CN116283304B - Preparation method of large-size ceramic substrate - Google Patents
Preparation method of large-size ceramic substrate Download PDFInfo
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- CN116283304B CN116283304B CN202310390628.6A CN202310390628A CN116283304B CN 116283304 B CN116283304 B CN 116283304B CN 202310390628 A CN202310390628 A CN 202310390628A CN 116283304 B CN116283304 B CN 116283304B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 239000000758 substrate Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 238000003825 pressing Methods 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 229920000642 polymer Polymers 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims description 20
- 238000011068 loading method Methods 0.000 claims description 15
- 239000012798 spherical particle Substances 0.000 claims description 15
- 238000007906 compression Methods 0.000 claims description 12
- 239000011268 mixed slurry Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- 230000006835 compression Effects 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000004014 plasticizer Substances 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 9
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
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- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 235000021323 fish oil Nutrition 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims description 3
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
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- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
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- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 3
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- 239000000463 material Substances 0.000 abstract description 9
- 229910052582 BN Inorganic materials 0.000 description 20
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 20
- 238000000465 moulding Methods 0.000 description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000009694 cold isostatic pressing Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 238000002955 isolation Methods 0.000 description 6
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- 238000003892 spreading Methods 0.000 description 5
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- 239000007789 gas Substances 0.000 description 4
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- 239000000395 magnesium oxide Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000009461 vacuum packaging Methods 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000009690 centrifugal atomisation Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
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- 238000001816 cooling Methods 0.000 description 2
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- 239000000203 mixture Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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Abstract
The invention relates to a preparation method of a large-size ceramic substrate, which comprises the following steps: mixing ceramic powder with preset average particle size, sintering aid with preset average particle size and polymer forming agent to obtain mixed material, making into particles with preset average particle size, uniformly laying the obtained particles in metal mold with preset condition, pressing to obtain blank, and directly sintering. The invention has the advantages of few preparation procedures, high efficiency and good product performance, the maximum side length of the blank body can reach 250mm, the thinnest thickness can reach 0.3mm, the maximum side length of the sintered ceramic substrate is 200mm, and the thinnest thickness is 0.25mm.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of a large-size ceramic substrate.
Background
With the increasing demands of high-power semiconductor devices and intelligent power components, ceramic substrates are increasingly used due to their excellent heat dissipation characteristics, low thermal resistance, high insulation, long service life and the like. Ceramic substrates are typically thin, with a thickness that varies with the substrate material and application, but is typically between 0.25mm and 2 mm.
In the prior art, a casting or mould pressing method is mostly adopted for forming the ceramic sheet. The casting forming is a slurry doctor blade method, which mixes ceramic slurry and macromolecule solution into uniform slurry, and then controls the thickness of the slurry on a conveyor belt through the height of a scraper, and the slurry is dried and solidified subsequently to form a blank body. A large amount of organic solvents and high molecular forming agents are used for tape casting, so that the method has large drying shrinkage and is suitable for forming ultrathin ceramic plates (less than 0.2 mm); the method has the defects that 1) the types of the used organic solvents are multiple, the irritation is high, and the environmental assessment cost such as waste liquid discharge is increased; 2) The added macromolecule content is more (generally more than 20 percent), so that a separate glue discharging process is needed before the blank body is subjected to glue discharging; 3) The forming agent can be discharged in the form of gas or aerosol in the process of discharging the glue, and a set of independent tail gas treatment equipment is needed; 4) In order to prevent the blank from cracking, the temperature rise in the glue discharging process is slow, the heating process is usually more than or equal to 20 hours, and the temperature rise is up to more than 40 hours. For thicker blanks, a multilayer ultrathin lamination-encapsulation-isostatic pressing mode is generally adopted (patent CN114804840A is an alumina ceramic substrate and a preparation method and application thereof).
