CN109796208B - Si3N4Ceramic structural member and method for manufacturing same - Google Patents
Si3N4Ceramic structural member and method for manufacturing same Download PDFInfo
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Abstract
The invention discloses Si3N4A ceramic structural member and a method of making the same; the method prints Si in 3D for the first time3N4When in ceramic, Si powder is used as a raw material, the grain composition of a sintering aid and the Si powder is adjusted, the problems that silicon nitride is easy to agglomerate due to moisture absorption, micron-sized silicon nitride is extremely difficult to sinter and the like are solved, the manufacturing cost and time of a traditional process die are saved, the grain size of the powder of the mixed raw material is limited, the preparation is made for subsequent cold isostatic pressing and reaction sintering, and the sintering aid powder is additionally arranged in the raw material to prepare for subsequent liquid-phase re-sintering; the density of the ceramic structural member prepared by the method is (2.14-2.6) g/cm3The bending strength is (151-300) MPa, and the total shrinkage rate of the ceramic structural part is less than 1% after reaction sintering and liquid phase re-sintering.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of 3D printing, and particularly relates to Si3N4A ceramic structural member and a method of making the same.
[ background of the invention ]
The nitride ceramic material is a material capable of realizing structure-function integration, has excellent performance in the aspects of mechanics, chemistry, electricity, heat and the like, and has excellent mechanical property, high bending strength, excellent oxidation resistance, good corrosion resistance, high abrasion resistance and low friction coefficientThe composite material has the advantage that oxide ceramics and metal ceramics cannot be replaced in the field of heat-resistant and high-temperature-resistant structural materials, and has wide application in industries such as metallurgy, aviation, chemical engineering, ceramics, electronics, machinery, semiconductors and the like. Silicon nitride (Si3N4) is a compound with strong covalent bond, can form a silicon dioxide protective film in air, and has good stability. The silicon nitride material has high hardness (HRA of 91-93), high decomposition temperature, and small thermal expansion coefficient (2.7 × 10-6V (20-1000 ℃)), low thermal conductivity (9.46W/m · K), high strength, little high temperature creep, good oxidation resistance, and is widely used for high temperature resistant components of gas engines, corrosion resistant components in the chemical industry, crucible materials in the semiconductor industry, high temperature bearing materials, dental materials, high speed cutting tools, radomes, support materials for nuclear reactors, spacers, carriers for fissile materials, and the like, and thin silicon nitride films and coatings have been widely studied in the fields of high speed memory devices and optical waveguides.
With the development of the industry, these conventional processes have been unable to meet the demand of high-tech products. The 3D printing rapid forming technology is a novel forming technology which is rapidly developed in recent years, the technology can be mainly applied to Fused Deposition Manufacturing (FDM), selective laser sintering technology (SLS) and three-dimensional light solidification forming (SLA) technology in ceramic forming at present, the application of the technologies is combined with the subsequent sintering technology to greatly shorten the forming period of a ceramic component, the problem that the design size change or adjustment which cannot be overcome by the traditional technology is solved, and a mould needs to be redesigned and manufactured is solved; the manufacturing cost of the die is high, the period is long, and the shape of the prepared product is simple.
Si of current SLS molding3N4The ceramic is mostly made of Si3N4The powder is directly printed and sintered, the preparation cost of raw materials is high, the particle size of the raw material powder is larger, the subsequent liquid phase sintering is not facilitated, and the strength of the powder after printing and sintering is lower; research reports that SLS printing of silicon nitride ceramic powder with smaller particle size can be realized by spray granulation or film coating method, but the SLS printing is not beneficial to the dimensional precision control of subsequent components due to higher resin content and larger shrinkage deformation, and the SLS printing is not beneficial to the dimensional precision control of subsequent components due to sinteringThe compactness is low, so that the prepared structural part has poor mechanical property and lower bending strength, and can not be applied in a high-temperature environment. The main reason for the low density after sintering is Si3N4The powder is degreased after SLS molding, and contains more carbon residue, Si3N4Large shrinkage deformation of the powder, resulting in high internal porosity, and Si3N4The powder has larger grain diameter, which is not beneficial to liquid phase sintering and causes the reduction of mechanical property; although the film coating method can reduce the porosity of the test piece after printing and degreasing, the smaller grain size Si is realized3N4SLS printing of powders, but with longer cycle times and higher costs than dry blending. Therefore, a preparation method is needed for preparing Si with high mechanical property and high density3N4A ceramic structural member.
