CN116573952A - Adhesive jet printing silicon carbide-aluminum composite material and preparation method thereof - Google Patents
Adhesive jet printing silicon carbide-aluminum composite material and preparation method thereof Download PDFInfo
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- CN116573952A CN116573952A CN202310570951.1A CN202310570951A CN116573952A CN 116573952 A CN116573952 A CN 116573952A CN 202310570951 A CN202310570951 A CN 202310570951A CN 116573952 A CN116573952 A CN 116573952A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 238000007639 printing Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000853 adhesive Substances 0.000 title description 6
- 230000001070 adhesive effect Effects 0.000 title description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 142
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 130
- 239000000843 powder Substances 0.000 claims abstract description 64
- 239000000919 ceramic Substances 0.000 claims abstract description 49
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 239000000725 suspension Substances 0.000 claims abstract description 22
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000005238 degreasing Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 11
- 238000005269 aluminizing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 60
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 230000008595 infiltration Effects 0.000 claims description 19
- 238000001764 infiltration Methods 0.000 claims description 19
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000001723 curing Methods 0.000 claims description 11
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 2
- VAPQAGMSICPBKJ-UHFFFAOYSA-N 2-nitroacridine Chemical compound C1=CC=CC2=CC3=CC([N+](=O)[O-])=CC=C3N=C21 VAPQAGMSICPBKJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 229940068886 polyethylene glycol 300 Drugs 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 229940047670 sodium acrylate Drugs 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000000930 thermomechanical effect Effects 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 238000005452 bending Methods 0.000 description 7
- 238000013001 point bending Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000555 poly(dimethylsilanediyl) polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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Abstract
The application discloses a silicon carbide-aluminum composite material for binder jet printing and a preparation method thereof, and relates to the field of composite materials. Preparing silicon carbide spherical granulating powder; performing binder jet printing based on silicon carbide spherical granulating powder to obtain a first blank; removing residual powder, curing and degreasing the first blank to obtain a second blank; impregnating the second blank in an impregnating solution to perform impregnating treatment, and drying to obtain a third blank, wherein the impregnating solution is nano SiC ceramic suspension or a mixed solution of polycarbosilane and nano SiC powder; the nano SiC ceramic suspension is a mixed solution of nano SiC, a solvent and a dispersing agent, and the concentration of the nano SiC is 10-40 vol%; the mass of the nano SiC powder is 5-15% of that of the polycarbosilane; sintering the third blank to obtain a silicon carbide ceramic sintered body; and (5) carrying out aluminizing in the silicon carbide sintered body to obtain the silicon carbide-aluminum composite material. The application can improve the density and the thermal-mechanical property of the silicon carbide ceramic sprayed and printed by the binder.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to a silicon carbide-aluminum composite material for adhesive jet printing and a preparation method thereof.
Background
Silicon carbide (SiC) ceramics have excellent comprehensive properties of high temperature resistance, corrosion resistance, wear resistance, irradiation resistance, high strength, high hardness, small thermal expansion rate and the like, and are widely applied to the fields of automobiles, machinery, chemical industry, environmental protection, space technology, information electronics, energy sources and the like. In particular, the excellent heat conduction performance (theoretical heat conductivity is up to 490 W.m < -1 >. K < -1 >) is widely used for heat dissipation of electronic components or industrial heat exchange devices. Among them, heat-dissipating devices like industrial grade heat-dissipating devices or heat-exchanging devices involve complex shapes and large sizes, such as finned heat-dissipating devices or fluid channels. The traditional silicon carbide ceramic forming process comprises isostatic pressing, tape casting, injection molding, slip casting, gel casting and the like, and usually adopts a die for auxiliary forming, and the required silicon carbide product is obtained by machining after sintering. However, due to the inherent hardness and brittleness of silicon carbide ceramics and the long preparation period of complex molds, conventional molding methods have long periods and high cost when preparing complex lightweight silicon carbide components, and large-sized components are usually obtained by splicing methods, resulting in high rejection rates, and some internal complex structures are difficult or impossible to manufacture.
