CN114085084A - High-strength silicon nitride ceramic and preparation method thereof - Google Patents
High-strength silicon nitride ceramic and preparation method thereof Download PDFInfo
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- CN114085084A CN114085084A CN202010866098.4A CN202010866098A CN114085084A CN 114085084 A CN114085084 A CN 114085084A CN 202010866098 A CN202010866098 A CN 202010866098A CN 114085084 A CN114085084 A CN 114085084A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 92
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 92
- 238000005245 sintering Methods 0.000 claims abstract description 52
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005238 degreasing Methods 0.000 claims abstract description 26
- 238000005469 granulation Methods 0.000 claims abstract description 26
- 230000003179 granulation Effects 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000007921 spray Substances 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 11
- 238000005452 bending Methods 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 6
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 2
- 238000000110 selective laser sintering Methods 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 13
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- 238000010146 3D printing Methods 0.000 abstract description 6
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- 239000003921 oil Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 238000005475 siliconizing Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 238000003825 pressing Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 230000007123 defense Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 102000020897 Formins Human genes 0.000 description 1
- 108091022623 Formins Proteins 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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Abstract
The invention discloses a high-strength silicon nitride ceramic and a preparation method thereof. The method comprises the steps of carrying out spray granulation on silicon nitride powder and a sintering aid, mixing resin powder and curing agent powder, preparing a ceramic blank by SLS (selective laser sintering) in 3D printing, and treating the ceramic blank by twice cold isostatic pressing technology, so that the porosity in the ceramic blank is reduced, and the density of the ceramic blank is improved; before cold isostatic pressing, a rubber sleeve is sleeved on the ceramic blank, and the rubber sleeve can prevent water or oil from entering the surface of the blank in the cold isostatic pressing process; after cold isostatic pressing, the ceramic blank particles are arranged more closely, and the density is improved; the mechanical property of the test piece is improved; the resin in the ceramic body can be removed by degreasing; finally, removing a small amount of silicon on the surface of the member after siliconizing through physical polishing or chemical corrosion, and improving the dimensional precision of the test piece; the steps are simple and easy to realize.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of silicon nitride ceramic preparation, and particularly relates to a high-strength silicon nitride ceramic and a preparation method thereof.
[ background of the invention ]
Silicon nitride (Si)3N4) The silicon nitride ceramic has the advantages of high strength, high hardness, high thermal shock resistance, high temperature resistance, low density, oxidation resistance, stable performance in a high temperature state and the like, has low dielectric constant and loss tangent value, and is one of the ceramic materials with the most application potential in aerospace parts. The ceramic matrix composite has high hardness, belongs to anisotropic materials, is difficult to form and process, meets great obstacles in certain key parts with complex shapes and precise sizes used in high and new technical fields of machinery, automobiles, aerospace, national defense military industry and the like at present, and particularly in the field of national defense military manufacturing, the manufacturing technology of carbide and nitride ceramics with high quality and complex structures and composite material parts thereof becomes an important research subject influencing the development of the carbide and nitride ceramics. Therefore, the 'material preparation' and 'part manufacturing' of the ceramic matrix composite material need to be finished uniformly to improve the finished product rate of parts, and the exploration of the integrated manufacturing method of the precise complex ceramic matrix composite material parts has important application prospects and urgent requirements in the development of the national defense industry.
With the development of industry, the traditional process can not meet the requirements of high-tech products. The 3D printing rapid prototyping technology is a novel prototyping technology which is rapidly developed in recent years, and the technology can be applied to the main selective laser sintering technology (SLS) and the three-dimensional light curing prototyping (SLA) technology in ceramic prototyping at present. The SLA technology has longer material preparation period, and the silicon nitride paste is unstable and easy to agglomerate and harden, and meanwhile, the SLA technology takes longer time than the SLS technology. Two main problems of the silicon nitride ceramic prepared by the SLS process at present are that firstly, silicon nitride powder is extremely easy to agglomerate, powder is not easy to spread in the SLS process, and the ligand strength is low after the second forming, so that the later degreasing and sintering are not easy to realize.
Patent No. CN110330344A discloses a patent for preparing high-porosity silicon nitride ceramic based on selective laser sintering, wherein hollow silicon nitride spheres and sintering aids are uniformly mixed, so that the obtained silicon nitride has very low strength, and even the formed shape can not be maintained after degreasing.
