CN116444275A - Method for preparing low-porosity SiC ceramic matrix composite by combining SLS and PIP - Google Patents
Method for preparing low-porosity SiC ceramic matrix composite by combining SLS and PIP Download PDFInfo
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 34
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- 229920000647 polyepoxide Polymers 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000000835 fiber Substances 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 33
- 238000005336 cracking Methods 0.000 claims abstract description 30
- 238000005238 degreasing Methods 0.000 claims abstract description 27
- 239000011230 binding agent Substances 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000005470 impregnation Methods 0.000 claims abstract description 13
- 238000010146 3D printing Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 88
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 229920003257 polycarbosilane Polymers 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- 239000012298 atmosphere Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000009987 spinning Methods 0.000 claims description 9
- 230000004584 weight gain Effects 0.000 claims description 9
- 235000019786 weight gain Nutrition 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 238000010041 electrostatic spinning Methods 0.000 claims description 8
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- 238000005516 engineering process Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 16
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 102
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- 238000007598 dipping method Methods 0.000 description 24
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- 230000000052 comparative effect Effects 0.000 description 13
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- 238000000227 grinding Methods 0.000 description 6
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 238000000626 liquid-phase infiltration Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- 229910000831 Steel Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 238000007792 addition Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
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- 238000004377 microelectronic Methods 0.000 description 1
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- 238000003892 spreading Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000008096 xylene Substances 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
- 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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention relates to the field of 3D printing of SiC ceramics, in particular to a method for preparing a SiC ceramic matrix composite material with low porosity by combining SLS and PIP, which comprises the following steps: (1) Uniformly mixing SiC powder with a binder in a mixer to obtain composite powder, wherein the binder is a mixture of epoxy resin fibers and epoxy resin particles; (2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology, so as to obtain an SiC ceramic primary blank; (3) Degreasing and high-temperature sintering the SiC ceramic primary blank obtained in the step (2) to obtain SiC porous ceramic; (4) And (3) densifying the SiC porous ceramic in the step (3) by using a precursor impregnation cracking technology (PIP) to obtain the SiC ceramic matrix composite with low porosity. By the method, the SiC ceramic matrix composite material with lower porosity and higher density is successfully obtained.
Description
Technical Field
The invention relates to the field of 3D printing of SiC ceramics, in particular to a method for preparing a SiC ceramic matrix composite material with low porosity by combining SLS and PIP.
Background
Silicon carbide ceramics have excellent performances such as high strength, high hardness, wear resistance, corrosion resistance and the like in a high-temperature environment, are widely applied to various fields such as aerospace, nuclear energy, automobiles, petrochemical industry, microelectronics and the like at present, but the high strength and the high hardness of the silicon carbide ceramics also bring great difficulty to material processing, especially parts with complex surfaces and internal structures, have long processing period and high cost, and become bottleneck problems.
The additive manufacturing technology is a novel forming mode, and different from the traditional subtractive manufacturing mode, the additive manufacturing technology can directly form a three-dimensional structure by increasing a model drawn by a computer layer by layer. The Selective Laser Sintering (SLS) technique was one of the 3D printing additive manufacturing techniques, originally proposed by declicard, division of Austin by the university of Texas in 1986, and subsequently commercialized by DTM corporation. The laser selectively irradiates on the powder in the working cylinder, the melted resin is used as a binder to bond the surrounding powder together, then the working cylinder descends, the feeding cylinders at the two ends ascend, the powder spreading roller pushes the powder in the feeding cylinders to cover the sintered part of the working cylinder, a layer of sintering is completed, the sintering is repeated until the sintering of the test piece is completed, the unsintered powder is removed, and the three-dimensional solid part is obtained. However, ceramic parts produced by the SLS process still have some fatal defects such as low density, high porosity, and poor mechanical properties due to non-uniformity.
To improve the compactibility and mechanical properties of molded parts, some scholars have proposed hybrid manufacturing methods such as Selective Laser Sintering (SLS)/Cold Isostatic Pressing (CIP) and Selective Laser Sintering (SLS)/Melt Infiltration (MI), which can improve the compactibility and mechanical properties of ceramic matrix composites. However, the methods of SLS/CIP and SLS/MI still have some drawbacks to overcome. Such as the SLS/CIP method is not suitable for manufacturing ceramic matrix composites with complex internal structures, the high temperature performance of the samples manufactured by SLS/MI is not ideal, etc.