And the press molding is to mix ceramic powder with a small amount of polymer molding agent (the content is usually less than or equal to 5 wt.%) and press molding the mixture on a press through a metal die; because the polymer forming agent is less, and the ceramic powder has no plastic deformation capability, the press forming is not generally used for forming a sheet blank less than 1 mm; in most cases, in order to obtain a part with the thickness smaller than 1mm, the part needs to be thinned to a required size through grinding and other means after sintering; on the one hand, the procedures and the manufacturing cost are increased, and on the other hand, as the ceramics are made of brittle materials, the mechanical properties of the ceramic plate are inevitably deteriorated and influenced in the processing process. In the pressing process, the blank with the thickness less than 1mm is extremely easy to deform and crack due to the elastic aftereffect, the strength of the formed blank is difficult to support and transport, and the deformation control in the sintering process is difficult. The patent CN112661518A discloses a two-step pressing forming method of a high-heat-conductivity silicon nitride ceramic insulating plate, which comprises the steps of firstly pressing the silicon nitride ceramic insulating plate into a blank by a metal die, then placing the blank into a steel plate for vacuum packaging and pressing the steel plate into a sheet with high pressure (more than or equal to 300 and MPa) by cold isostatic pressing to prepare the sheet with the thickness of 0.25 mm. In this way, the high-pressure isostatic cool pressing is beneficial to the slowing down of elasticity aftereffect and the improvement of blank strength, thereby being beneficial to later transfer and sintering, but the molding process is firstly carried out, then the steel plate is put on for vacuum packaging and cold isostatic pressing, and then the vacuum packaging is disassembled to take out the product, so that the molding process is more, and the equipment and manufacturing cost are increased.
Disclosure of Invention
The invention provides a preparation method of a large-size ceramic substrate aiming at the defects of the prior art. The preparation process is few, the efficiency is high, the product performance is good, the maximum size of the blank body can reach 250mm, the thinnest thickness can reach 0.3mm, the maximum size of the sintered substrate can reach 200mm, and the thinnest thickness can reach 0.25mm.
The invention provides a preparation method of a large-size ceramic substrate, which comprises the following steps: mixing ceramic powder with preset average particle size, sintering aid with preset average particle size and polymer forming agent to obtain mixed material, making into particles with preset average particle size, uniformly laying the obtained particles in metal mold with preset condition, pressing to obtain blank, and directly sintering.
In some embodiments of the invention, the particles have a predetermined average particle size of 40-120 μm.
According to the invention, the particles have a predetermined average particle diameter of, for example, 40 μm, 50 μm, 60 μm, 80 μm, 100 μm or 120 μm.
In some embodiments of the invention, the particles are near-spherical particles.
In some embodiments of the invention, the preset average particle size of the ceramic powder and the sintering aid are each less than or equal to 1 μm; preferably 0.3-1 μm; more preferably 0.5-0.8. Mu.m.
In some embodiments of the present invention, the metal mold is made of Cr12MoV mold steel or cemented carbide.
In some embodiments of the present invention, the preset conditions of the metal mold are: the Rockwell hardness of the working surface is more than or equal to 60, the roughness of the working surface is less than or equal to 0.2, and the parallelism of the working surface is less than or equal to 0.02.
In some embodiments of the invention, the charge height of the metal mold is calculated from a preset green body thickness and a compression ratio of the particles.
In some embodiments of the present invention, the calculation formula of the charge height of the metal mold is shown in formula (1),
h Material =h Blank /σ Compression ratio （1）
Wherein, h Material is the charging height of the metal mould, h Blank is the preset blank thickness and sigma Compression ratio is the compression ratio of the particles.
According to the invention, the thickness of the preset blank body is more than or equal to 0.3 mm; for example 0.3 mm, 0.4 mm, 0.5 mm, 0.8 mm or 1.1mm.
According to the invention, the compression ratio of the particles is 0.3-0.6.
In some embodiments of the invention, the side length of the metal mold is no greater than 250 mm.
According to the invention, the dimensions of the metal mould are 180 mm ×250 mm or 130 mm ×130 mm.
In some embodiments of the invention, the polymer forming agent is added in an amount of 5wt.% or less of the total amount of the mixed raw materials.
In some embodiments of the invention, the polymeric molding agent includes a binder, a dispersant, and a plasticizer.
In some embodiments of the invention, the binder is added in an amount of 2wt.% or less of the total amount of the mixed raw materials.
In some embodiments of the invention, the dispersant is added in an amount of 1wt.% or less of the total amount of the mixed raw materials.
In some embodiments of the invention, the plasticizer is added in an amount of 2wt.% or less of the total amount of the blend stock.
In some embodiments of the invention, the binder comprises at least one of polyvinyl butyral, polyvinyl acetate, polyethylene glycol.
In some embodiments of the invention, the dispersant comprises at least one of glycerol trioleate, fish oil, and castor oil phosphate.
In some embodiments of the invention, the plasticizer comprises at least one of phthalate, dibutyl phthalate, and dioctyl phthalate.
In some embodiments of the invention, the method of pressing is gradient compression; the conditions of the gradient pressurizing and pressing are as follows: the pressure is less than or equal to 20 MPa to 15s, and the pressure is 80 to 150 to MPa for 5 to 15s.
