CN116161970A - Lamination sintering process method of high-performance silicon nitride ceramic substrate - Google Patents
Lamination sintering process method of high-performance silicon nitride ceramic substrate Download PDFInfo
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Abstract
The invention discloses a lamination sintering process method of a high-performance silicon nitride ceramic substrate. Cutting a silicon nitride casting blank sheet prepared by casting forming into proper size, preparing deionized water, a dispersing agent and boron nitride powder into suspension slurry according to a proportion, spraying the suspension slurry on the surface of the cut casting blank sheet, and then drying the sprayed casting blank sheet; placing the tape casting blank lamination subjected to powder coating into a boron nitride ceramic sagger, pressing a boron nitride ceramic block with holes on the silicon nitride lamination blank, and performing glue discharging treatment on the silicon nitride lamination blank placed in the boron nitride sagger; and continuously pressing a tungsten carbide ceramic block on the silicon nitride laminated blank placed in the boron nitride sagger after glue discharge, pressing the tungsten carbide ceramic block on the boron nitride ceramic block, and sintering the silicon nitride laminated blank in a sintering furnace. The invention can produce large-area silicon nitride ceramic substrate materials with higher heat conductivity, excellent mechanical property and lower production cost.
Description
Technical field:
the invention belongs to the technical field of high-heat-conductivity silicon nitride ceramic substrate production, and particularly relates to a lamination sintering process method of a high-performance silicon nitride ceramic substrate.
The background technology is as follows:
currently, global power device technology is evolving towards higher currents, higher voltages, and higher power densities, whereby the large heat generated during operation of power devices presents a significant challenge for their stable service. In the use process of the power device, the used insulating substrate material is a key point affecting the whole heat dissipation of the power device. Because the power device is often required to face complex mechanical environments (such as jolt and vibration) in the use process, the insulating substrate material for the power device is also required to have good heat conduction capability and excellent mechanical properties.
The silicon nitride ceramic has the advantages of high resistivity, high theoretical thermal conductivity and good force performance, and has very stable physical and chemical properties, thus being a ceramic substrate material for power devices with very competitive force. However, the sintering preparation technology of silicon nitride is an important bottleneck restricting the industrial production thereof. At present, two modes for preparing the high-heat-conductivity high-strength and high-toughness silicon nitride ceramic substrate are available: one is to sinter a bulk monolithic ceramic of a specific size and then process it to cut it to a specific size, but this approach is costly and difficult to process and difficult to meet mass production requirements. The other is to prepare a casting slice by a casting molding method, and then prepare the silicon nitride ceramic substrate by a proper glue discharging and air pressure sintering process. Compared with the previous mode, the process combining tape casting and air pressure sintering has huge cost and efficiency advantages, and is the optimal solution for preparing high-performance silicon nitride ceramics on a large scale in the current industry.
Nevertheless, there are still many technical difficulties in preparing high performance ceramics by combining tape casting with a venting and air pressure sintering process. The most important of these problems are two: firstly, how to ensure that a silicon nitride ceramic casting blank piece obtained by casting molding keeps the integral flatness after glue discharging and air pressure sintering; and secondly, the stack sintering of the blank sheets after tape casting is effectively realized without bonding.
The Chinese patent CN201910167833.X discloses a high heat conduction silicon nitride ceramic substrate and a preparation method thereof, wherein the ceramic substrate is formed by stacking a plurality of silicon nitride casting blanks, two adjacent silicon nitride casting blanks are provided with an intermediate layer, the intermediate layer consists of two graphite plates and two graphite strips, the two graphite strips are respectively positioned between two ends of the two graphite plates and form a cavity, the graphite plates are provided with a plurality of holes communicated with the cavity, and a slurry separation layer is arranged between the graphite plates and the corresponding silicon nitride casting blanks. However, the preparation method requires complicated accessory structure and complicated operation, which is unfavorable for large-scale industrial production. Moreover, the graphite plate is in contact with the silicon nitride casting biscuit, so that carbon elements invade the sintered silicon nitride ceramic substrate, the resistivity is reduced, and the graphite plate is not beneficial to being used as an insulating heat-conducting substrate.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The invention comprises the following steps:
the invention aims to provide a lamination sintering process method of a high-performance silicon nitride ceramic substrate, which improves the problems existing in the glue discharging and sintering process after the casting molding of the silicon nitride ceramic, thereby overcoming the defects in the prior art.