The preparation method of the SiC composite material mainly comprises a chemical vapor infiltration method (CVI), a molten silicon infiltration method (LSI), a polymer impregnation cracking technology (PIP) and the like. Compared with CVI, LSI and other methods, the PIP method has great advantages in the aspects of saving material preparation time, reducing material sintering temperature, reducing material manufacturing cost and the like.
At present, although there are reports on the combination of SLS and PIP for manufacturing ceramic matrix composites, the obtained SiC ceramic matrix composites still have the defects of insufficient compactness and higher porosity. In addition, although the combined use of PIP techniques can improve the density of the SLS-prepared SiC ceramic matrix composite to some extent, the polymer precursors can clog the external pores in the SiC ceramic matrix during multiple dip-cracking, resulting in failure of the polymer precursors to enter the internal pores during subsequent dip-cracking, and thus failure to achieve lower porosity and thus greater density.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which comprises the following steps:
(1) Uniformly mixing SiC powder with a binder in a mixer to obtain composite powder, wherein the binder is a mixture of epoxy resin fibers and epoxy resin particles;
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology, so as to obtain an SiC ceramic primary blank;
(3) Degreasing and high-temperature sintering the SiC ceramic primary blank obtained in the step (2) to obtain SiC porous ceramic;
(4) And (3) densifying the SiC porous ceramic in the step (3) by using a precursor impregnation cracking technology (PIP) to obtain the SiC ceramic matrix composite with low porosity.
Further, the composite powder in the step (1) comprises 80-95% (mass percent) of SiC powder, and the balance is binder. Further, in step (1) of the method, the composite powder contains 80 to 90% by mass of SiC powder, and the balance being a binder. Further, in step (1) of the method, the composite powder contains 85% (mass percent) SiC powder, and the balance is a binder.
Further, the average particle diameter of the SiC powder in the step (1) is 20 to 70 μm. Further, the average particle diameter of the SiC powder in the step (1) is 40 to 60. Mu.m. Further, the average particle diameter of the SiC powder in the step (1) is 50. Mu.m.
Further, the average diameter of the epoxy resin fibers in the step (1) is 1-3 μm and the length is 0.5-2mm.
Further, the average particle diameter of the epoxy resin particles in the step (1) is 3 to 5 μm,
further, the mass ratio of epoxy resin fibers to epoxy resin particles in the binder in the step (1) is 1:4-8. Further, the mass ratio of the epoxy resin fibers to the epoxy resin particles in the binder epoxy resin in the step (1) is 1:4.
Further, the epoxy resin fiber in the step (1) is prepared by the following method:
dissolving epoxy resin in an organic solvent to obtain a spinning solution;
spinning the spinning solution by a high-voltage electrostatic spinning method to obtain fibers with average diameters of 1-3 mu m,
quenching the obtained fiber to obtain the epoxy resin fiber with the length of 0.5-2mm.
Further, the particular type of epoxy resin used in the process of the present invention is not limited and may be routinely selected by one of ordinary skill in the art based on particular practices. Further, the epoxy resin used in the method of the present invention is bisphenol A type epoxy resin E-12.
Further, the organic solvent comprises one or more of dichloromethane, chloroform, acetone, methyl ethyl ketone, cyclohexanone, ethyl acetate, toluene, xylene, ethanol or ethylene glycol.
Further, the parameters of the high-voltage electrostatic spinning method are as follows: the high-voltage electrostatic voltage is 5-30kV, the distance between the jet head and the receiving plate is 5-50cm, the outflow speed of the solution from the jet head is 0.1-15mL/h, the ambient temperature is 15-50 ℃, and the air relative humidity is 30-90%. Further, the parameters of the high-voltage electrostatic spinning method are as follows: the high-voltage electrostatic voltage is 20-25kV, the distance between the jet head and the receiving plate is 15-25cm, the outflow speed of the solution from the jet head is 8-10mL/h, the ambient temperature is 25-30 ℃, and the relative air humidity is 45-50%. Further, the parameters of the high-voltage electrostatic spinning method are as follows: the high-voltage electrostatic voltage is 20kV, the distance between the jet head and the receiving plate is 15cm, the outflow speed of the solution from the jet head is 8mL/h, the ambient temperature is 25 ℃, and the relative humidity of air is 45%.
Further, the fiber receiving equipment adopted by the high-voltage electrostatic spinning method is a cage type receiver.
Further, the quenching process includes cooling the received fibers in liquid nitrogen to harden, and then cutting to a desired length.
