-83) was used to determine D when in use 50 80+/-5 mu m;
D 50 measured by a malvern 3000 laser particle sizer;
the acrylic adhesive is KFA-440 of the interaction chemistry;
the metallic molybdenum powder, silicon dioxide, talcum powder and chromium oxide are all commercially available, and the Fisher particle size is between 1 and 2.3 microns;
dibutyl phthalate is commercially available and has purity of 99%;
the ball mill is a commercially available 300L ball mill with a ceramic lining or a nylon lining, the working parameters are that the rotating speed is 40+/-5 rpm, the grinding balls are alumina balls, the particle size is about 30mm, and the ball-ball ratio is controlled to be 1:1.
Example 1
The embodiment provides a raw ceramic for bearing firing and a preparation method thereof, and the raw materials of the raw ceramic for bearing firing comprise, by weight:
the preparation method of the firing-supporting raw porcelain comprises the following steps:
weighing the raw materials according to the formula, adding the alumina powder, the white corundum powder and the toluene into a ball mill, and performing ball milling for 3 hours;
then adding acrylic adhesive, performing secondary ball milling for 3 hours;
and (3) casting after defoaming, wherein in a casting machine used for casting, the temperatures of 4 temperature areas are respectively as follows: casting the green ceramic with the thickness of 0.6mm at 65 ℃ +/-5 ℃, 75 ℃ +/-5 ℃, 85 ℃ +/-5 ℃ and 95 ℃ +/-5 ℃ and cutting into firing-bearing green ceramic chips with the thickness of 230mm (Y) and 130mm (X).
Example 2
The embodiment provides a raw ceramic for bearing firing and a preparation method thereof, and the raw materials of the raw ceramic for bearing firing comprise, by weight:
55 parts of alumina powder
White corundum powder 20 parts
Acrylic adhesive 15 parts
10 parts of toluene;
the preparation method of the firing-supporting raw porcelain comprises the following steps:
weighing the raw materials according to the formula, adding the alumina powder, the white corundum powder and the toluene into a ball mill, and performing ball milling for 3 hours;
then adding acrylic adhesive, performing secondary ball milling for 3 hours;
and (3) casting after defoaming, wherein in a casting machine used for casting, the temperatures of 4 temperature areas are respectively as follows: casting the green ceramic with the thickness of 0.6mm at 65 ℃ +/-5 ℃, 75 ℃ +/-5 ℃, 85 ℃ +/-5 ℃ and 95 ℃ +/-5 ℃ and cutting into firing-bearing green ceramic chips with the thickness of 230mm (Y) and 130mm (X).
Example 3
The embodiment provides a raw ceramic for bearing firing and a preparation method thereof, and the raw materials of the raw ceramic for bearing firing comprise, by weight:
the preparation method of the firing-supporting raw porcelain comprises the following steps:
weighing the raw materials according to the formula, adding the alumina powder, the white corundum powder and the toluene into a ball mill, and performing ball milling for 3 hours;
then adding acrylic adhesive, performing secondary ball milling for 3 hours;
and (3) casting after defoaming, wherein in a casting machine used for casting, the temperatures of 4 temperature areas are respectively as follows: casting the green ceramic with the thickness of 0.6mm at 65 ℃ +/-5 ℃, 75 ℃ +/-5 ℃, 85 ℃ +/-5 ℃ and 95 ℃ +/-5 ℃ and cutting into firing-bearing green ceramic chips with the thickness of 230mm (Y) and 130mm (X).
Comparative example 1
Substantially the same as in example 1, the only difference is that: the white corundum powder adopts 400# commercial powder and D 50 :25±5μm。
Comparative example 2
Substantially the same as in example 1, the only difference is that: the raw materials of the firing ceramic comprise, by mass, 10% of the additive amount of the acrylic adhesive, namely the alumina powder and the white corundum.
Comparative example 3
Substantially the same as in example 1, the only difference is that: the raw materials of the firing ceramic comprise, by mass, 40% of the additive amount of the acrylic adhesive, namely the alumina powder and the white corundum.
Comparative example 4
Substantially the same as in example 1, the only difference is that: the raw materials of the firing ceramic comprise, by mass, 50% of the additive amount of the acrylic adhesive, namely the alumina powder and the white corundum.