In order to achieve the above object, the present invention provides a lamination sintering process method of a high performance silicon nitride ceramic substrate, comprising the steps of:
(1) Cutting a silicon nitride casting blank sheet prepared by casting forming into proper size, preparing deionized water, a dispersing agent and boron nitride powder into suspension slurry according to a proportion, wherein the dispersing agent has the effect of effectively relieving the agglomeration problem of the boron nitride powder, spraying the suspension slurry on the surface of the cut casting blank sheet, and then drying the sprayed casting blank sheet to finish surface powder coating of the casting blank sheet;
(2) Placing the tape casting blank sheet laminated after powder coating into a boron nitride ceramic sagger, and pressing a boron nitride ceramic block with holes on the silicon nitride laminated blank sheet, wherein the size of the boron nitride ceramic block is matched with that of the silicon nitride laminated blank sheet so as to prevent warping in the glue discharging process and ensure gasification escape of organic matters in the glue discharging process, and the purpose of selecting the boron nitride ceramic block is that the physical and chemical properties are stable, and the boron nitride ceramic block cannot react and adhere with the silicon nitride blank sheet in the glue discharging and later sintering processes; performing glue discharging treatment on the silicon nitride laminated blank placed in the boron nitride sagger;
(3) Continuously pressing a tungsten carbide ceramic block on a silicon nitride laminated blank placed in a boron nitride sagger after glue discharge, wherein the tungsten carbide ceramic block is pressed on the boron nitride ceramic block, the size of the tungsten carbide ceramic block is matched with that of the silicon nitride laminated blank, and sufficient vertical pressing force is provided for the silicon nitride laminated blank in the sintering process so as to prevent the blank from warping, and the tungsten carbide ceramic block is selected to have stable physicochemical properties, high density and high melting point and can well maintain the shape in the high-temperature sintering process; and sintering the silicon nitride laminated blank in a sintering furnace.
Preferably, in the technical scheme, 90-95 wt% of deionized water, 4-9 wt% of boron nitride powder and 0.2-1 wt% of dispersing agent are prepared into suspension slurry.
Preferably, in the technical scheme, the dispersing agent is one of castor oil, fish oil, oleic acid and stearic acid, and the aim is to enable the boron nitride powder to have better suspension dispersion performance in deionized water.
Preferably, in the technical scheme, the average particle size of the boron nitride powder is 10-30 μm.
Preferably, in the technical scheme, a spray gun with the caliber of 100-800 mu m is adopted, compressed air flow with the air pressure of 0.2-0.5 Mpa is sprayed out from a central hole of the spray gun, a negative pressure area is formed at the front end of the spray nozzle, suspension slurry in the container is sucked into the negative pressure area and sprayed out from the spray nozzle, the suspension slurry rapidly enters the compressed air flow to be rapidly diffused, the suspension slurry is micronized, and the slurry flies to and adheres to the surface of a silicon nitride casting blank sheet in a paint mist shape, so that a continuous coating film is formed.
Preferably, in the technical scheme, the sprayed casting blank sheet is subjected to forced air drying by using hot air at 60 ℃.
Preferably, in the technical scheme, the thickness of the surface powder coating of the casting blank sheet needs to reach 100-300 mu m.
Preferably, in the technical scheme, the number of the laminated laying layers of the powder-coated casting blank is less than or equal to 30.
Preferably, in the technical scheme, the proportion of the hole area of the boron nitride ceramic block to the area of the boron nitride ceramic block is more than or equal to 50 percent, and the mass of the boron nitride ceramic block is more than 1 time of the total mass of the silicon nitride laminated blank.