In some embodiments of the invention, the preparation method comprises the following specific steps:
S1: mixing ceramic powder, sintering aid and polymer forming agent to obtain mixed raw material, and uniformly ball-milling by wet method to obtain mixed slurry;
S2: centrifuging or pressurizing the mixed slurry prepared in the step S1, atomizing and drying to obtain nearly spherical particles with the average particle diameter of 40-120 mu m;
S3: uniformly paving the nearly spherical particles prepared in the step S2 in a metal mold, wherein the Rockwell hardness of the working surface of the metal mold is more than or equal to 60, the roughness of the working surface is less than or equal to 0.2, and the parallelism of the working surface is less than or equal to 0.02; calculating to obtain the loading height of the metal mold through the preset blank thickness and the compression ratio of the particles;
S4: and carrying out gradient pressurizing and pressing on the nearly spherical particles paved in the metal mold on a press to form a blank, wherein the conditions of the gradient pressurizing and pressing are as follows: the pressure is less than or equal to 20 MPa to 15s, and the pressure is 80 to 150 to MPa for 5 to 10s; then slowly releasing pressure;
s5: sintering the blank body prepared in the step S4 at 1850-1950 ℃ for more than or equal to 3 hours.
In some embodiments of the invention, the ceramic frit comprises silicon nitride or aluminum nitride.
In some embodiments of the invention, the sintering aid comprises at least one of yttria (Y 2O3), magnesia (MgO), and calcium fluoride (CaF 2).
In some embodiments of the invention, the sintering aid is added in an amount of 3wt to 6wt.% of the total amount of mixed raw materials.
In some embodiments of the present invention, the sintering process of the green body in the step S5 includes at least one low-temperature heat preservation treatment; the temperature of the low-temperature heat preservation treatment is less than or equal to 600 ℃, and the vacuum or nitrogen carrying treatment is performed at the same time.
In some embodiments of the invention, the wet ball milling medium is alcohol or absolute alcohol.
In some embodiments of the present invention, the pressing plates are laid on the upper and lower surfaces of the blank in the step S5 for sintering.
According to the invention, the platen comprises a boron nitride platen.
In some embodiments of the present invention, the step S5 is sintering a single green body or sintering a plurality of green bodies in a stacked manner.
In some embodiments of the present invention, when the multi-piece green body is sintered in the step S5, a spacer powder is laid between the multi-piece green body.
According to the invention, the isolating powder comprises a boron nitride isolating powder.
The invention has the beneficial effects that:
(1) The preparation method provided by the invention realizes one-step compression molding of the large-size ceramic substrate through presetting control of particle sizes of the granulated powder and the particles, special requirements on a die and reasonable selection and compounding of a high polymer molding agent; the forming process is few, the possible damage condition of the blank in the excessive operation process is avoided, the operation is simple and convenient, the cost is low, and the production practical value is realized.
(2) The preparation method provided by the invention effectively eliminates the problem of thin blank cracking caused by elasticity after effect through reasonable optimization and compounding of the forming agent and the regulation and control of powder characteristics such as particle size distribution, sphericity and the like; the problem of uneven cracking of thin blanks is solved by special requirements on parameters such as materials, hardness, parallelism and the like of the die and control of a pressing process.
(3) The preparation method provided by the invention has the advantages that the forming agent is less, the degumming is directly carried out in the low-temperature heat preservation treatment stage in the sintering process, the integrated degumming and sintering is realized, the independent degumming equipment and working procedures are not needed, the charging and discharging are reduced, the independent degumming tail gas treatment system is also not needed, the preparation efficiency is improved, and the product performance is good.
(4) The preparation method provided by the invention directly sinters the particles after the particles are pressed into the green body in the metal mold, has simple and convenient operation and few working procedures, avoids the possible damage condition of the green body in excessive operation procedures, and saves the cost.
(5) The preparation method provided by the invention can prepare the large-size ceramic substrate with better performance; the maximum size of the green body can reach 250mm, the minimum thickness can reach 0.3mm, the maximum size of the sintered substrate can reach 200mm, and the minimum thickness can reach 0.25mm.