Application example 1
The firing ceramic obtained in example 1 was used to prepare electronic ceramics, and the specific steps include:
placing the raw porcelain of the product to be burned on the first raw porcelain 1 to be burned, covering the upper surface of the raw porcelain 2 of the product to be burned with the second raw porcelain 3 to form a sequentially overlapped combination to be burned (shown in figure 1), and then placing the combination to be burned into a sintering furnace for sintering (the debonding temperature is 500 ℃,3.5 hours; 500-1100 ℃,3.5 hours; 1100-1600 ℃,5.5 hours; and the heating speed is 1 minute and 5 ℃); after sintering, the first sintering-bearing raw porcelain 1 becomes a first sintering-bearing product, the raw porcelain 2 of the product to be sintered becomes a ceramic product, the second sintering-bearing raw porcelain 3 becomes a second sintering-bearing product, the first sintering-bearing product, the ceramic product and the second sintering-bearing product are sequentially overlapped, the first sintering-bearing product and the second sintering-bearing product are respectively peeled off, the ceramic product is obtained, and the ceramic product is processed into electronic ceramic;
the first and second green-ceramic bodies 1 and 3 are the green-ceramic bodies obtained in example 1;
wherein, the raw porcelain 2 of the product to be burned is obtained by the following method:
(1) Preparation of alumina slurry
The alumina slurry comprises the following components: 47% of powdery aluminum oxide, 4% of auxiliary agent powder, 3% of molybdenum powder solution, 12% of acrylic adhesive, 0.3% of plasticizer and 33.7% of toluene; wherein the auxiliary agent powder consists of silicon dioxide, talcum powder and chromium oxide, and the mass ratio of the silicon dioxide to the talcum powder to the chromium oxide is 5:3:1; the molybdenum powder solution is obtained by dispersing metal molybdenum powder in isopropanol, and the mass fraction of the molybdenum powder solution is 30%; powdered alumina was purchased from Meta aluminum, trade name AMB, D measured during use 50 60-70 μm;
drying the powder alumina and the auxiliary agent powder which are weighed according to the proportion in a drying room with the temperature of 80+/-10 ℃ until the water content is reduced to 0.75 percent for standby;
the preparation method of the alumina slurry comprises the following steps:
the first step: putting the dried powder alumina into a ball mill;
and a second step of: putting the dried auxiliary agent powder into a ball mill;
and a third step of: putting isopropanol into a stainless steel barrel, then putting metal molybdenum powder into the stainless steel barrel containing isopropanol, uniformly stirring to obtain molybdenum powder solution, and finally putting the molybdenum powder solution into a ball mill;
fourth step: toluene is put into a ball mill;
fifth step: covering the ball mill cover to perform the first ball milling, stopping after 2 hours of operation, opening the cover, putting part of acrylic adhesive into the ball mill, covering the cover, starting to operate the ball mill to perform the second ball milling, and performing the particle size D of particles in slurry in the ball milling process 50 Monitoring; wherein, part of the acrylic adhesive accounts for 1.5% of the total addition amount of the acrylic adhesive;
sixth step: when the granularity reaches the granularity preset value D 50 The second ball milling time is about 50 hours when the ball milling time is 1.9-2.5 mu m;
meanwhile, when the granularity reaches the requirement, opening the cover of the ball mill, and putting the rest acrylic adhesive into the ball mill; and putting dibutyl phthalate into a ball mill, and then operating for 5 hours to obtain the alumina slurry. The preparation process has no gelation.
(2) Preparation of raw porcelain for to-be-fired product
Uniformly mixing the alumina slurry prepared in the step (1), then carrying out vacuum defoaming, removing bubbles in the slurry, and then, feeding the slurry into a casting machine to cast green ceramic, and cutting the slurry according to a certain size to obtain a sheet-shaped green ceramic to be burned product;
the temperature of the 4 temperature areas of the casting machine are respectively as follows: 75+ -10deg.C, 95+ -10deg.C, 120+ -10deg.C, 130+ -10deg.C;
the green ceramic tile with the thickness of 0.6mm is cast, and cut into green ceramic tiles with the thickness of 60mm (20 mm (Y X)).
X direction: refers to the casting direction; y direction: the direction perpendicular to the casting;
the green porcelain piece is manufactured into the green porcelain of the product to be burned by the following method:
printing 18-22 mu m self-made printing electronic paste on the green ceramic chip, and sintering the ceramic chip without printing paste in a furnace.
