CN110655405B - Preparation method of ceramic matrix composite structure - Google Patents
Preparation method of ceramic matrix composite structure Download PDFInfo
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- CN110655405B CN110655405B CN201910941782.1A CN201910941782A CN110655405B CN 110655405 B CN110655405 B CN 110655405B CN 201910941782 A CN201910941782 A CN 201910941782A CN 110655405 B CN110655405 B CN 110655405B
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000000110 selective laser sintering Methods 0.000 claims abstract description 11
- 238000005470 impregnation Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000007654 immersion Methods 0.000 claims abstract 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 27
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 10
- 229920003257 polycarbosilane Polymers 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims 4
- 230000008676 import Effects 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 238000009694 cold isostatic pressing Methods 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 12
- 239000000919 ceramic Substances 0.000 abstract description 6
- 238000010146 3D printing Methods 0.000 abstract description 2
- 238000011049 filling Methods 0.000 description 8
- 238000007789 sealing Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000010073 coating (rubber) Methods 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- 239000012700 ceramic precursor Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000004814 ceramic processing Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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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
- C04B35/515—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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
本发明公开了一种所述陶瓷基复合材料结构的制备方法包括步骤：1)建立陶瓷基复合材料的三维结构的数字模型；2)将所述数字模型导入SLS设备，进行选择性激光烧结，得到试件；3)对试件进行脱脂处理，得到坯体；4)坯体称得质量为x1，然后放入密封袋中，且密封袋中注满浸渍液，将密封袋送入CIP设备加压处理，取出后得到湿坯体；5)对湿坯体进行高温裂解处理，冷却后称得质量为x2；当x2＜1.01*x1时即得陶瓷基复合材料结构件。将3D打印陶瓷技术与PIP法浸渍裂解工艺和CIP冷等静压技术相结合，实现了梯度点阵碳化硅陶瓷基复合材料结构的近净成型，制备出高致密性的梯度点阵SiCp/SiC陶瓷基复合材料结构件。
The invention discloses a preparation method of the ceramic matrix composite material structure, comprising the steps of: 1) establishing a digital model of the three-dimensional structure of the ceramic matrix composite material; 2) importing the digital model into an SLS device to perform selective laser sintering, Obtain the test piece; 3) Degrease the test piece to obtain a green body; 4) The green body is weighed with a mass of x 1 , and then placed in a sealed bag, and the sealed bag is filled with immersion liquid, and the sealed bag is sent to CIP The equipment is pressurized and taken out to obtain a wet green body; 5) The wet green body is subjected to high temperature cracking treatment, and the mass is weighed as x 2 after cooling; when x 2 <1.01*x 1 , a ceramic matrix composite material structure is obtained. Combining the 3D printing ceramic technology with the PIP method impregnation cracking process and the CIP cold isostatic pressing technology, the near-net shape of the gradient lattice SiC ceramic matrix composite structure was realized, and the high-density gradient lattice SiC p / SiC ceramic matrix composite structural parts.
Description
Technical Field
The invention relates to the technical field of manufacturing workpieces with special shapes by using powder, in particular to a preparation method of a ceramic matrix composite structure.
Background
In recent years, SiC ceramic materials have received much attention from domestic and foreign researchers because of their excellent properties such as high temperature resistance, wear resistance, high strength, and high strength. However, the characteristics of high strength and high hardness bring great difficulties to production and processing. The traditional ceramic processing technology often has the problems of complex mold, higher cost, long period and the like, and the complex structural part is formed with difficulty, so that the exploration of the SiC ceramic matrix composite material with high performance and complex structure formed by a non-grinding tool method is particularly important.
Compared with other rapid forming technologies, the Selective Laser Sintering (SLS) technology has the advantages of high speed and high precision for forming large-size ceramic structural parts, and is widely applied at present, but the SLS technology adopts powder for layered manufacturing, so that the green body prepared by the process has the problems of low density, low strength and the like.
Disclosure of Invention
The ceramic precursor conversion process (PIP) is an advanced ceramic material which is difficult to obtain by the traditional ceramic process by prefabricating a polymer which can be converted into the ceramic material and fully utilizing the good processing characteristics of the polymer in a heat treatment mode. The density of the ceramic material can be improved by multiple dipping and cracking, and a new way is provided for the preparation technology of the ceramic structural member with a complex structure and high forming precision.