[ summary of the invention ]
The present invention aims to overcome the disadvantages of the prior art and provide a high-strength silicon nitride ceramic and a preparation method thereof; the method is used for solving the technical problems that silicon nitride powder is easy to agglomerate, is difficult to spread in an SLS process, is low in ligand strength after molding and is not beneficial to degreasing and sintering in the later period in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of high-strength silicon nitride ceramics comprises the following steps:
step 1, uniformly mixing initial silicon nitride powder and a sintering aid, and then performing spray granulation to obtain granulated silicon nitride powder, wherein the grain diameter of the granulated silicon nitride powder is 20-100um, and the flowability is 50-100S/50 g;
step 4, carrying out primary cold isostatic pressing treatment on the ceramic blank, wherein the cold isostatic pressing pressure is 110-200 Mpa;
step 5, carrying out degreasing treatment on the ceramic component subjected to the first cold isostatic pressing to obtain a degreased ceramic component;
step 6, carrying out secondary cold isostatic pressing treatment on the degreased ceramic component, wherein the cold isostatic pressing strength is 180-300 Mpa;
and 7, sintering the ceramic component obtained by the secondary cold isostatic pressing to obtain the high-strength silicon nitride ceramic.
The invention is further improved in that:
preferably, in step 1, the sintering aid comprises yttrium oxide and aluminum oxide, and the mass fractions of the initial silicon nitride powder, yttrium oxide and aluminum oxide after mixing are 87% -92%, 3% -8% and 1% -5%, respectively.
Preferably, in step 1, the particle sizes of the silicon nitride, the yttrium oxide and the aluminum oxide are all 0.3um-10 um.
Preferably, in the step 2, the adding amount of the resin powder is 5-20% of the mass of the silicon nitride powder after mixing and granulation; the addition amount of the curing agent is 5-20% of the mass of the silicon nitride powder after mixing and granulation.
Preferably, in step 2, the resin powder is epoxy resin or phenolic resin.
Preferably, in step 5 and step 7, the component to be treated is subjected to sheath treatment before two times of cold isostatic pressing, and air in the sheath is pumped and adjusted.
Preferably, in the step 5, the degreasing temperature is 600-1160 ℃, and the degreasing time is 50-160 min.
Preferably, in the step 7, the sintering time is 90-180 min, and the sintering temperature is 1600-1800 ℃.
Preferably, the sintering atmosphere is nitrogen, and the nitrogen pressure is 1.5-4 MPa.
The high-strength silicon nitride ceramic prepared by the preparation method has the density of 2.42-2.93 g/cm3The bending strength is 455-728 MPa.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of high-strength silicon nitride ceramic. The method comprises the steps of carrying out spray granulation on silicon nitride powder and a sintering aid, mixing resin powder and curing agent powder, preparing a ceramic blank by SLS (selective laser sintering) in 3D printing, and treating the ceramic blank by a twice Cold Isostatic Pressing (CIP) technology, so that the porosity in the ceramic blank is reduced, and the density of the ceramic blank is improved; before cold isostatic pressing, a rubber sleeve is sleeved on the ceramic blank, and the rubber sleeve can prevent water or oil from entering the surface of the blank in the cold isostatic pressing process; the first cold isostatic pressing can improve the strength of the blank body before rubber discharging, and cracking and even structural collapse caused in the rubber discharging process are avoided; the secondary cold isostatic pressing can reduce newly generated pores after rubber discharge, improve the density and the strength, greatly improve the density and the strength through the twice cold isostatic pressing, ensure that the ceramic blank particles are more closely arranged after the cold isostatic pressing, improve the density and improve the mechanical property of a test piece; the resin in the ceramic body can be removed by degreasing; finally, the silicon nitride ceramic is densified through air pressure sintering, the strength and the density are further improved, and the method is simple in step and easy to implement. According to the method, the mixed silicon nitride powder and the sintering aid are prepared into the granulated spherical silicon nitride powder through spray granulation for the first time, the spherical silicon nitride powder is good in fluidity, so that the spherical silicon nitride powder is good in fluidity when applied to an SLS technology and easy to spread, and the problems that the SLS technology is easy to agglomerate and sticky powder is not easy to spread when silicon nitride powder is printed are solved.
The invention also discloses a high-strength silicon nitride ceramic, wherein the bending strength of the high-strength silicon nitride ceramic prepared by SLS at present is less than 100MPa, and the bending strength of the high-strength silicon nitride ceramic is partially even less than 50 MPa; the density of the high-strength silicon nitride ceramic is 2.42-2.93 g/cm3The bending strength is 455-728 Mpa, and the strength performance of the silicon nitride ceramic is greatly improved.