[ summary of the invention ]
The present invention is directed to overcoming the above-mentioned disadvantages of the prior art and providing Si3N4A ceramic structural member and a method of making the same; according to the invention, silicon nitride is generated by degreasing reaction sintering after Si powder SLS printing, and Cold Isostatic Pressing (CIP) technology is introduced into the process for preparing ceramics, so that the density of the printed component is improved, and meanwhile, a sintering aid is added into the raw materials and liquid phase sintering is carried out after reaction sintering, so that the internal porosity of the final structural component is reduced, and the mechanical property of the structural component is improved.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
si3N4The preparation method of the ceramic structural part comprises the following steps:
step 1, mixing Si powder, sintering aid powder and binder powder to obtain uniformly mixed ceramic powder;
step 2, printing the uniform ceramic powder prepared in the step 1 by an SLS printing method to prepare a ceramic blank;
step 3, the ceramic blank obtained in the step 2 is sleeved with a sheath after being cooled or a protective film is additionally arranged on the surface of the blank; carrying out cold isostatic pressing on the ceramic blank sleeved with the sheath or the protective film, and cooling the test piece after the cold isostatic pressing to obtain the test piece after the cold isostatic pressing;
step 4, degreasing the cold isostatic pressed test piece obtained in the step 3 in a nitrogen environment, and reacting and sintering after degreasing to obtain sintered Si3N4A ceramic test piece;
step 5, sintering Si obtained in step 43N4The ceramic test piece is pressurized and liquid-phase sintered in a nitrogen environment to obtain high-density Si3N4A ceramic structural member.
The invention is further improved in that:
preferably, in the step 2, the slice layering thickness is 0.1mm to 0.3mm in the SLS printing process.
Preferably, in step 2, the mass percentage of the Si powder in the mixed powder is: 65-80 percent of the sintering aid powder, and the sintering aid powder comprises the following components in percentage by mass: 8-20 percent of binder powder and 5-17 percent of binder powder by mass percent.
Preferably, in the step 2, the grain size of the Si powder is 10-200 μm.
Preferably, in step 2, the binder is epoxy resin or phenolic resin, and the particle size of the binder powder is 1-10 μm.
Preferably, in step 2, the sintering aid is any one or a mixture of several of alumina, yttria and silica; the particle size of the sintering aid powder is 1-25 μm.
Preferably, in the step 4, the cold isostatic pressure is 200-300 Mpa, and the test piece is cooled for 10-30 min after the cold isostatic pressure.
Preferably, in the step 5, the degreasing temperature is 600-900 ℃, and the degreasing time is 60-120 min; the reaction sintering time is 30-90 min, and the reaction sintering temperature is 1300-1400 ℃.
Preferably, in the step 6, the temperature of the pressurized liquid phase sintering is 1700-1800 ℃, and the pressure is 0.1-0.2 MPa.
Si prepared by any one of the preparation methods3N4Ceramic structural member of said Si3N4The density of the ceramic structural member is 2.14-2.6g/cm3The bending strength is 151-300 MPa.
