CN115231903B - Preparation process of large-size high-purity ceramic substrate - Google Patents
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Abstract
The invention relates to a preparation process of a large-size high-purity ceramic substrate, which is prepared by taking micron alpha-alumina as a main phase material and nano gamma-alumina as a sintering aid, adding additives such as a proper solvent, a dispersing agent, a binder, a plasticizer and the like, and performing hot-pressing sintering after tape casting. The preparation process adopts tape casting to obtain a thin green sheet lamination, then firstly discharges glue, and then applies gradient pressure to the multilayer green sheet and carries out hot-pressing sintering. Because the technology of hot-pressing sintering after glue discharging of the green blank sheet is adopted, the organic additives in the green blank sheet can be completely discharged in the glue discharging process, the defects of air holes, gaps and the like and gas residues caused by glue discharging after the conventional direct lamination are avoided, and the density and the flatness of the ceramic substrate are greatly improved. The density of the ceramic substrate prepared by the preparation process of the large-size high-purity ceramic substrate can reach more than 99 percent and the density can reach 3.9g/cm 3 The above.
Description
Technical Field
The invention relates to the field of ceramic substrate preparation, in particular to a preparation process of a large-size ceramic substrate with high density and high purity.
Background
With the rapid development of products with large working current, high temperature and high frequency, such as semiconductor power modules, high-power integrated circuits, 5G devices and the like, higher requirements are put forward on chip carriers. The ceramic material has stable chemical property, good electrical insulation property, excellent high-frequency characteristic, high thermal conductivity, low dielectric constant and linear expansion coefficient which is very similar to that of electronic components, and is widely applied to the field of electronic substrates. The physical properties of the ceramic substrate are closely related to the purity, the density and the flatness of the ceramic substrate. Therefore, the requirements for high purity, high density and high flatness of the ceramic substrate are higher and higher. The higher the purity of the ceramic substrate is, the higher the required sintering temperature is, the larger the size is, the higher the non-uniformity of the material of the original particles is, and the more difficult the flatness of the substrate is to ensure. Chinese patent CN 112174648A discloses a preparation method of a high-purity alumina substrate, and although the sintering temperature is reduced by introducing a sintering aid, the introduced sintering aid is other substances, so that the purity of the alumina substrate is reduced. Therefore, it is necessary to develop a process for preparing a large-sized ceramic substrate with high density and high purity.
Disclosure of Invention
Therefore, aiming at the defects of the conventional ceramic substrate preparation process used for preparing large-size high-purity ceramic substrates, the invention provides a preparation process of the large-size high-purity ceramic substrate so as to meet the requirements of large-size ceramic substrates required by semiconductor power modules, high-power integrated circuits, 5G equipment and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
preferably, the purity of the alpha alumina is more than or equal to 99.7 percent.
Preferably, the purity of the gamma alumina is more than or equal to 99.5 percent.
A preparation process of a large-size high-purity ceramic substrate comprises the following preparation steps:
(1) Modified nano gamma-alumina particles: modifying the nano gamma-alumina particles by using a coupling agent;
(2) And preparing slurry: adding the micrometer alpha-alumina, the modified nanometer gamma-alumina, the solvent and the dispersant in the formula ratio into a ball mill in proportion, performing ball milling dispersion, adding the binder and the plasticizer for secondary ball milling, and discharging to obtain casting slurry with the viscosity of 2000-3000mPa & s in a vacuum defoaming mode;
(3) And casting: casting and molding the casting slurry on a casting machine, and cutting the obtained casting blank sheet into a corresponding size and shape;
(4) And rubber discharging: placing the tape-casting green sheets in a mold, stacking to a specified thickness, placing in a hot-pressing sintering furnace for rubber discharge without applying pressure;
(5) And low-pressure forming: after the binder removal is finished, applying axial pressure to the binder in a hot-pressing sintering furnace, and maintaining the pressure for a period of time to laminate and compact the binder;
(6) And sintering: and after the lamination is finished, raising the temperature of the hot-pressing sintering furnace, adjusting the pressure, and carrying out hot-pressing sintering on the ceramic substrate to obtain the large-size high-purity ceramic substrate.