(6) Compared with tape casting, the preparation method 1) provided by the invention saves energy, has less added forming agent, does not need to independently discharge glue, only needs to add a plurality of heat preservation sections in the sintering process, and the accumulated time of the heat preservation sections is not longer than 5 hours; 2) The labor is saved, the process of discharging glue from the furnace is omitted, and the efficiency is improved; 3) The material resources are saved, a special tail gas treatment device is not needed to be additionally arranged, and the requirements can be met by a wax collecting tank of the sintering furnace; 4) The environment-friendly type molding agent is environment-friendly, various toxic and strongly pungent organic solvents are not required to be used and discharged, and the required discharged molding agent is reduced by one order of magnitude.
(7) Compared with a two-step pressing method of dry pressing and cold isostatic pressing, the preparation method provided by the invention can be molded by one-step compression molding without cold isostatic pressing, 1) the efficiency is high, and the processes of steel plate clamping, film layer packaging, cold isostatic pressing and batch sheet unsealing are saved; 2) The equipment cost is saved, and a cold isostatic press is not required to be purchased; 3) The reliability is high, and the possible damage of the blank sheet in the operation is avoided because of no packaging, cold isostatic pressing and unpacking processes.
Detailed Description
In order that the invention may be more readily understood, the invention will be described in detail below with reference to the following examples, which are given by way of illustration only and are not limiting of the scope of application of the invention.
The invention provides a preparation method of a large-size ceramic substrate, which can realize one-step press molding of the large-size ceramic substrate; the forming process is few, the possible damage condition of the blank in the excessive operation process is avoided, the operation is simple and convenient, the cost is low, and the production practical value is realized.
Example 1
The embodiment provides a preparation method of a large-size ceramic substrate, which specifically comprises the following steps:
S1: mixing 94 wt percent of alpha-Si 3N4 powder with 4 wt percent of Y 2O3 and 2 wt percent of MgO by wet ball milling with alcohol as a ball milling medium to form mixed slurry; 1.2 wt% binder (polyvinyl butyral), 0.8 wt% dispersant (castor oil phosphate), 2 wt% plasticizer (dioctyl phthalate); wherein the average particle size of the Si 3N4 powder, the Y 2O3 powder and the MgO powder is 0.5-0.8 mu m;
S2: the mixed slurry prepared in the step S1 is passed through a pressure type atomization drying tower to obtain nearly spherical particles with the average particle diameter of 80 mu m;
S3: uniformly spreading the nearly spherical particle powder prepared in the step S2 in a 180 mm multiplied by 250 mm metal mold, wherein the working surface of the metal mold is made of Cr12MoV mold steel, the hardness is HRC60, the roughness is 0.1, the upper and lower surface parallelism is 0.02, and the loading height is 0.78 and mm;
S4: the upper punch of the press (made of Cr12MoV die steel) is pressed down to have loading pressure, when the loading pressure is 10 MPa, the pressure is maintained for 5s, when the loading pressure is 120 MPa, the pressure is maintained for 15s, when the pressure is released to 2 MPa, the pressure is maintained for 10 s, the pressure is released slowly, and the thickness of a blank is 0.3 mm;
s5: placing the blank body obtained in the step S4 on a boron nitride pressing plate paved with boron nitride isolation powder, spreading the boron nitride isolation powder among the blank bodies, superposing 5 blank bodies on one boron nitride pressing plate, paving the boron nitride pressing plate on the uppermost blank body, placing the blank body in an air pressure sintering furnace, vacuumizing at the temperature of 600 ℃, keeping the temperature at 300 ℃ and 600 ℃ for 1h, removing the added polymer forming agent, heating to 1900 ℃, keeping the air pressure at 2MPa, keeping the temperature for 6h, and cooling to 1400 ℃ under the controlled temperature.
S6: and removing the boron nitride isolating powder on the surface of the sintered sheet by using an ultrasonic mode to obtain the large-size ceramic substrate.