[ description of the drawings ]
FIG. 1 is a microscopic morphology of silicon nitride and a sintering aid after spray granulation in example 1 of the present invention;
FIG. 2 shows the micro-morphology of the pattern after two cold isostatic pressing sinterings after the SLS process of example 1 of the present invention;
FIG. 3 is a microstructure of comparative example 1 of the present invention, i.e., the pattern after SLS processing and without isostatic cool pressing sintering;
FIG. 4 is a density chart of samples prepared in comparative example 1, comparative example 2 and example 1 of the present invention;
FIG. 5 is a graph showing the flexural strength of the test pieces prepared in comparative example 1, comparative example 2 and example 1 according to the present invention;
[ detailed description ] embodiments
The invention is described in further detail below with reference to the following figures and specific examples:
the invention discloses a high-strength silicon nitride ceramic and a preparation method thereof, and the preparation method comprises the following steps:
s1, uniformly mixing the initial silicon nitride powder and the sintering aid, and then performing spray granulation; the primary particle size of the silicon nitride powder is 0.3-10 um, and the mass fraction is 87-92%; the sintering aid is yttrium oxide and aluminum oxide, the particle size is 0.3-10 um, and the mass fractions are 3-8% and 1-5% respectively; the particle size of the silicon nitride powder obtained after spray granulation is 20-100um, and the fluidity is 50-100S/50 g. If the particle diameter of the silicon nitride powder after spray granulation is outside the range, the performance is not good.
S2, mixing the silicon nitride powder, the resin powder and the curing agent after spray granulation by a mixer; the resin powder comprises epoxy resin or phenolic resin which is used as a binder, and the content of the epoxy resin or phenolic resin is 5-20% of the mass fraction of the silicon nitride powder; the curing agent is an epoxy resin curing agent, and the content of the curing agent is 5-20% of the resin;
s3, carrying out layered slicing processing on the STL format file through magics software to obtain the layered thickness and the layer number, exporting the layered thickness and the layer number as an SLC file, and importing the SLC format file into a 3D printer; the thickness of each layer is 0.05-0.15 mm;
s4, adding the uniformly mixed ceramic powder obtained in the step S2 into a charging barrel of a 3D printer, paving the powder, heating a working box of the 3D printer to the temperature of 30-70 ℃, and printing layer by layer from bottom to top by a laser head of the 3D printer according to the layering data obtained in the step S2 at the temperature to obtain a ceramic body; the laser power is 15-35W, and the scanning speed is 2000-4000 mm/s; obtaining a ceramic body.
S5, taking the ceramic blank out of the 3D printing work box, placing for 20-50min at room temperature, and removing redundant powder;
s6, performing sheath treatment on the ceramic blank, pumping air in the sheath, and covering the sheath with a bagPutting the sheathed ceramic blank into a cold isostatic press for carrying out first cold isostatic pressing treatment to reduce the porosity and obtain a cold isostatic pressed component; the first cold isostatic pressing pressure is 110-200 MPa, the time is 3-5min, the strength after the first cold isostatic pressing reaches 177-305MPa, and the density reaches 1.88-2.13g cm3。
S7, placing the cold isostatic pressed component into a vacuum high-temperature furnace for degreasing to remove resin in the ceramic blank, wherein the degreasing temperature is 600-1160 ℃, and the degreasing time is 50-160 min;
and S8, carrying out cold isostatic pressing on the degreased silicon nitride ceramic again, wherein the pressure is 180-300 MPa, and the time is 3-5min, and because the density of the blank in the first cold isostatic pressing process is very high, the pressure in the second cold isostatic pressing process needs to be higher than that in the first cold isostatic pressing process, so that the density and the strength are further increased.
The first cold isostatic pressing is used for improving the strength of the blank before rubber discharge and avoiding cracking and even structural collapse caused in the rubber discharge process. The secondary cold isostatic pressing is used for reducing newly generated pores after rubber is discharged and improving the density and the strength.
S9, directly putting the silicon nitride ceramic piece subjected to secondary cold isostatic pressing into a sintering furnace for sintering, wherein the air pressure sintering time is 90-180 min, the sintering temperature is 1600-1800 ℃, the sintering atmosphere is nitrogen, and the nitrogen pressure is 1.5-4 MPa.
The density of the silicon nitride ceramic part prepared by the method is 2.42-2.93 g/cm3The bending strength is 455-728 MPa.