Preferably, the volume ratio of the alumina powder is 100 parts respectively, and the composition ratio is as follows: 90-92 parts of modified micron alpha-alumina and 8-10 parts of modified nano gamma-alumina. The additive amount of the solvent is 28-32% of the total mass of the alumina powder, the additive amount of the dispersing agent is 2-4% of the total mass of the alumina powder, the additive amount of the adhesive is 8-10% of the total mass of the alumina powder, and the additive amount of the plasticizer is 6-8% of the total mass of the alumina powder.
Preferably, the average particle size of the micro alpha-alumina is 0.5 μm, and the average particle size of the nano gamma-alumina is 10nm.
Preferably, the solvent is a binary azeotropic mixture of absolute ethyl alcohol and butanone, the dispersant is tributyl phosphate, the adhesive is polyvinyl butyral, and the plasticizer is polyethylene glycol.
Further, the time of ball milling dispersion is 24-48 hours, and the time of secondary ball milling is 24 hours.
Further, the glue discharging temperature is 400-600 ℃, the glue discharging atmosphere is air atmosphere, the heat preservation time is 2-4 hours, and 1 piece of green body blank is stacked.
Further, the maximum pressure of the axial gradient lamination is 20-40MPa, and the dwell time is 3-10 minutes.
Further, the sintering atmosphere is a vacuum atmosphere, and the vacuum pressure is lower than 10pa.
Furthermore, the temperature in the hot-pressing sintering furnace is 1580-1650 ℃, the heat preservation time is 1-2 hours, and the pressure in the hot-pressing sintering furnace is 60-100MPa.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the nano gamma-alumina as the sintering aid, the nano gamma-alumina has higher specific surface area and stronger chemical activity, the sintering temperature can be reduced in the sintering process, the adopted gamma-alumina can be converted into the alpha-alumina after the sintering, the process is accompanied with volume shrinkage, the control of the product size and the reduction of cracking are facilitated, in addition, the conversion of the gamma-alumina into the alpha-alumina avoids the introduction of impurities due to the addition of the sintering aid, and the purity of the substrate is improved.
2. The invention adopts the process of firstly laminating and then laminating high-temperature hot-pressing sintering, and the green sheets are not compacted in the glue discharging process, so that the organic additives in the green sheets can be completely discharged, the air holes and gas residues generated by directly laminating and then discharging the glue are avoided, the air holes are reduced, and the flatness of the ceramic substrate is improved.
The invention adopts the tape casting process and the high-temperature hot-pressing sintering process, the tape casting avoids the uniformity deterioration and the deformation of the substrate caused by uneven powder distribution, and the hot-pressing sintering temperature is lower than the normal-pressure sintering temperature, so the growth of crystal grains is inhibited, and the obtained sintered body is compact, fine in crystal grains, low in porosity and higher in strength.
Drawings
The invention is further described with reference to the following detailed description of embodiments and drawings, in which:
FIG. 1 is a schematic diagram of the preparation of the present invention.
Detailed Description
Example 1: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder is prepared from the following raw materials in parts by weight, wherein the raw materials are calculated according to the mass part of 100 parts of aluminum oxide powder: 90 parts of modified micron alpha-alumina and 10 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Proportionally adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill, and carrying out ball milling and dispersion for 48 hours; and then adding a binder and a plasticizer for secondary ball milling for 24 hours, discharging, defoaming in vacuum to obtain casting slurry with the viscosity of 2400mPa & s, and sieving for later use.
(3) And (3) casting and molding the casting slurry on a casting machine, drying the casting slurry in a casting machine drying tunnel, and cutting a casting green sheet into a corresponding size shape after a completely dried raw belt flows out of the casting machine drying tunnel along with a film belt.
(4) And placing the cut cast green sheets in a mold, stacking the cast green sheets to a specified thickness, placing the mold in a hot-pressing sintering furnace, and removing the glue, wherein the glue removing atmosphere is an air atmosphere, the glue removing temperature rise rate is 3 ℃/min, the glue removing heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace, keeping the pressure at the highest 40MPa for 5min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of a hot-pressing sintering furnace, adjusting the pressure, and carrying out hot-pressing sintering on the laminate, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1580 ℃, the heat preservation time is 1.5 hours, and the pressure in the hot-pressing sintering furnace is 100Mpa.