Preferably, in the technical scheme, the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 500-1000 ℃, the heating rate is 0.5-5 ℃/min, and the heat preservation time is 24-72 hours.
Preferably, in the technical scheme, the mass of the tungsten carbide ceramic block is required to be 2 times greater than the total mass of the silicon nitride laminated blank.
Preferably, in the technical scheme, firstly, the temperature is kept for 1 to 5 hours under the condition of flowing hydrogen at the temperature of between 500 and 1000 ℃; then heating to 1900-2000 deg.C, heating at 5-15 deg.C/min for 3-15 hr, maintaining nitrogen pressure of 1-20 MPa, cooling to 1200 deg.C, and cooling with furnace.
Compared with the prior art, the invention has the following beneficial effects:
first, the tape casting sheets are stacked together to remove glue and sintered without bonding and warping, and the tape casting sheets are sintered uniformly. Secondly, finally preparing the large-area silicon nitride ceramic substrate material with higher heat conductivity, excellent mechanical property and lower production cost through a proper glue discharging and sintering system.
Description of the drawings:
FIG. 1 is a diagram showing a sintered state of a cast silicon nitride laminate in a boron nitride sagger according to the present invention;
reference numerals: 1-boron nitride sagger, 2-tungsten carbide ceramic block, 3-boron nitride ceramic block, 4-silicon nitride ceramic blank and 5-boron nitride powder coating layer.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
A lamination sintering process method of a high-performance silicon nitride ceramic substrate comprises the following steps:
(1) Cutting a silicon nitride casting blank sheet prepared by casting into proper size, preparing deionized water with the weight percentage of 90-95 wt%, boron nitride powder with the weight percentage of 4-9 wt% and a dispersing agent with the weight percentage of 0.2-1 wt% into suspension slurry, spraying the suspension slurry on the surface of the cut casting blank sheet, and then drying the sprayed casting blank sheet to finish surface powder coating of the casting blank sheet, wherein the thickness of the surface powder coating is required to reach 100-300 mu m;
(2) Placing the casting blank lamination subjected to powder coating into a boron nitride ceramic sagger, and pressing a boron nitride ceramic block with holes on the silicon nitride lamination blank, wherein the proportion of the hole area of the boron nitride ceramic block to the area of the boron nitride ceramic block is more than or equal to 50%, and the mass of the boron nitride ceramic block is more than 1 time of the total mass of the silicon nitride lamination blank; performing glue discharging treatment on the silicon nitride laminated blank placed in the boron nitride sagger, wherein the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 500-1000 ℃, the heating rate is 0.5-5 ℃/min, and the heat preservation time is 24-72 hours;
(3) Continuously pressing a tungsten carbide ceramic block on the silicon nitride laminated blank placed in the boron nitride sagger after glue discharge, wherein the tungsten carbide ceramic block is pressed on the boron nitride ceramic block, and the mass of the tungsten carbide ceramic block is required to be 2 times greater than the total mass of the silicon nitride laminated blank; sintering the silicon nitride laminated blank in a sintering furnace, and firstly preserving heat for 1-5 h under the conditions of 500-1000 ℃ and flowing hydrogen; then heating to 1900-2000 deg.C, heating at 5-15 deg.C/min for 3-15 hr, maintaining nitrogen pressure of 1-20 MPa, cooling to 1200 deg.C, and cooling with furnace.