Prepared by any one of the preparation methodsSi of (2)3N4Ceramic structural member of said Si3N4The density of the ceramic structural member is 2.14-2.6g/cm3The bending strength is 151-300 MPa.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses Si3N4An indirect SLS preparation method of a ceramic structural member. The method is used for preparing Si for indirect SLS3N4The ceramic structural part overcomes the problems that silicon nitride powder is extremely difficult to sinter in a micron-sized mode due to unique moisture absorption and agglomeration, firstly, Si powder, sintering aid and binder powder are mixed and then a ceramic blank is prepared by an SLS (selective laser sintering) technology in 3D (three-dimensional) printing, and the ceramic blank is treated by a 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 or a protective film is additionally arranged on the surface of the ceramic blank, and the rubber sleeve or the protective film 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 for the first time; resin in the ceramic body can be removed through degreasing, but the porosity of the product is high at the moment, and the aggregate is Si powder; then reacting and sintering under nitrogen atmosphere to ensure that silicon reacts with nitrogen to form Si in the sintering process3N4Silicon powder in the test piece is converted into silicon nitride, so that the generation of the silicon nitride is realized, and the mechanical property of the test piece is improved; then the Si is sintered by liquid phase3N4The density of the test piece is further improved, the porosity of the test piece is reduced, and the mechanical property of the test piece is improved; the method prints Si in 3D for the first time3N4When in ceramic, Si powder is used as one of the raw materials, the grain composition of the sintering aid and the Si powder is adjusted, the powder grain size of the mixed raw material is limited, preparation is made for subsequent cold isostatic pressing and reaction sintering, and the sintering aid powder is additionally arranged in the raw material to prepare for subsequent liquid-phase re-sintering, so that the cost and time for manufacturing a die are saved; the method does not directly print silicon nitride powder as a raw material, so degreasing and receiving caused by SLS printing of silicon nitride by the conventional film coating method can be overcomeLarge shrinkage deformation and difficult liquid phase sintering of the micron silicon nitride after printing; the silicon powder is directly formed by an SLS printer and then is reacted and sintered to generate the silicon nitride member, the steps are simple, the operation is easy, the personalized customization of the silicon nitride ceramic is realized, and the research and development period is shortened.
The invention also discloses Si3N4A ceramic structural member having a density of (2.14-2.6) g/cm3The bending strength is (151) -300 MPa, the total shrinkage rate of the reaction sintering stage and the liquid phase re-sintering stage is less than 1%, the compactness is high, and the mechanical property is good.
[ description of the drawings ]
FIG. 1 is a structural diagram of a printed silicon powder according to the present invention;
FIG. 2 is a schematic view of a sintered structural member according to the present invention;
FIG. 3 shows the final high density Si in the present invention3N4An internal SEM image of the ceramic structural member;
[ detailed description ] embodiments
The present invention is described in further detail below with reference to specific steps; the invention discloses Si3N4A ceramic structural member and a method of making the same; the structural member is Si3N4Ceramic structural member of said Si3N4The density of the ceramic structural member is 2.14-2.6g/cm3The bending strength is 51-300 MPa, and the preparation method specifically comprises the following steps:
s1, constructing a three-dimensional model of the structural part, and converting the three-dimensional model into an STL format file; processing the STL format file by hierarchical slicing through magics software to obtain the hierarchical thickness and the number of layers, wherein the hierarchical thickness is 0.1-0.3 mm, and the number of the hierarchical layers is determined according to the size of an actual ceramic structural part; exporting to an SLC file and importing to a 3D printer;
s2, uniformly mixing Si powder, sintering aid powder and binder powder by a mixer to obtain uniformly mixed ceramic powder; the mass percentage of Si powder in the mixed powder is as follows: 65-80 percent of the sintering aid powder, and the sintering aid powder comprises the following components in percentage by mass: 8-20 percent of binder powder and 5-17 percent of binder powder by mass percent. The binder is epoxy resin or phenolic resin; the particle size of the Si powder is 10-200 mu m, the particle size of the sintering aid powder is 1-25 mu m, and the particle size of the adhesive powder is 1-10 mu m, wherein the sintering aid is any one or a mixture of more of aluminum oxide, yttrium oxide and silicon dioxide, and the sintering aid powder and the adhesive powder are mixed in any proportion when the sintering aid powder, the sintering aid powder and the adhesive powder are mixed; in the step, Si powder is used as one of the raw materials, the grain size and the mass part of the powder of the mixed raw material are limited by adjusting the grain composition of a sintering aid and the Si powder, and preparation is made for subsequent cold isostatic pressing and reaction sintering;
s3, putting the uniform ceramic powder prepared in the step S2 into a working box of a 3D printer, and printing by a laser head to prepare a ceramic blank; the working temperature of the working box is 30-70 ℃, and the working gas is nitrogen atmosphere; the laser power is 16-25W, the scanning speed is 2000-4000 mm/s, and the laser head prints layer by layer from bottom to top according to the layered data obtained in the step 1 in the printing process to obtain a ceramic blank;
s4, cooling the ceramic blank obtained in the step S3, and then sheathing a sheath or additionally arranging a protective film on the surface of the blank; and (3) carrying out cold isostatic pressing treatment on the ceramic blank sleeved with the sheath or the protective film, wherein the pressure intensity of the cold isostatic pressing is 200-300 Mpa, so as to obtain a test piece after the cold isostatic pressing, and cooling the ceramic blank after the cold isostatic pressing at room temperature for 10-30 min, so as to obtain a cooled ceramic blank.