Comparative example 1
Step 1: taking 91%, 6% and 3% of the total mass of silicon nitride powder, yttrium oxide powder and aluminum oxide powder with the particle size of 0.5um respectively, and carrying out spray drying granulation on the silicon nitride powder, the yttrium oxide powder and the aluminum oxide powder together, wherein the particle size after granulation is 20-70 um. The micro-topography is shown in figure 1. FIG. 1 is a microscopic morphology of silicon nitride powder after spray granulation, from which it can be seen that the sphericity is better and the particle size is 20-70 um.
Step 2: taking epoxy resin powder with the particle size of 75um, wherein the mass of the epoxy resin powder is 13 percent of the mass fraction of the granulated silicon nitride mixed powder, and taking epoxy resin curing agent with the particle size of 50um, wherein the mass fraction of the epoxy resin curing agent is 10 percent of the mass of the epoxy resin powder. And mixing the silicon nitride powder, the resin powder and the curing agent after spray granulation by a mixer.
And step 3: and (3) carrying out layered slicing processing on the STL format file through magics software to obtain the layered thickness and the layer number, exporting the layered thickness and the layer number as an SLC file, and importing the SLC format file into a 3D printer.
Step 4, adding the uniformly mixed ceramic powder obtained in the step 2 into a charging barrel of a 3D printer, paving the powder, heating a working box of the 3D printer to the temperature of 30-70 ℃, and printing layer by layer from bottom to top by a laser head of the 3D printer according to the layered data obtained in the step S2 at the temperature to obtain a ceramic blank; the laser power is 32W, and the scanning speed is 2800 mm/s; the layering thickness is 0.08mm, and a ceramic body is obtained.
And 5: placing the component subjected to cold isostatic pressing into a vacuum high-temperature furnace for degreasing to remove resin in the ceramic blank, wherein the degreasing temperature is 600-1160 ℃, and the degreasing time is 50-160 min;
and 6, directly putting the degreased silicon nitride ceramic into a sintering furnace for sintering, wherein the air pressure sintering time is 120min, the sintering temperature is 1700 ℃, the sintering atmosphere is nitrogen, and the nitrogen pressure is 2.5 MPa.
Comparative example 2
Step 1: taking 91%, 6% and 3% of the total mass of silicon nitride powder, yttrium oxide powder and aluminum oxide powder with the particle size of 0.5um respectively, and carrying out spray drying granulation on the silicon nitride powder, the yttrium oxide powder and the aluminum oxide powder together, wherein the particle size after granulation is 20-70 um. The micro-topography is shown in figure 1. FIG. 1 is a microscopic morphology of silicon nitride powder after spray granulation, from which it can be seen that the sphericity is better and the particle size is 20-70 um.
Step 2: taking epoxy resin powder with the particle size of 75um, wherein the mass of the epoxy resin powder is 13 percent of the mass fraction of the granulated silicon nitride mixed powder, and taking epoxy resin curing agent with the particle size of 50um, wherein the mass fraction of the epoxy resin curing agent is 10 percent of the mass of the epoxy resin powder. And mixing the silicon nitride powder, the resin powder and the curing agent after spray granulation by a mixer.
And step 3: and (3) carrying out layered slicing processing on the STL format file through magics software to obtain the layered thickness and the layer number, exporting the layered thickness and the layer number as an SLC file, and importing the SLC format file into a 3D printer.
Step 4, adding the uniformly mixed ceramic powder obtained in the step 2 into a charging barrel of a 3D printer, paving the powder, heating a working box of the 3D printer to the temperature of 30-70 ℃, and printing layer by layer from bottom to top by a laser head of the 3D printer according to the layered data obtained in the step S2 at the temperature to obtain a ceramic blank; the laser power is 32W, and the scanning speed is 2800 mm/s; the layering thickness is 0.08mm, and a ceramic body is obtained.
Step 5, taking the ceramic blank out of a 3D printing work box, placing for 40min at room temperature, and removing redundant powder; and (3) performing sheath treatment on the ceramic blank, pumping out air in the sheath, and putting the ceramic blank sheathed with the sheath into a cold isostatic press for cold isostatic pressing treatment, wherein the cold isostatic pressure is 140MPa, and the pressure maintaining time is 3 minutes, so as to obtain the cold isostatic pressed component.
Step 6, placing the component subjected to cold isostatic pressing into a vacuum high-temperature furnace for degreasing to remove resin in the ceramic blank, wherein the degreasing temperature is 600-1160 ℃, and the degreasing time is 50-160 min;
and 7, directly putting the silicon nitride ceramic piece subjected to the primary cold isostatic pressing degreasing into a sintering furnace for sintering, wherein the air pressure sintering time is 120min, the sintering temperature is 1700 ℃, the sintering atmosphere is nitrogen, and the nitrogen pressure is 2.5 MPa.