Example 2
The embodiment provides a preparation method of a large-size ceramic substrate, which specifically comprises the following steps:
S1: mixing 95 wt percent of AlN powder with 4.5 wt percent of Y 2O3 and 0.5 wt percent of CaF 2 by wet ball milling with absolute ethyl alcohol as a ball milling medium to form mixed slurry; 1 wt% binder (polyvinyl butyral), 0.5% wt% dispersant (glycerol trioleate), 1% wt% plasticizer (phthalate); wherein the average particle size of AlN powder, caF 2 powder and Y 2O3 powder is 0.4-1 μm;
s2: the mixed slurry prepared in the step S1 is passed through a centrifugal atomization drying tower to obtain nearly spherical particles with the average particle diameter of 100 mu m;
S3: uniformly spreading the nearly spherical particle powder prepared in the step S2 in a metal mold of 130 mm multiplied by 130 mm, wherein the working surface of the metal mold is made of hard alloy, the hardness HRA92, the roughness 0.2, the upper and lower surface parallelism 0.02 and the loading height 1.1 mm;
S4: the upper punch (made of hard alloy) of the press is pressed down to load pressure, the pressure is maintained for 5s when the load pressure is 20MPa, the pressure is maintained for 5s when the load pressure is 150 MPa, the pressure is maintained for 10 s when the pressure is released to 3 MPa, the pressure is released slowly, and the thickness of a blank is pressed to be 0.5mm;
S5: uniformly coating a layer of boron nitride isolation powder on the surface of the green body prepared in the step S4, flatly stacking 8 green bodies between two high-purity boron nitride pressing plates, and placing the green bodies in a normal-pressure sintering furnace for sintering; vacuumizing before 600 ℃ and preserving heat for 1h at 300 ℃ and 600 ℃ to remove the added polymer forming agent, heating to 1880 ℃ and preserving heat for 5h.
S6: and removing the boron nitride isolating powder on the surface of the sintered thin plate by means of sand blasting, ultrasonic and the like to obtain the large-size ceramic substrate.
Example 3
S1: mixing 95 wt percent of alpha-Si 3N4 powder with 3 wt percent of Y 2O3 and 2wt percent of MgO, and uniformly mixing by wet ball milling with alcohol as a ball milling medium to form mixed slurry; 2wt.% of binder (polyethylene glycol), 1wt.% of dispersant (fish oil), 1wt.% of plasticizer (dibutyl phthalate) are added; wherein the average particle size of the Si 3N4 powder, the Y 2O3 powder and the MgO powder is 0.5-1 mu m;
S2: the mixed slurry prepared in the step S1 is passed through a pressure type atomization drying tower to obtain nearly spherical particles with the average particle diameter of 120 mu m;
S3: uniformly spreading the nearly spherical particle powder prepared in the step S2 in a 180mm multiplied by 250 mm metal mold, wherein the working surface of the metal mold is made of Cr12MoV mold steel, the hardness is HRC60, the roughness is 0.1, the upper and lower surface parallelism is 0.02, and the loading height is 2 mm;
S4: the upper punch of the press (made of Cr12MoV die steel) is pressed down to have loading pressure, when the loading pressure is 4 MPa, the pressure is maintained at 15 s, when the loading pressure is 150 MPa, the pressure is maintained for 8s, when the pressure is released to 2 MPa, the pressure is maintained at 10s, the pressure is released slowly, and the thickness of a blank is pressed to be 0.8mm;
S5: placing the blank body obtained in the step S4 on a boron nitride pressing plate paved with boron nitride isolation powder, paving the boron nitride isolation powder among the blank bodies, superposing 7 blank bodies on one boron nitride pressing plate, paving the boron nitride pressing plate on the uppermost blank body, placing an air inlet pressure sintering furnace, vacuumizing before 300 ℃, carrying nitrogen at 300-600 ℃, keeping the temperature for 1h at 350 ℃ and 600 ℃ to remove the added macromolecule forming agent, heating to 1880 ℃, keeping the pressure for 4h at 6MPa, and cooling to 1400 ℃ under controlled temperature.
S6: and removing the boron nitride isolating powder on the surface of the sintered sheet by using an ultrasonic mode to obtain the large-size ceramic substrate.
Example 4
The embodiment provides a preparation method of a large-size ceramic substrate, which specifically comprises the following steps:
S1: 93wt.% of AlN powder and 7 wt wt.% of Y 2O3 are subjected to wet ball milling and uniformly mixed by taking absolute ethyl alcohol as a ball milling medium to form mixed slurry; 1 wt% of a binder (polyvinyl acetate), 0.5% wt% of a dispersant (fish oil), 1% wt% of a plasticizer (dibutyl phthalate); wherein the average particle size of AlN powder and Y 2O3 powder is 0.3-0.8 μm;
S2: the mixed slurry obtained in the step S1 is passed through a centrifugal atomization drying tower to obtain nearly spherical particles with the average particle diameter of 40 mu m;
S3: uniformly spreading the nearly spherical particle powder prepared in the step S2 in a metal mold with the thickness of 130 mm multiplied by 130 mm, wherein the working surface of the metal mold is made of hard alloy, the hardness HRA92, the roughness 0.2, the upper and lower surface parallelism 0.02 and the loading height 2 mm;
S4: the upper punch (made of hard alloy) of the press is pressed down to have loading pressure, when the loading pressure is 6 MPa, the pressure is maintained at 10 s, when the loading pressure is 120 MPa, the pressure is maintained at 10 s, when the pressure is released to 3 MPa, the pressure is maintained at 10 s, the pressure is released slowly, and the thickness of a blank body is formed by pressing is 1.1mm;
S5: uniformly coating a layer of boron nitride isolation powder on the surface of the green body prepared in the step S4, flatly stacking 6 green bodies between two high-purity boron nitride pressing plates, and placing the green bodies in a normal-pressure sintering furnace for sintering; vacuum pumping is carried out before 300 ℃, nitrogen carrier belt is carried at 300-600 ℃, heat preservation is carried out for 1h at 300 ℃ and 600 ℃, added polymer forming agent is removed, temperature is raised to 1850 ℃, and heat preservation is carried out for 3h.