Based on the problems of low density and low strength of a green body in the existing single practical SLS technology, the invention provides a preparation method of a ceramic matrix composite structure, which is used for preparing SiC by combining selective laser sintering with normal-pressure impregnation cracking in the early stagePOn the basis of research on the SiC ceramic matrix composite, the improved Cold Isostatic Pressing (CIP) process is introduced, and the SiC with the near-net-shape gradient lattice structure is successfully preparedPthe/SiC ceramic matrix composite combines three molding processes of SLS, PIP and CIP to realize the preparation of the complex member of the SiC ceramic matrix composite.
The preparation method of the ceramic matrix composite structure comprises the following steps:
1) establishing a digital model of the three-dimensional structure of the ceramic matrix composite material;
2) introducing the digital model into an SLS device, and carrying out selective laser sintering by taking SiC composite powder mixed with epoxy resin as a raw material to obtain a test piece;
3) degreasing the test piece to obtain a blank body;
4) the blank is weighed to have mass x1Then placing the blank into a sealing bag, filling the sealing bag with the impregnation liquid, conveying the sealing bag into CIP equipment for pressurization treatment, and taking out the sealing bag to obtain a wet blank;
5) carrying out pyrolysis treatment on the wet blank, and weighing the mass as x after cooling2；
Wherein, when x2≥1.01*x1Repeating steps 4 and 5 when x is2＜1.01*x1And obtaining the ceramic matrix composite structural member. The ceramic matrix composite structure is a gradient lattice member.
Further, the epoxy resin in the step 2 accounts for 3-8% of the raw materials in mass ratio. The SiC composite powder includes: the mixed powder of the silicon carbide micro powder and the silicon carbide granulation powder. And 3, the temperature of the degreasing treatment is 600-800 ℃. Step 4, the impregnation liquid is polycarbosilane solution; preferably, the polycarbosilane solution comprises polycarbosilane, diethylbenzene and tetrahydrofuran; preferably, the volume ratio of polycarbosilane, diethylbenzene and tetrahydrofuran is 4:3: 3. And 4, pressurizing at 150-200 MPa for the pressurizing treatment, and keeping the pressure for 1-5 min. And 5, carrying out pyrolysis treatment at 1200-1400 ℃, and keeping the temperature for 0.5-1 h.
The invention has the beneficial effects that:
1. the gradient lattice ceramic structural member which cannot be formed by the traditional casting method is realized by the 3D printing technology, and the forming time is greatly shortened;
2. according to the invention, the test piece coated in the impregnation liquid is subjected to pressurized impregnation by a CIP technology, so that the closed porosity of the test piece is greatly reduced on the premise of ensuring that the size of the test piece is not shrunk, and the compactness of the test piece is improved;
3. the 3D ceramic printing technology is combined with a PIP method impregnation cracking process and a CIP cold isostatic pressing technology, so that the near-net forming of the gradient lattice silicon carbide ceramic matrix composite structure is realized, and the SiC of the high-compactness gradient lattice is preparedpThe structure is made of/SiC ceramic matrix composite.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below. It is clear that the described figures are only some embodiments of the invention, not all embodiments, and that a person skilled in the art can also derive other designs and figures from them without inventive effort.
FIG. 1 is a schematic view of a digital model of a three-dimensional structure established in step 1) of example 1;
FIG. 2 is a perspective view of the ceramic matrix composite structure obtained in step 5) of example 1.