Example 1
Step 1: taking 91%, 6% and 3% of the total mass of silicon nitride powder, yttrium oxide powder and aluminum oxide powder with the particle size of 0.5um respectively, and carrying out spray drying granulation on the silicon nitride powder, the yttrium oxide powder and the aluminum oxide powder together, wherein the particle size after granulation is 20-70 um. The micro-topography is shown in figure 1. FIG. 1 is a microscopic morphology of silicon nitride powder after spray granulation, from which it can be seen that the sphericity is better and the particle size is 20-70 um.
Step 2: taking epoxy resin powder with the particle size of 75um, wherein the mass of the epoxy resin powder is 13 percent of the mass fraction of the granulated silicon nitride mixed powder, and taking epoxy resin curing agent with the particle size of 50um, wherein the mass fraction of the epoxy resin curing agent is 10 percent of the mass of the epoxy resin powder. And mixing the silicon nitride powder, the resin powder and the curing agent after spray granulation by a mixer.
And step 3: and (3) carrying out layered slicing processing on the STL format file through magics software to obtain the layered thickness and the layer number, exporting the layered thickness and the layer number as an SLC file, and importing the SLC format file into a 3D printer.
Step 4, adding the uniformly mixed ceramic powder obtained in the step 2 into a charging barrel of a 3D printer, paving the powder, heating a working box of the 3D printer to the temperature of 30-70 ℃, and printing layer by layer from bottom to top by a laser head of the 3D printer according to the layered data obtained in the step S2 at the temperature to obtain a ceramic blank; the laser power is 32W, and the scanning speed is 2800 mm/s; the layering thickness is 0.08mm, and a ceramic body is obtained.
Step 5, taking the ceramic blank out of a 3D printing work box, placing for 40min at room temperature, and removing redundant powder; and (3) performing sheath treatment on the ceramic blank, pumping air in the sheath, putting the ceramic blank sheathed with the sheath into a cold isostatic press for performing primary cold isostatic pressing treatment, wherein the pressure of the primary cold isostatic press is 140MPa, and the pressure maintaining time is 3 minutes, so as to obtain the component subjected to cold isostatic pressing.
And 6, putting the member subjected to the primary cold isostatic pressing into a vacuum high-temperature furnace for degreasing to remove resin in the ceramic blank, wherein the degreasing temperature is 700 ℃, and the degreasing time is 120 min.
And 7, carrying out cold isostatic pressing on the degreased silicon nitride ceramic again, wherein the pressure is 220MPa, and the pressure maintaining time is 5 minutes.
And 8, directly putting the silicon nitride ceramic piece subjected to secondary cold isostatic pressing into a sintering furnace for sintering, wherein the air pressure sintering time is 120min, the sintering temperature is 1700 ℃, the sintering atmosphere is nitrogen, and the nitrogen pressure is 2.5 MPa.
The final density was 2.68g/cm3The strength of the silicon nitride ceramic sample was 585 MPa.
FIG. 2 shows the micro-morphology of the sample after two cold isostatic pressing sinterings after the SLS process; fig. 3 shows the micro-morphology of comparative example 1, and it can be seen that the sample prepared by the present example has higher density.
Referring to FIG. 4, density values of final samples prepared in comparative example 1, comparative example 2 and the present example are shown in FIG. 4Comparative example 1 SLS silicon nitride without isostatic cool pressing and after sintering, the density was 1.2g/cm3Comparative example 2 after primary cold isostatic pressing sintering, the density was 1.921.2g/cm3In this embodiment, the density of the product can reach 2.671.2g/cm after two times of cold isostatic pressing3。
As can be seen from FIG. 5, the bending strength of the SLS silicon nitride without isostatic cool pressing in comparative example 1 after sintering is 12MPa, the strength of comparative example 2 after one isostatic cool pressing sintering is 262MPa, and the strength of the SLS silicon nitride without isostatic cool pressing in this example can reach 683MPa after two isostatic cool pressing. It can be seen from the density and strength results of fig. 4 and 5 that a substantial increase occurs after the secondary cold isostatic pressing.
See tables 1 and 2 below for details of example 2-example 15.