Further, the parameters of the SLS in step (2) are: the laser power is 15-27W, the scanning speed is 1000-3600mm/s, the scanning interval is 0.08-0.15mm, and the layering thickness is 0.08-0.20mm. Further, the parameters of the SLS in step (2) are: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm, layering thickness 0.10mm. Further, the degreasing treatment in the step (3) is carried out under the condition of heat treatment for 0.5-2h at 600-800 ℃ in nitrogen or inert protective gas atmosphere. Further, the degreasing treatment in the step (3) is performed under the condition of heat treatment at 700 ℃ for 1 hour under an inert protective gas atmosphere. Still further, the degreasing process in step (3) includes heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min.
Further, the condition of the high-temperature sintering treatment in the step (3) is that the high-temperature sintering treatment is carried out for 30-90min at 1000-1600 ℃ under the atmosphere of inert protective gas.
Further, in the step (3), the shielding gas is argon or nitrogen.
Further, the PIP in step (4) comprises immersing the SiC porous ceramic of step (3) in a precursor immersion liquid, curing at 120-150 ℃, and cracking at 1000-1400 ℃.
Further, the precursor impregnating solution comprises polycarbosilane as a precursor and divinylbenzene as a crosslinking agent, wherein the mass ratio of the polycarbosilane to the divinylbenzene is 1:4.
Further, the impregnation comprises impregnating the SiC porous ceramic of the step (3) in a precursor impregnating solution in an impregnating furnace, vacuumizing for 30min at 65 ℃, and pressurizing for 30min at 65 ℃ under 0.2Mpa.
Further, the curing includes curing at 120 ℃ for 3 hours and further curing at 150 ℃ for 3 hours.
Further, the time of the cracking is 30-90min.
Further, the method comprises repeating step (4) one or more times until the SiC porous ceramic has a rate of weight gain of less than 1% compared to the rate of weight gain after the previous precursor dip cracking.
In another aspect, the present invention also provides a low porosity SiC ceramic matrix composite prepared according to the methods described herein.
The beneficial effects of the invention are that
According to the invention, the SLS technology and the PIP technology are combined to prepare the SiC ceramic matrix composite material, so that the defect of low compactness of SiC ceramic prepared by the SLS technology alone is overcome.
However, although the use of PIP technology in combination can improve the density of the prepared SiC ceramic matrix composite to some extent, the polymer precursors can clog the external pores in the SiC ceramic matrix during multiple dip-cracking, resulting in failure of the polymer precursors to enter the internal pores during subsequent dip-cracking, and thus failure to achieve lower porosity and greater density.
Therefore, the invention uses the epoxy resin particles and the epoxy resin fibers as the compound binder when the SLS technology is used for preparing the SiC ceramic primary blank, thereby successfully realizing lower porosity and higher density after the subsequent densification by using the PIP technology.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
The epoxy fibers used in this example section were prepared as follows:
bisphenol A type epoxy resin E-12 (purchased from Guangzhou new rare metallurgy chemical industry Co., ltd.) is dissolved in chloroform to prepare spinning solution with the concentration of 60 weight percent of epoxy resin;
spinning the spinning solution by a high-voltage electrostatic spinning method, wherein the parameters of the high-voltage electrostatic spinning method are as follows: the high-voltage electrostatic voltage is 20kV, the distance between the jet head and the receiving plate is 15cm, the outflow speed of the solution from the jet head is 8mL/h, the ambient temperature is 25 ℃, and the relative air humidity is 45%; placing the fibers on the collecting plate into a vacuum drying oven for drying for 2 hours to obtain fibers with uniform diameter distribution and average diameter of about 2 mu m;
quenching the obtained fiber: the fibers received by the cage receiver were cooled in liquid nitrogen to harden, and then cut with a steel cutter to obtain epoxy fibers having a length of about 1 mm.