Detailed Description
The first embodiment is as follows: the preparation method of the ceramic matrix composite structure comprises the following steps:
1) setting a digital model for designing a gradient lattice three-dimensional structure of the ceramic matrix composite structure, converting the digital model into an STL format file, and importing the STL format file into 3D printer software for automatic layering;
2) mechanically mixing SiC composite powder with a proper amount of resin powder, drying the composite powder, adding the composite powder into a 3D printer feeding cylinder, setting parameters of a 3D printer, namely layered thickness, filling speed, profile speed, filling interval, filling power, profile power and heating temperature, starting equipment, printing a test piece layer by layer, cooling the test piece to room temperature after printing is completed, and taking out the test piece for powder cleaning;
3) carrying out high-temperature degreasing treatment on the test piece after powder cleaning to obtain a blank body;
4) weighing the mass x of the blank1Filling the blank into a rubber coating bag filled with impregnation liquid, carrying out vacuum sealing treatment, putting the sealed rubber coating bag into a cold isostatic pressing device, and carrying out pressurization treatment to obtain a wet blank;
5) carrying out high-temperature cracking on the wet blank, and weighing the wet blank to be x after cooling2Due to x2＜1.01*x1Therefore, the ceramic precursor is completely converted, and the ceramic matrix composite structural member is obtained.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: and (3) using UG software to draw a three-dimensional model of the gradient lattice structure in the step 1, wherein the rest is the same as that of the first specific embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the step 2, the silicon carbide composite powder is a mixed powder of silicon carbide micro powder and silicon carbide granulation powder, and the rest is the same as that in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the step 2, the binder powder is epoxy resin, the mass percentage content is 3-8%, and the rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the 3D printer in step 2 is an HK S500 model SLS rapid prototyping system, the others being the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the degreasing temperature in the step 3 is 600-800 ℃, and the rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the dipping solution in the step 4 is polycarbosilane solution, and the rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the CIP in the step 4 has the pressurizing pressure of 150-200 MPa and the pressure maintaining time of 1-5 min, and the rest is the same as one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and 5, the temperature of the high-temperature degreasing in the step 5 is 1200-1400 ℃, the heat preservation time is 0.5-1 h, and the rest is the same as one of the first to eighth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: SiC of gradient lattice structurepThe preparation method of the/SiC ceramic matrix composite material comprises the following steps:
1) designing a digital model of a gradient lattice three-dimensional structure, converting the digital model into an STL format file, and importing the STL format file into 3D printer software for automatic layering;
2) mechanically mixing the SiC micro powder and SiC granulated powder mixed powder with epoxy resin powder accounting for 5% of the total mass for 12 hours, drying the composite powder at 120 ℃, adding the composite powder into a feeding cylinder of a 3D printer, and paving for later use; setting 3D printer parameters: the method comprises the steps of enabling the layering thickness to be 0.1mm, the filling speed to be 1500-4400 mm/s, the profile speed to be 1500-4000 mm/s, the filling interval to be 0.1-0.2 mm, the filling power to be 14-18W, the profile power to be 12-18W and the heating temperature to be 40-60 ℃, then starting equipment, printing the test piece layer by layer, and taking out the test piece for powder cleaning after the test piece is printed and cooled to the room temperature;
3) placing the test piece after powder cleaning into a high-temperature sintering furnace for degreasing treatment at 600-800 ℃ to obtain a blank;
4) weighing 206.31g of blank, putting the blank into a rubber coating bag filled with impregnation liquid, discharging air, and sealing; putting the sealed rubber coating bag into a cold isostatic pressing device, pressurizing at 200MPa, and maintaining the pressure for 3min to obtain a wet blank;
5) carrying out pyrolysis on the wet blank at 1380 ℃, keeping the temperature for 0.5h, and weighing 209.15 g;
since 209.15 > 1.01 x 206.31, steps 4, 5 were repeated. Repeating twice, respectively measuring mass data of 211.45 (> 1.01 x 209.15) and 211.87 (< 1.01 x 211.45), thus judging that the ceramic precursor conversion is completely finished, namely the required gradient lattice SiCpThe structure is made of/SiC ceramic matrix composite.
Claims (9)
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| CN113735590B (en) * | 2021-09-29 | 2022-06-28 | 北京理工大学 | Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material |
| CN116444275B (en) * | 2023-04-26 | 2024-07-16 | 哈尔滨理工大学 | Method for preparing low-porosity SiC ceramic matrix composite by combining SLS and PIP |
| CN116675538B (en) * | 2023-05-30 | 2023-12-22 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
| CN117209297B (en) * | 2023-09-15 | 2025-01-03 | 哈尔滨工业大学 | Preparation method of carbon fiber/SiHfBOC composite material based on high-temperature protection of silicon oxide-hafnium oxide composite oxide layer |
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| CN106495699A (en) * | 2016-11-10 | 2017-03-15 | 哈尔滨理工大学 | A kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell |
| CN107573080A (en) * | 2017-09-29 | 2018-01-12 | 山东大学 | A kind of infusion process prepares SiCN/Si3N4The method of composite ceramics |
| CN107602130A (en) * | 2017-10-17 | 2018-01-19 | 哈尔滨理工大学 | The method that porous SiC ceramics are prepared based on 3D forming techniques |
| CN108484173B (en) * | 2018-06-05 | 2020-09-08 | 中国建筑材料科学研究总院有限公司 | SiCf/SiC composite material and preparation method thereof |
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