Example 1
(1) Cutting a casting blank into a size of 20cm multiplied by 20cm, preparing suspension slurry from 92wt% of deionized water, 7.5wt% of boron nitride powder with an average particle size of 15 mu m and 0.5wt% of castor oil, spraying the suspension slurry on the surface of the cut casting blank, wherein the aperture of a spray gun used for spraying is 300 mu m, and the drying process of the sprayed casting blank is to use hot air at 60 ℃ for blast drying, and the thickness of the surface powder after drying reaches 200 mu m;
(2) Stacking 10 silicon nitride casting blank sheets with powder coated on the surfaces, placing the silicon nitride casting blank sheets in a boron nitride ceramic sagger, and pressing and placing boron nitride ceramic blocks with holes on the laminated blank sheets, wherein the mass of the boron nitride ceramic blocks is equal to that of the laminated blank sheets, and the hole areas of the ceramic blocks account for 60% of the area of the boron nitride ceramic blocks; the glue discharging process comprises the following steps: the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 550 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 30 hours;
(3) Continuously pressing a compact tungsten carbide ceramic block with the mass being 2 times of the total mass of the laminated blank on the silicon nitride laminated blank placed in the boron nitride sagger after glue discharge; firstly, preserving heat for 3 hours under the flowing hydrogen condition of 800 ℃; then the temperature is raised to 1950 ℃, the heating rate is 10 ℃/min, the heat preservation time is 6 hours, the nitrogen pressure of 6MPa is maintained, then the temperature is reduced to 1200 ℃, and finally the furnace is cooled.
The high-performance silicon nitride ceramic substrate is finally prepared through the process, the surface of the substrate is free from warpage, adhesion between the substrates does not occur, the final substrate thermal conductivity is higher than 80W/(m.k), and the bending strength is higher than 800MPa.
Example 2
(1) Cutting a casting blank into a size of 25cm multiplied by 25cm, preparing suspension slurry from 91wt% of deionized water, 8wt% of boron nitride powder with an average particle size of 20 mu m and 1wt% of castor oil, spraying the suspension slurry on the surface of the cut casting blank, wherein the aperture of a spray gun used for spraying is 500 mu m, and the drying process of the sprayed casting blank is to use hot air at 60 ℃ for blast drying, and the thickness of the surface powder after drying reaches 250 mu m;
(2) Stacking 15 silicon nitride casting blank sheets with powder coated on the surfaces, placing the silicon nitride casting blank sheets in a boron nitride ceramic sagger, and pressing and placing boron nitride ceramic blocks with holes on the laminated blank sheets, wherein the mass of the boron nitride ceramic blocks is equal to that of the laminated blank sheets, and the hole areas of the ceramic blocks account for 70% of the area of the boron nitride ceramic blocks; the glue discharging process comprises the following steps: the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 600 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 36 hours;
(3) Continuously pressing a compact tungsten carbide ceramic block with the mass being 3 times of the total mass of the laminated blank on the silicon nitride laminated blank placed in the boron nitride sagger after glue discharge; firstly, preserving heat for 2 hours under the flowing hydrogen condition at 700 ℃; then the temperature is raised to 2000 ℃, the heating rate is 10 ℃/min, the heat preservation time is 4 hours, the nitrogen pressure of 7MPa is maintained, then the temperature is reduced to 1200 ℃, and finally the furnace is cooled.
The high-performance silicon nitride ceramic substrate is finally prepared through the process, the surface of the substrate is free from warpage, adhesion between the substrates does not occur, the final substrate thermal conductivity is greater than 85W/(m.k), and the bending strength is higher than 750MPa.
Example 3
(1) Cutting a casting blank into 30cm multiplied by 30cm, preparing suspension slurry from 93wt% of deionized water, 6.5wt% of boron nitride powder with an average particle size of 30 mu m and 0.5wt% of castor oil, spraying the suspension slurry on the surface of the cut casting blank, wherein the aperture of a spray gun used for spraying is 400 mu m, and the drying process of the sprayed casting blank is to use hot air at 60 ℃ for blast drying, and the thickness of the surface powder after drying reaches 230 mu m;
(2) Stacking 20 silicon nitride casting blank sheets with powder coated on the surfaces, placing the silicon nitride casting blank sheets in a boron nitride ceramic sagger, and pressing and placing boron nitride ceramic blocks with holes on the laminated blank sheets, wherein the mass of the boron nitride ceramic blocks is equal to that of the laminated blank sheets, and the hole areas of the ceramic blocks account for 70% of the area of the boron nitride ceramic blocks; the glue discharging process comprises the following steps: the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 25 hours;
(3) Continuously pressing a compact tungsten carbide ceramic block with the mass being 3 times of the total mass of the laminated blank on the silicon nitride laminated blank placed in the boron nitride sagger after glue discharge; firstly, preserving heat for 3 hours under the flowing hydrogen condition at 700 ℃; then the temperature is raised to 1950 ℃, the heating rate is 10 ℃/min, the heat preservation time is 15 hours, the nitrogen pressure of 10MPa is maintained, then the temperature is reduced to 1200 ℃, and finally the furnace is cooled.