Example 1:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Mixing 85wt% of SiC powder (obtained from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 26 μm) with 15wt% of binder in a mixer to obtain composite powder;
wherein the binder is a mixture of 20wt% of the epoxy resin fibers prepared as described above with 80wt% of the epoxy resin E-12 particles (available from Guangzhou New thin Metallurgical chemical Co., ltd., average particle size of 3 to 5 μm);
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃;
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
Example 2:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Mixing 85wt% of SiC powder (obtained from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 50 μm) with 15wt% of binder in a mixer to obtain composite powder;
wherein the binder is a mixture of 20wt% of the epoxy resin fibers prepared as described above with 80wt% of the epoxy resin E-12 particles (available from Guangzhou New thin Metallurgical chemical Co., ltd., average particle size of 3 to 5 μm);
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃,
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
Example 3:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Mixing 85wt% of SiC powder (obtained from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 65 μm) with 15wt% of binder epoxy resin in a mixer to obtain composite powder,
wherein the binder epoxy resin is a mixture of 20wt% of the epoxy resin fibers prepared as described above with 80wt% of the epoxy resin E-12 particles (available from Guangzhou New thin Metallurgical chemical Co., ltd., average particle size of 3 to 5 μm);
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃,
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
Comparative example 1:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Mixing 85wt% of SiC powder (obtained from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 50 μm) with 15wt% of binder epoxy resin in a mixer to obtain composite powder,
wherein the binder epoxy resin was a mixture of 20wt% of the epoxy resin fibers prepared as described above (except that the epoxy resin fibers cut to a length of about 0.2mm by a steel cutter were used in this comparative example) and 80wt% of the particles of the epoxy resin E-12 (available from Guangzhou New rare metallurgical chemical Co., ltd., average particle size of 3 to 5 μm);
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃,
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
Comparative example 2:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Uniformly mixing 85wt% of SiC powder (purchased from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 50 μm) with 15wt% of binder epoxy resin in a mixer to obtain composite powder;
wherein the binder epoxy resin was a mixture of 20wt% of the epoxy resin fibers prepared as described above (except that the epoxy resin fibers cut to a length of about 5mm by a steel cutter were used in this comparative example) and 80wt% of the epoxy resin E-12 particles (available from Guangzhou New thin Metallurgical chemical Co., ltd., average particle size of 3 to 5 μm);
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃,
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
Comparative example 3:
the embodiment provides a method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, which is prepared as follows:
(1) Uniformly mixing 85wt% of SiC powder (purchased from Shandong Qingdao mountain land grinding materials Co., ltd., average particle size of 50 μm) with 15wt% of epoxy resin E-12 particles (purchased from Guangzhou New rare metallurgy chemical industry Co., ltd., average particle size of 3-5 μm) in a mixer to obtain composite powder;
(2) 3D printing is carried out on the composite powder in the step (1) by using a Selective Laser Sintering (SLS) technology to obtain an SiC ceramic primary blank, wherein the SLS parameters are as follows: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm and layering thickness 0.10mm;
(3) Degreasing the SiC ceramic primary blank obtained in the step (2), wherein the degreasing temperature is 700 ℃, the heat preservation time is 1h, and the temperature-raising program of the degreasing process is as follows: heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min;
then sintering at 1200 ℃ for 60min under the atmosphere of argon shielding gas to obtain SiC porous ceramic;
(4) Dipping the SiC porous ceramic of the step (3) in a precursor dipping solution containing polycarbosilane (purchased from Sirofil fiber Co., ltd., number average molecular weight 1395) as a precursor and divinylbenzene as a crosslinking agent (mass ratio of polycarbosilane to divinylbenzene is 1:4) in a dipping furnace, vacuumizing at 65 ℃ for 30min, and pressurizing at 65 ℃ for 30min at 0.2Mpa;
after the impregnation is completed, the SiC porous ceramic is solidified for 3 hours at 120 ℃ and then solidified for 3 hours at 150 ℃,
cracking the cured SiC porous ceramic in a vacuum sintering furnace with nitrogen protection at 1200 ℃ for 30min, wherein the temperature-raising program of the cracking process is as follows: heating from room temperature to 200 ℃ at a heating rate of 10 ℃/min, heating from 200 ℃ to 1100 ℃ at a heating rate of 6 ℃/min, and heating from 1100 ℃ to 1200 ℃ at a heating rate of 10 ℃/min;
and (3) repeating the step (4) one or more times until the weight gain rate of the SiC porous ceramic is less than 1% compared with that of the SiC porous ceramic after the previous precursor dipping and cracking, thereby obtaining the SiC ceramic matrix composite material with low porosity.
The density and porosity of the SiC ceramic matrix composites prepared in examples 1 to 3 and comparative examples 1 to 3 were measured by archimedes' method, and the results are shown in table 1 below:
TABLE 1
| Porosity (%) | Density (g/cm) 3 ) | |
| Example 1 | 14.39 | 2.77 |
| Example 2 | 10.68 | 2.88 |
| Example 3 | 12.16 | 2.84 |
| Comparative example 1 | 18.83 | 2.63 |
| Comparative example 2 | 20.42 | 2.57 |
| Comparative example 3 | 25.81 | 2.40 |
From the results of table 1, it is seen that the porosity of the SiC ceramic matrix composites prepared in examples 1 to 3 of the present invention is significantly reduced compared to the porosity of the SiC ceramic matrix composites prepared without the addition of the epoxy fibers (comparative example 3). Wherein the average particle diameter of the SiC powder has a certain influence on the effect of reducing the porosity, and the porosity is lowest when the average particle diameter of the SiC powder is 50 μm.