Example 2: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder consists of the following raw materials in parts by weight, calculated according to 100 parts by weight of aluminum oxide powder, and the composition ratio is as follows: 90 parts of modified micron alpha-alumina and 10 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Proportionally adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill, and carrying out ball milling and dispersion for 48 hours; and then adding a binder and a plasticizer for secondary ball milling for 24 hours, discharging, defoaming in vacuum to obtain casting slurry with the viscosity of 2400mPa & s, and sieving for later use.
(3) And (3) casting and molding the casting slurry on a casting machine, drying the casting slurry in a casting machine drying tunnel, and cutting a casting green sheet into a corresponding size shape after a completely dried raw belt flows out of the casting machine drying tunnel along with a film belt.
(4) And placing the cut cast green sheets in a mold, stacking to a specified thickness, placing in a hot-pressing sintering furnace, and discharging the glue, wherein the glue discharging atmosphere is an air atmosphere, the glue discharging temperature rise rate is 3 ℃/min, the glue discharging heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace in a hot-pressing sintering furnace, keeping the pressure at the maximum of 30MPa for 8min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of the hot-pressing sintering furnace and adjusting the pressure to carry out hot-pressing sintering on the laminated layer, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1615 ℃, the heat preservation time is 1 hour, and the pressure in the hot-pressing sintering furnace is 80Mpa.
Example 3: the preparation process of the large-size high-purity ceramic substrate of the embodiment comprises the following steps:
(1) The aluminum oxide powder consists of the following raw materials in parts by weight, calculated according to 100 parts by weight of aluminum oxide powder, and the composition ratio is as follows: 90 parts of modified micron alpha-alumina and 10 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Proportionally adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill, and carrying out ball milling and dispersion for 48 hours; and adding a binder and a plasticizer, carrying out secondary ball milling for 24 hours, discharging, carrying out vacuum defoaming to obtain casting slurry with the viscosity of about 2400mPa & s, and sieving for later use.
(3) And (3) carrying out tape casting molding on the tape casting slurry on a tape casting machine, drying in a tape casting machine drying tunnel, and cutting a tape casting green blank sheet into a corresponding size shape after the completely dried green tape flows out of the tape casting machine drying tunnel along with the film tape.
(4) And placing the cut cast green sheets in a mold, stacking the cast green sheets to a specified thickness, placing the mold in a hot-pressing sintering furnace, and removing the glue, wherein the glue removing atmosphere is an air atmosphere, the glue removing temperature rise rate is 3 ℃/min, the glue removing heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace in a hot-pressing sintering furnace, keeping the pressure at the maximum of 20MPa for 10min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of the hot-pressing sintering furnace and adjusting the pressure to carry out hot-pressing sintering on the laminated layer, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1650 ℃, the heat preservation time is 1 hour, and the pressure in the hot-pressing sintering furnace is 60Mpa.
Example 4: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder is prepared from the following raw materials in parts by weight, wherein the raw materials are calculated according to the mass part of 100 parts of aluminum oxide powder: 92 parts of modified micron alpha-alumina and 8 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Proportionally adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill, and carrying out ball milling and dispersion for 48 hours; and adding a binder and a plasticizer, carrying out secondary ball milling for 24 hours, discharging, carrying out vacuum defoaming to obtain casting slurry with the viscosity of about 2400mPa & s, and sieving for later use.
(3) And (3) casting and molding the casting slurry on a casting machine, drying the casting slurry in a casting machine drying tunnel, and cutting a casting green sheet into a corresponding size shape after a completely dried raw belt flows out of the casting machine drying tunnel along with a film belt.