S5, degreasing the test piece obtained in the step S4 at 600-900 ℃ for 60-120 min, then degreasing the test piece in a nitrogen environment, reacting and sintering the test piece, wherein the reaction and sintering time is 30-90 min, the reaction and sintering temperature is 1300-1400 ℃, and Si is obtained after sintering3N4A ceramic test piece.
S6, putting the test piece obtained in the step S5 into an air pressure sintering furnace, pressurizing the test piece in the nitrogen environment, and performing liquid phase sintering at the liquid phase sintering temperature of 1700-1800 ℃ and the pressure of 0.1-0.2MPa to obtain the high-density Si3N4A ceramic structural member.
The density of the ceramic structural part obtained by the steps is 2.14-2.6g/cm3The bending strength is (151-300) MPa, the shrinkage rate after reaction sintering and liquid phase re-sintering is less than 1 percent, and in the preparation process, the ceramic structural part expands during reaction sintering and contracts during liquid phase sintering and mutuallyThe total yield after offset is less than 1%.
Example 1
S1, constructing a three-dimensional model of the structural part, and converting the three-dimensional model into an STL format file; processing the STL format file by hierarchical slicing through magics software to obtain the hierarchical thickness and the layer number, wherein the hierarchical thickness is 0.15 mm; exporting to an SLC file and importing to a 3D printer;
s2, uniformly mixing Si powder, alumina powder and epoxy resin powder by a mixer to obtain uniformly mixed ceramic powder; the mass percentage of Si powder in the mixed powder is as follows: 70 percent, and the mass percentage of the mixed powder of the alumina, the yttrium oxide and the silicon dioxide is as follows: 15% (wherein, 5% of alumina, 3.5% of yttria and 6.5% of silicon dioxide) and 15% of epoxy resin powder.
S3, putting the uniform ceramic powder prepared in the step S2 into a working box of a 3D printer, and printing by a laser head to prepare a ceramic blank; the working temperature of the working box is 50 ℃, and the working gas is nitrogen atmosphere; the laser power is 20W, the scanning speed is 3000mm/s, and the laser head prints layer by layer from bottom to top according to the layered data obtained in the step 1 in the printing process to obtain a ceramic blank;
s4, cooling the ceramic blank obtained in the step S3, and then sheathing a sheath or additionally arranging a protective film on the surface of the blank; and (3) carrying out cold isostatic pressing treatment on the ceramic blank sleeved with the sheath or the protective film, wherein the cold isostatic pressing pressure is 250Mpa, so as to obtain a test piece after cold isostatic pressing, and cooling the ceramic blank after cold isostatic pressing at room temperature for 20min, so as to obtain a cooled ceramic blank.
S5, degreasing the test piece obtained in the step S4 at 800 ℃ for 80min, then degreasing and reacting and sintering the test piece in a nitrogen environment, wherein the reacting and sintering time is 70min, the reacting and sintering temperature is 1400 ℃, and Si is obtained after sintering3N4A ceramic test piece.
S6, putting the test piece obtained in the step S5 into an air pressure sintering furnace, pressurizing the test piece in the nitrogen environment, and performing liquid phase sintering, wherein the liquid phase sintering temperature is 1800 ℃, and the pressure is 0.0.2MPa, so that high-density Si is obtained3N4A ceramic structural member.
Pottery obtained through the stepsA ceramic structural member with a density of 2.6g/cm3The flexural strength was 300 MPa.
Fig. 1 is a photograph of the ceramic blank obtained in step S3 after the silicon powder is printed in the present embodiment; fig. 2 is a photo image of the structural member obtained in the final step S6 in this embodiment, and as can be seen from comparison between fig. 1 and fig. 2, the main aggregate of the printed silicon powder is silicon powder, so that the whole ceramic blank is black, and after the internal chemical reaction in the later sintering stage, silicon nitride and a small amount of silicon oxynitride are generated, so that the whole blank is white and gray.