Furthermore, as is evident from the results of comparative examples 1 and 2, the lengths of the epoxy resin fibers have a significant effect on the effect of reducing the porosity, and epoxy resin fibers that are too short (0.22 mm, comparative example 1) or too long (5 mm, comparative example 2) result in a significantly increased porosity as compared to examples 1 to 3 (the length of the epoxy resin fibers is 1 mm).
In the description of the specification, reference to the term "one embodiment," "a particular embodiment," "an example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or by similar arrangements, by those skilled in the art, without departing from the scope of the invention or beyond the scope of the appended claims.
Claims (10)
1. A method for preparing a low-porosity SiC ceramic matrix composite by combining SLS and PIP, the method is characterized by comprising the following steps of:
(1) Uniformly mixing SiC powder with a binder in a mixer to obtain composite powder, wherein the binder is a mixture of epoxy resin fibers and epoxy resin particles,
wherein the average particle diameter of the SiC powder is 20-70 mu m,
the average diameter of the epoxy resin fiber is 1-3 mu m, the length is 0.5-2mm,
the average particle diameter of the epoxy resin particles is 3-5 mu m,
the mass ratio of the epoxy resin fibers to the epoxy resin particles in the adhesive is 1:4-8;
(2) 3D printing is carried out on the composite powder in the step (1) by SLS, and a SiC ceramic primary blank is obtained;
(3) Degreasing and high-temperature sintering the SiC ceramic primary blank obtained in the step (2) to obtain SiC porous ceramic;
(4) And (3) densifying the SiC porous ceramic in the step (3) by using PIP to obtain the SiC ceramic matrix composite with low porosity.
2. The method of claim 1, wherein the epoxy resin fibers in step (1) are prepared by:
dissolving epoxy resin in an organic solvent to obtain a spinning solution;
spinning the spinning solution by a high-voltage electrostatic spinning method to obtain fibers with average diameters of 1-3 mu m, and quenching the obtained fibers to obtain the epoxy resin fibers with lengths of 0.5-2mm.
3. The method of claim 1, wherein the composite powder in step (1) comprises 80-95% SiC powder, the remainder being binder epoxy.
4. The method of claim 1, wherein the parameters of the SLS in step (2) are: the laser power is 15-27W, the scanning speed is 1000-3600mm/s, the scanning interval is 0.08-0.15mm, and the layering thickness is 0.08-0.20mm;
preferably, the parameters of the SLS in step (2) are: laser power 18W, scanning speed 3600mm/s, scanning interval 0.15mm, layering thickness 0.10mm.
5. The method according to claim 1, wherein the degreasing treatment in step (3) is performed under nitrogen or an inert protective gas atmosphere at 600 to 800 ℃ for 0.5 to 2 hours;
preferably, the degreasing treatment in the step (3) is performed under the condition of heat treatment at 700 ℃ for 1 hour under nitrogen or inert protective gas atmosphere;
preferably, the degreasing treatment in step (3) includes heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, heating from 300 ℃ to 600 ℃ at a heating rate of 3 ℃/min, and heating from 600 ℃ to 700 ℃ at a heating rate of 5 ℃/min.
6. The method according to claim 1, wherein the conditions of the high-temperature sintering treatment in step (3) are heat treatment at 1000 to 1600 ℃ for 30 to 90min under an inert protective gas atmosphere.
7. The method of claim 1, wherein the PIP in step (4) comprises impregnating the SiC porous ceramic of step (3) in a precursor impregnation solution, curing at 120-150 ℃, and cracking at 1000-1400 ℃.
8. The method of claim 7, wherein the precursor dip comprises polycarbosilane as a precursor and divinylbenzene as a crosslinking agent, wherein the mass ratio of polycarbosilane to divinylbenzene is 1:4;
preferably, the impregnation comprises evacuating in an impregnation oven at a temperature of 65℃for 30min, then pressurizing at a temperature of 65℃for 30min, at a pressure of 0.2MPa,
preferably, the curing comprises curing at 120℃for 3 hours, further curing at 150℃for 3 hours,
preferably, the time of the cleavage is 30-90min.
9. The method of any one of claims 1-8, comprising repeating step (4) one or more times until the SiC porous ceramic has a rate of weight gain of less than 1% after a previous precursor dip cracking.
10. A low porosity SiC ceramic matrix composite made by the method of any one of claims 1-9.
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