(4) And placing the cut cast green sheets in a mold, stacking to a specified thickness, placing in a hot-pressing sintering furnace, and discharging the glue, wherein the glue discharging atmosphere is an air atmosphere, the glue discharging temperature rise rate is 3 ℃/min, the glue discharging heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace in a hot-pressing sintering furnace, keeping the pressure at the maximum of 20MPa for 5min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of the hot-pressing sintering furnace and adjusting the pressure to carry out hot-pressing sintering on the laminated layer, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1580 ℃, the heat preservation time is 1.5 hours, and the pressure in the hot-pressing sintering furnace is 100Mpa.
Example 5: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder consists of the following raw materials in parts by weight, calculated according to 100 parts by weight of aluminum oxide powder, and the composition ratio is as follows: 92 parts of modified micron alpha-alumina and 8 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill in proportion, and performing ball milling and dispersion for 48 hours; and adding a binder and a plasticizer, carrying out secondary ball milling for 24 hours, discharging, carrying out vacuum defoaming to obtain casting slurry with the viscosity of about 2400mPa & s, and sieving for later use.
(3) And (3) casting and molding the casting slurry on a casting machine, drying the casting slurry in a casting machine drying tunnel, and cutting a casting green sheet into a corresponding size shape after a completely dried raw belt flows out of the casting machine drying tunnel along with a film belt.
(4) And placing the cut cast green sheets in a mold, stacking to a specified thickness, placing in a hot-pressing sintering furnace, and discharging the glue, wherein the glue discharging atmosphere is an air atmosphere, the glue discharging temperature rise rate is 3 ℃/min, the glue discharging heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace in a hot-pressing sintering furnace, keeping the pressure at the maximum of 30MPa for 8min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of the hot-pressing sintering furnace and adjusting the pressure to carry out hot-pressing sintering on the laminated layer, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1615 ℃, the heat preservation time is 1 hour, and the pressure in the hot-pressing sintering furnace is 80Mpa.
Example 6: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder consists of the following raw materials in parts by weight, calculated according to 100 parts by weight of aluminum oxide powder, and the composition ratio is as follows: 92 parts of modified micron alpha-alumina and 8 parts of modified nano gamma-alumina; the addition amount of a binary azeotropic mixture of absolute ethyl alcohol and butanone is 28% of the total mass of the alumina powder, the addition amount of tributyl phosphate is 4% of the total mass of the alumina powder, the addition amount of polyvinyl butyral is 8% of the total mass of the alumina powder, and the addition amount of polyethylene glycol is 6% of the total mass of the alumina powder.
(2) Adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant into a ball mill in proportion, and performing ball milling and dispersion for 48 hours; and adding a binder and a plasticizer, carrying out secondary ball milling for 24 hours, discharging, carrying out vacuum defoaming to obtain casting slurry with the viscosity of about 2400mPa & s, and sieving for later use.
(3) And (3) casting and molding the casting slurry on a casting machine, drying the casting slurry in a casting machine drying tunnel, and cutting a casting green sheet into a corresponding size shape after a completely dried raw belt flows out of the casting machine drying tunnel along with a film belt.
(4) And placing the cut cast green sheets in a mold, stacking the cast green sheets to a specified thickness, placing the mold in a hot-pressing sintering furnace, and removing the glue, wherein the glue removing atmosphere is an air atmosphere, the glue removing temperature rise rate is 3 ℃/min, the glue removing heat preservation temperature is 600 ℃, and the heat preservation time is 3 hours.
(5) And after the glue discharging is finished, continuously applying axial pressure to the hot-pressing sintering furnace in a hot-pressing sintering furnace, keeping the pressure at the maximum of 20MPa for 10min, and compacting the lamination.
(6) And after lamination and compaction, raising the temperature of the hot-pressing sintering furnace and adjusting the pressure to carry out hot-pressing sintering on the laminated layer, wherein the sintering atmosphere is a vacuum atmosphere, the sintering temperature is 1650 ℃, the heat preservation time is 1 hour, and the pressure in the hot-pressing sintering furnace is 60Mpa.