Self-made printing electronic paste: is formed by mixing tungsten powder (as conductive phase), alumina (as binder phase) and binder;
tungsten powder: 50 parts of FSSS with a particle size of 1-5. Mu.m
Alumina: 1 part FSSS particle size 0.1-2 microns
Niobium oxide: 1 part of
Acetone: 38 parts of
And (2) a binder: 10 parts (fused by nitrocellulose and dibutyl phthalate 1:2);
adding acetone into tungsten powder and alumina powder sintering aid, putting into 300L ceramic internal village or nylon internal village, grinding for 24 hours, and rotating at the speed of: 50.+ -.10 rpm.
6 parts of binder are added and grinding is continued for 2 hours.
Adding the mixture into a stirring tank after discharging, adding 4 parts of binder after removing acetone in vacuum, and continuously stirring for 0.5 hour;
and (5) discharging after the viscosity is qualified.
Application example 2
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with the one prepared in example 2.
Application example 3
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with the one prepared in example 3.
Comparative example 1 was used
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with comparative example 1.
Comparative example 2 was used
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with comparative example 2.
Comparative example 3 was used
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with comparative example 3.
Comparative example 4 was used
Substantially the same as in application example 1, the only difference is that: the green ceramic was replaced with comparative example 4.
Performance testing
1. The states of the first firing product (obtained after firing the first firing raw ceramic), the second firing product (obtained after firing the second firing raw ceramic) and the ceramic product (obtained after firing the ceramic to be fired product) and each other are observed in the ceramic forming process and after the ceramic forming, and the specific results are shown in table 1.
TABLE 1
2. After porcelain forming, the warping degree of the ceramic product is measured, and the specific test method comprises the following steps:
the thickness of the ceramic sheet (including warpage) was measured using a vernier caliper, the middle of the ceramic sheet was entirely clamped by the vernier caliper, the thickness was measured, and the thickness of the ceramic sheet with the printed electronic paste subtracted from the thickness of the ceramic sheet without the printed electronic paste was the warpage of the ceramic sheet.
See table 2 for specific results.
TABLE 2
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.

Claims (10)

1. The application of the tape casting formed green ceramic in preparing the electronic ceramic is characterized in that the raw materials of the green ceramic comprise the following components in parts by weight: 30-60 parts of alumina powder, 20-40 parts of white corundum powder, 2-20 parts of acrylic adhesive and 10-40 parts of solvent;
wherein the particle size D of the alumina powder 50 The granularity D of the white corundum powder is 30-80 mu m 50 30-80 μm;
in the raw materials of the firing ceramic, the addition amount of the acrylic adhesive accounts for 15-30% of the total addition amount of the alumina powder and the white corundum powder;
the sintering temperature of the green ceramic is less than or equal to 1650 ℃ when the green ceramic is used.
2. The use according to claim 1, characterized in that the raw materials of the green ceramic comprise, in parts by weight: 50-60 parts of alumina powder, 20-40 parts of white corundum powder, 15-20 parts of acrylic adhesive and 10-40 parts of solvent;
or, the raw materials of the firing ceramic comprise the following components in parts by weight: 40-55 parts of alumina powder, 20-30 parts of white corundum powder, 15-20 parts of acrylic adhesive and 10-20 parts of solvent.
3. The use according to claim 1, characterized in that the mass ratio of alumina powder to white corundum powder is 1:0.1-0.8, the particle size D of the white corundum powder 50 Particle size D smaller than the alumina powder 50
The solvent is toluene.
4. The use according to claim 1, wherein the method for preparing the green ceramic comprises:
weighing the raw materials according to the formula, adding the alumina powder, the white corundum powder and the solvent into a ball mill, and performing ball milling for one time;
then adding an acrylic adhesive, and performing secondary ball milling;
casting after deaeration;
controlling the ball milling time of the primary ball milling and the secondary ball milling to be 2-4 hours respectively; in the casting machine for casting, the temperatures of the 4 temperature areas are respectively as follows: 55-75deg.C, 65-85deg.C, 75-95deg.C, 85-105deg.C.