Table 1 examples 2-6
| Number of examples | 2 | 3 | 4 | 5 | 6 |
| Mass fraction of silicon nitride% | 87 | 92 | 90 | 87 | 88 |
| Yttria，％ | 8 | 5 | 7 | 8 | 8 |
| Aluminum oxide,% of | 5 | 3 | 3 | 5 | 4 |
| Particle diameter um of granulated silicon nitride | 30 | 100 | 40 | 60 | 50 |
| Resin powder type | Epoxy resin | Phenolic resin | Epoxy resin | Phenolic resin | Epoxy resin |
| The content of resin powder% | 10 | 8 | 12 | 15 | 5 |
| Content of curing agent% | 10 | 8 | 12 | 15 | 5 |
| Layer thickness, mm | 0.05 | 0.15 | 0.1 | 0.06 | 0.07 |
| Heating temperature of | 50 | 70 | 30 | 40 | 60 |
| Laser power, W | 35 | 15 | 20 | 16 | 18 |
| Scanning speed, mm/s | 2000 | 4000 | 3000 | 2200 | 2800 |
| Standing at room temperature for min | 20 | 30 | 40 | 50 | 22 |
| First cold isostatic pressing pressure, Mpa | 115 | 200 | 110 | 120 | 130 |
| Degreasing temperature, DEG C | 1000 | 800 | 600 | 1120 | 1100 |
| Degreasing time, min | 60 | 120 | 160 | 50 | 70 |
| Second cold isostatic pressure, Mpa | 180 | 220 | 300 | 200 | 240 |
| Sintering time, min | 100 | 120 | 130 | 140 | 150 |
| Sintering temperature of | 1700 | 1650 | 1620 | 1680 | 1720 |
| Sintering pressure, |
2 | 2.5 | 3 | 3.5 | 4 |
Table 2 examples 7 to 11
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of high-strength silicon nitride ceramics is characterized by comprising the following steps:
step 1, uniformly mixing initial silicon nitride powder and a sintering aid, and then performing spray granulation to obtain granulated silicon nitride powder, wherein the grain diameter of the granulated silicon nitride powder is 20-100um, and the flowability is 50-100S/50 g;
step 2, mixing the granulated silicon nitride powder, resin powder and curing agent to form mixed powder;
step 3, printing the mixed powder into a ceramic blank through SLS;
step 4, carrying out primary cold isostatic pressing treatment on the ceramic blank, wherein the cold isostatic pressing pressure is 110-200 Mpa;
step 5, carrying out degreasing treatment on the ceramic component subjected to the first cold isostatic pressing to obtain a degreased ceramic component;
step 6, carrying out secondary cold isostatic pressing treatment on the degreased ceramic component, wherein the cold isostatic pressing strength is 180-300 Mpa;
and 7, sintering the ceramic component obtained by the secondary cold isostatic pressing to obtain the high-strength silicon nitride ceramic.
2. The method according to claim 1, wherein in step 1, the sintering aid comprises yttria and alumina, and the mass fractions of the initial silicon nitride powder, yttria and alumina after mixing are 87% -92%, 3% -8% and 1% -5%, respectively.
3. The method of claim 2, wherein in step 1, the particle sizes of the silicon nitride, yttrium oxide and aluminum oxide are all 0.3um-10 um.
4. The method for preparing high-strength silicon nitride ceramic according to claim 1, wherein in the step 2, the addition amount of the resin powder is 5-20% of the mass of the silicon nitride powder after mixing and granulation; the addition amount of the curing agent is 5-20% of the mass of the silicon nitride powder after mixing and granulation.
5. The method of claim 1, wherein in step 2, the resin powder is epoxy resin or phenolic resin.
6. The method for preparing a high-strength silicon nitride ceramic according to claim 1, wherein in step 5 and step 7, the member to be treated is jacketed before the cold isostatic pressing for two times, and air in the jacket is pumped and adjusted.
7. The method for preparing high-strength silicon nitride ceramic according to claim 1, wherein in the step 5, the degreasing temperature is 600-1160 ℃ and the degreasing time is 50-160 min.
8. The method for preparing high-strength silicon nitride ceramic according to claim 1, wherein in the step 7, the sintering time is 90-180 min, and the sintering temperature is 1600-1800 ℃.
9. The method of claim 1, wherein the sintering atmosphere is nitrogen, and the pressure of nitrogen is 1.5-4 MPa.
10. A high-strength silicon nitride ceramic obtained by the production method according to any one of claims 1 to 9, wherein the silicon nitride ceramic has a density of 2.42 to 2.93g/cm3The bending strength is 455-728 MPa.
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