S6: and removing the boron nitride isolating powder on the surface of the sintered thin plate by means of sand blasting, ultrasonic and the like to obtain the large-size ceramic substrate.
Performance tests were performed on the large-sized ceramic substrates prepared in examples 1 to 4. The test results are shown in Table 1.
TABLE 1 Large size ceramic substrate Performance
As can be seen from Table 1, the large-size ceramic substrate prepared by the method provided by the invention can achieve a thinner thickness, and has better strength, thermal conductivity and fracture toughness.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (3)
1. The preparation method of the large-size ceramic substrate is characterized by comprising the steps of: mixing ceramic powder with preset average particle size, sintering aid with preset average particle size and polymer forming agent to obtain mixed raw material, preparing particles with preset average particle size, uniformly paving the prepared particles in a metal mold with preset conditions, pressing to obtain a green body, and directly sintering;
And/or the preset average particle size of the ceramic powder and the sintering aid is less than or equal to 1 mu m, the Rockwell hardness of the working surface of the metal mold is more than or equal to 60, the roughness of the working surface is less than or equal to 0.2, and the parallelism of the working surface is less than or equal to 0.02;
the metal mold is made of Cr12MoV mold steel or hard alloy;
The addition amount of the polymer forming agent is less than or equal to 5wt.% of the total amount of the mixed raw materials;
And/or the polymer forming agent comprises a binder, a dispersing agent and a plasticizer; the addition amount of the binder is less than or equal to 2wt.% of the total amount of the mixed raw materials, the addition amount of the dispersing agent is less than or equal to 1wt.% of the total amount of the mixed raw materials, and the addition amount of the plasticizer is less than or equal to 2wt.% of the total amount of the mixed raw materials;
the binder comprises at least one of polyvinyl butyral, polyvinyl acetate and polyethylene glycol;
and/or the dispersant comprises at least one of triolein, fish oil and castor oil phosphate;
And/or the plasticizer comprises at least one of phthalate, dibutyl phthalate, and dioctyl phthalate;
The preparation method comprises the following specific steps:
S1: mixing ceramic powder, sintering aid and polymer forming agent to obtain mixed raw material, and uniformly ball-milling by wet method to obtain mixed slurry;
S2: centrifuging or pressurizing the mixed slurry prepared in the step S1, atomizing and drying to obtain nearly spherical particles with the average particle diameter of 40-120 mu m;
s3: uniformly paving the nearly spherical particles prepared in the step S2 in a metal mold; calculating to obtain the loading height of the metal mold through the preset blank thickness and the compression ratio of the particles;
S4: and carrying out gradient pressurizing and pressing on the nearly spherical particles paved in the metal mold on a press to form a blank, wherein the conditions of the gradient pressurizing and pressing are as follows: the pressure is less than or equal to 20 MPa to 15s, and the pressure is 80 to 150 to MPa for 5 to 10s; then slowly releasing pressure;
s5: sintering the blank body prepared in the step S4 at 1850-1950 ℃ for more than or equal to 3 hours;
the sintering process of the green body in the step S5 comprises at least one section of low-temperature heat preservation treatment; the temperature of the low-temperature heat preservation treatment is less than or equal to 600 ℃;
And/or, paving pressing plates on the upper surface and the lower surface of the blank in the step S5 for sintering.
2. The method of manufacturing according to claim 1, wherein the charge height of the metal mold is calculated by a preset green body thickness and a compression ratio of the pellets.
3. The method according to claim 2, wherein the calculation formula of the charge height of the metal mold is shown in formula (1),
H stock = h blank/sigma compression ratio (1)
Wherein, h is the charge height of the metal mould, h blank-preset blank thickness, sigma compression ratio-compression ratio of particles.
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