5. The application according to claim 1, characterized in that it comprises:
placing the raw porcelain of the product to be burned on the first raw porcelain to be burned, covering the upper surface of the raw porcelain of the product to be burned with the second raw porcelain to be burned to form a sequentially overlapped combination to be burned, and then placing the combination to be burned into a sintering furnace for sintering;
after sintering, the first sintering-bearing raw ceramic becomes a first sintering-bearing product, the ceramic of the product to be sintered becomes a ceramic product, the second sintering-bearing raw ceramic becomes a second sintering-bearing product, the first sintering-bearing product, the ceramic product and the second sintering-bearing product are sequentially overlapped, the first sintering-bearing product and the second sintering-bearing product are respectively peeled off, the ceramic product is obtained, and the ceramic product is processed into electronic ceramic.
6. The use according to claim 5, wherein the green porcelain of the product to be burned is made of an alumina slurry, the raw materials of which, in mass percent, comprise: 45-60% of powder alumina, 2-8% of auxiliary agent powder, 0.5-5% of molybdenum powder solution, 8-20% of acrylic adhesive, 0.05-3% of plasticizer and 15-40% of first organic solvent;
further, in the alumina slurry, 47-58% of powdery alumina, 2-7% of auxiliary agent powder, 0.8-3.5% of molybdenum powder solution, 10-18% of acrylic adhesive, 0.1-1.5% of plasticizer and 15-38% of first organic solvent;
the auxiliary agent powder comprises silicon dioxide, talcum powder and chromium oxide, wherein the mass ratio of the silicon dioxide to the talcum powder to the chromium oxide is 4-5.5:1.5-3.5:1;
the first organic solvent is an organic solvent which is difficult to dissolve with water or insoluble in water;
the molybdenum powder solution is obtained by dispersing metal molybdenum powder in a second organic solvent, the mass fraction of the molybdenum powder solution is 20-40%, and the second organic solvent is isopropanol.
7. The use according to any one of claims 1-4, 6, wherein the acrylic adhesive has a weight average molecular weight of 40-60 ten thousand, a glass transition temperature of-10-30 ℃, further wherein the acrylic adhesive has a weight average molecular weight of 45-55 ten thousand, a glass transition temperature of 0-20 ℃; still further, the acrylic adhesive is KFA-440 of the interactive chemistry.
8. The use according to claim 6, wherein the method for preparing the alumina slurry comprises the steps of:
(1) Respectively adding powder alumina, auxiliary agent powder, molybdenum powder solution and a first organic solvent into a ball mill, and performing first ball milling;
(2) Then adding part of acrylic adhesive into the ball mill, performing a second ball milling, and monitoring the particle size of particles in the slurry in the ball milling process;
(3) Stopping the second ball milling when the particle size reaches a preset value, adding the rest acrylic adhesive and plasticizer, and performing third ball milling to obtain alumina slurry;
wherein the part of the acrylic binder in the step (2) accounts for 0.5% -5% of the total addition amount of the acrylic binder in terms of mass percentage, the part of the acrylic binder in the step (2) accounts for 0.05% -2% of the addition amount of the powder alumina, and the time for the second ball milling accounts for more than 75% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling.
9. The use according to claim 8, wherein in step (1) the water content of the alumina powder and the auxiliary powder is controlled to be less than 0.75% respectively before being added to the ball mill; and/or, the part of the acrylic adhesive in the step (2) accounts for 1% -4% of the total addition amount of the acrylic adhesive in terms of mass percent; and/or, the part of the acrylic binder in the step (2) accounts for 0.1% -1.5% of the added amount of the powder alumina in terms of mass percent; and/or the time taken by the first ball milling is 1% -5% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling; and/or the time of the second ball milling is more than 80% of the total ball milling time of the first ball milling, the second ball milling and the third ball milling.
10. The use according to claim 6, wherein the method for preparing raw porcelain for the product to be fired comprises: uniformly mixing the alumina slurry, performing vacuum deaeration, removing bubbles in the slurry, then entering a casting machine to cast green ceramic, cutting according to a certain size to obtain a sheet-shaped green ceramic sheet, and printing electronic slurry for printing on the green ceramic sheet to prepare a green ceramic product to be burned;
the temperature of the 4 temperature areas of the casting machine are respectively as follows: 75.+ -. 10 ℃, 95.+ -. 10 ℃, 120.+ -. 10 ℃, 130.+ -. 10 ℃.
CN202310738706.7A 2022-07-29 2022-07-29 Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics Pending CN116768609A (en)

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