Comparative example 1: the preparation process of the large-size high-purity ceramic substrate comprises the following steps:
(1) The aluminum oxide powder consists of the following raw materials in parts by weight, calculated according to 100 parts by weight of aluminum oxide powder, and the composition ratio is as follows: 90 parts of modified micron alpha-alumina and 10 parts of modified nano gamma-alumina;
(2) Adding the weighed micron alpha-alumina, the modified nano gamma-alumina, the polyvinyl alcohol and the grinding balls into a ball mill in proportion, performing ball milling dispersion for 48 hours, drying and sieving for later use;
(3) Adding the mixture into a female die, and compacting and leveling by using a scraper;
(4) And (3) placing the female die with the uniformly mixed raw materials into a hot-pressing sintering furnace, sintering at 1650 ℃ for 1 hour in vacuum atmosphere and at the highest pressure of 30MPa in a sectional high-temperature high-pressure manner, and obtaining the ceramic substrate.
The results of the substrate testing for example 1~6 and comparative example 1 are shown in table 1.
The above embodiments are merely illustrative of the present invention, and not restrictive, and many modifications and changes may be made by those skilled in the art without departing from the spirit of the invention, and it is intended that all such modifications and changes as fall within the true spirit of the invention and the scope of the appended claims be interpreted by those skilled in the art.
Claims (5)
1. A preparation process of a large-size high-purity ceramic substrate is characterized by comprising the following steps:
s1, modified nano gamma-alumina particles: modifying the nano gamma-alumina particles by using a coupling agent;
s2, preparing slurry: adding the modified micron alpha-alumina, the modified nano gamma-alumina, the solvent and the dispersant in the formula ratio into a ball mill in proportion, carrying out ball milling dispersion, adding the binder and the plasticizer after the dispersion is finished, carrying out secondary ball milling, discharging, and carrying out vacuum defoaming to obtain casting slurry with the viscosity of 2000-3000mPa & s;
s3, casting: casting and molding the casting slurry by using a casting machine, and cutting the obtained casting blank sheet into a corresponding size and shape;
s4, removing glue: placing the casting green sheet into a mold, stacking to a specified thickness, placing into a hot-pressing sintering furnace for glue discharging, and not applying pressure;
s5, low-pressure forming: after the binder removal is finished, applying axial gradient pressure to the binder in a hot-pressing sintering furnace, and maintaining the pressure for a period of time to laminate and compact the binder;
s6, sintering: the temperature of the hot-pressing sintering furnace is raised, the pressure is adjusted, and the hot-pressing sintering is carried out on the hot-pressing sintering furnace to obtain a large-size high-purity ceramic substrate;
in the step S2, the powder comprises the following components in percentage by volume: 90-92 parts of modified micron alpha-alumina and 8-10 parts of modified nano gamma-alumina; the additive amount of the solvent is 28-32% of the total mass of the alumina powder, the additive amount of the dispersant is 2-4% of the total mass of the alumina powder, the additive amount of the binder is 8-10% of the total mass of the alumina powder, and the additive amount of the plasticizer is 6-8% of the total mass of the alumina powder; in the step S5, the axial gradient pressure is 20-40MPa, and the pressure maintaining time is 3-10 minutes; in the step S6, the pressure of the hot-pressing sintering furnace is 60-100Mpa, the sintering temperature is 1580-1650 ℃, the sintering atmosphere is vacuum atmosphere, and the heat preservation time is 1-2 hours.
2. The process for preparing a large-sized high-purity ceramic substrate according to claim 1, wherein in the step S2, the solvent is a binary azeotropic mixture of absolute ethyl alcohol and butanone, the dispersant is tributyl phosphate, the binder is polyvinyl butyral, and the plasticizer is polyethylene glycol.
3. The process for preparing a large-sized high-purity ceramic substrate according to claim 1, wherein in the step S2, the time for ball milling dispersion is 24-48 hours, and the time for secondary ball milling is 24 hours.
4. The process for preparing a large-sized high-purity ceramic substrate according to claim 1, wherein the modified micron α -alumina has an average particle size of 0.5 μm and the nano γ -alumina has an average particle size of 10nm.
5. The process of claim 1, wherein in the step S4, the de-gumming temperature is 400-600 ℃, the de-gumming atmosphere is air atmosphere, the holding time is 2-4 hours, and 1 or more green bodies are stacked.
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