The high-performance silicon nitride ceramic substrate is finally prepared through the process, the surface of the substrate is free from warpage, adhesion between the substrates does not occur, the final substrate thermal conductivity is greater than 90W/(m.k), and the bending strength is higher than 750MPa.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A lamination sintering process method of a high-performance silicon nitride ceramic substrate comprises the following steps of
(1) Cutting a cast silicon nitride blank sheet prepared by casting into proper sizes, preparing deionized water, a dispersing agent and boron nitride powder into suspension slurry according to a proportion, spraying the suspension slurry on the surface of the cut cast blank sheet, and then drying the sprayed cast blank sheet to finish surface powder coating of the cast blank sheet;
(2) Placing the casting blank lamination subjected to powder coating into a boron nitride ceramic sagger, and pressing a boron nitride ceramic block with holes on the silicon nitride lamination blank, wherein the size of the boron nitride ceramic block is matched with that of the silicon nitride lamination blank; performing glue discharging treatment on the silicon nitride laminated blank placed in the boron nitride sagger;
(3) Continuously pressing a tungsten carbide ceramic block on a silicon nitride laminated blank placed in the boron nitride sagger after glue discharge, wherein the tungsten carbide ceramic block is pressed on the boron nitride ceramic block, and the size of the tungsten carbide ceramic block is matched with that of the silicon nitride laminated blank; and sintering the silicon nitride laminated blank in a sintering furnace.
2. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: in the step (1), 90-95 wt% of deionized water, 4-9 wt% of boron nitride powder and 0.2-1 wt% of dispersing agent are prepared into suspension slurry.
3. The laminated sintering process of a high-performance silicon nitride ceramic substrate according to claim 2, wherein: the dispersing agent is one of castor oil, fish oil, oleic acid and stearic acid.
4. The laminated sintering process of a high-performance silicon nitride ceramic substrate according to claim 2, wherein: the average particle size of the boron nitride powder is 10 to 30 μm.
5. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: the thickness of the surface powder coating of the casting blank sheet in the step (1) needs to reach 100-300 mu m.
6. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: and (3) the number of the laminated laying layers of the powder-coated casting blank sheet in the step (2) is less than or equal to 30.
7. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: in the step (2), the proportion of the hole area of the boron nitride ceramic block to the area of the boron nitride ceramic block is more than or equal to 50 percent, and the mass of the boron nitride ceramic block is more than 1 time of the total mass of the silicon nitride laminated blank.
8. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: the glue discharging process in the step (2) is as follows: the glue discharging atmosphere is flowing nitrogen, the glue discharging temperature is 500-1000 ℃, the heating rate is 0.5-5 ℃/min, and the heat preservation time is 24-72 hours.
9. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: the mass of the tungsten carbide ceramic block in the step (3) is required to be 2 times larger than the total mass of the silicon nitride laminated blank.
10. The laminated sintering process of a high performance silicon nitride ceramic substrate according to claim 1, wherein: the sintering process in the step (3) is as follows: firstly preserving heat for 1-5 h at 500-1000 ℃ under the flowing hydrogen condition; then heating to 1900-2000 deg.C, heating at 5-15 deg.C/min for 3-15 hr, maintaining nitrogen pressure of 1-20 MPa, cooling to 1200 deg.C, and cooling with furnace.
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