Fig. 3 is an SEM image of the inside of the final sample, and it can be seen from the SEM image that the inside of the sample is denser after sintering, and the powders are tightly combined together by sintering, but a small amount of pores still exist inside, and these pores can increase the wave permeability of the silicon nitride ceramic, so that the silicon nitride ceramic has better application prospect.
The detailed process parameters of examples 2-5 are detailed in table 2.
Table 2 process parameters of examples 2-5
The process parameters of examples 6-9 are detailed in Table 3.
TABLE 3 Process parameters for examples 6-9
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 (7)
1. Si3N4The preparation method of the ceramic structural member is characterized by comprising the following steps of:
step 1, mixing Si powder, sintering aid powder and binder powder to obtain uniformly mixed ceramic powder;
the mass percentage of Si powder in the mixed powder is as follows: 65-80 percent of the sintering aid powder, and the sintering aid powder comprises the following components in percentage by mass: 8-20% of binder powder, and 5-17% of binder powder by mass;
step 2, printing the uniform ceramic powder prepared in the step 1 by an SLS printing method to prepare a ceramic blank;
step 3, the ceramic blank obtained in the step 2 is sleeved with a sheath after being cooled or a protective film is additionally arranged on the surface of the blank; carrying out cold isostatic pressing on the ceramic blank sleeved with the sheath or the protective film, and cooling the test piece after the cold isostatic pressing to obtain the test piece after the cold isostatic pressing; the cold isostatic pressure is 200-300 Mpa, and the test piece is cooled for 10-30 min after the cold isostatic pressure;
step 4, degreasing the cold isostatic pressed test piece obtained in the step 3 in a nitrogen environment, and reacting and sintering after degreasing to obtain sintered Si3N4A ceramic test piece;
step 5, sintering Si obtained in step 43N4The ceramic test piece is pressurized and liquid-phase sintered in a nitrogen environment to obtain high-density Si3N4A ceramic structural member;
the temperature of the pressurized liquid phase sintering is 1700-1800 ℃, and the pressure is 0.1-0.2 MPa.
2. Si according to claim 13N4The preparation method of the ceramic structural member is characterized in that in the step 2, the slicing layering thickness is 0.1-0.3 mm in the SLS printing process.
3. Si according to claim 13N4Manufacture of ceramic structural membersThe preparation method is characterized in that in the step 1, the grain size of the Si powder is 10-200 mu m.
4. Si according to claim 13N4The preparation method of the ceramic structural member is characterized in that in the step 1, the binder is epoxy resin or phenolic resin, and the particle size of the binder powder is 1-10 microns.
5. Si according to claim 13N4The preparation method of the ceramic structural member is characterized in that in the step 1, the sintering aid is any one or a mixture of more of alumina, yttria or silicon dioxide; the particle size of the sintering aid powder is 1-25 μm.
6. Si according to claim 13N4The preparation method of the ceramic structural member is characterized in that in the step 4, the degreasing temperature is 600-900 ℃, and the degreasing time is 60-120 min; the reaction sintering time is 30-90 min, and the reaction sintering temperature is 1300-1400 ℃.
7. Si produced by the production method according to any one of claims 1 to 63N4Ceramic structural component, characterized in that said Si3N4The density of the ceramic structural member is 2.14-2.6g/cm3The bending strength is 151-300 MPa.
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| CN113563087A (en) * | 2021-07-05 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Silicon nitride ceramic component and method for producing same |
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| CN115677356A (en) * | 2022-10-20 | 2023-02-03 | 基迈克材料科技（苏州）有限公司 | Preparation method of high-performance silicon nitride ceramic substrate |
| CN116041051B (en) * | 2023-01-16 | 2024-03-22 | 广东工业大学 | Granulating powder applied to 3DP printing and printing forming method thereof |
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| CN116813354A (en) * | 2023-06-06 | 2023-09-29 | 东莞理工学院 | Method for preparing silicon nitride ceramic in situ, prepared silicon nitride ceramic and application thereof |
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