Binder Jetting technology (Binder Jetting) is one of the technologies of additive manufacturing (commonly called 3D printing technology), and is to selectively jet and deposit a liquid Binder to bond ceramic powder materials, accumulate layer by layer to obtain a ceramic three-dimensional blank, and perform post-treatment such as Binder curing, degreasing, sintering and the like to obtain a required compact ceramic product. The technology has the advantages of low preparation cost, high printing speed, high printing precision, capability of printing large-size complex ceramic parts and the like, and can effectively solve the problem that the traditional forming technology is difficult to prepare large-size ceramic parts with complex shapes.
Infiltration is a common method for improving the density of SiC, chinese patent application number is CN 202210113916.2, publication number is CN 114480908B, the application creates a high-specific-fraction functional gradient aluminum-based silicon carbide composite material and a preparation method thereof, and the application discloses a gradient porous structure silicon carbide preform obtained by combining an additive manufacturing technology with infiltration polycarbosilane solution, polydimethylsilane solution or heteroelement polycarbosilane solution, and a liquid aluminum alloy filling technology is adopted to prepare the high-specific-fraction functional gradient aluminum-based silicon carbide composite material. However, the method directly infiltrates precursors such as polycarbosilane, and the precursors generate gas or thermal stress in the cracking process, so that ceramic blanks with weak strength are easy to damage and influence the integrity of the blanks, and the method directly uses large-particle SiC powder, which is not beneficial to the improvement of sintering activity. Therefore, the method for improving the green body density and the sintering activity without cracking or reducing the thermal stress generated by decomposition in the cracking process is provided, and has important significance for preparing the high-performance SiC ceramic.
However, the binder injection molding technique is limited by the particle size of the powder, and large-size silicon carbide powder (particle size: 20 μm) is usually selected to ensure the powder flowability, which not only causes more voids in the interior of the printing blank, but also greatly reduces the sintering activity of the silicon carbide ceramic, particularly the Si-C covalent bond of the silicon carbide, so that the silicon carbide ceramic diffuses slowly in the sintering process, and further causes that the high-density silicon carbide ceramic component is difficult to prepare by using the binder injection molding technique, and the thermal conductivity (pore thermal conductivity is 0 W.m -1 ·K -1 ) And the bending strength (most affected by the gas holes) is drastically reduced, which severely limits the development and application of large-sized, complex-structure silicon carbide ceramic heat converters. Therefore, a method for improving the density and the thermo-mechanical property of the adhesive jet printing silicon carbide ceramic is urgently needed.
Disclosure of Invention
The embodiment of the application provides a silicon carbide-aluminum composite material for adhesive jet printing and a preparation method thereof, aiming at achieving the purpose of improving the density and the thermo-mechanical property of the silicon carbide ceramic for adhesive jet printing.
The application provides a preparation method of a silicon carbide-aluminum composite material by binder jet printing, which uses submicron powder for spray granulation, so that the powder is ensured to have fluidity and the sintering activity of the powder is improved; the density of the formed blank is improved by printing, forming and degreasing and then impregnating with nano SiC ceramic suspension or a mixture of polycarbosilane and nano SiC powder, so that the compactness of the sintered silicon carbide ceramic is improved, and finally the compactness and the thermo-mechanical property of the silicon carbide ceramic are further improved by aluminizing.
In a first aspect, an embodiment of the present application provides a method for preparing a binder jet-printed silicon carbide-aluminum composite material, including:
s1, weighing silicon carbide powder, a sintering aid and a dispersing solvent to form a mixture, and sequentially performing ball milling, drying, sieving and spray granulation on the mixture to obtain silicon carbide spherical granulating powder;
s2, taking the silicon carbide spherical granulating powder as a printing raw material, and performing binder jet printing according to preset printing parameters and preset design structures to obtain a first blank;
s3, removing residual powder, curing and degreasing the first blank body to obtain a second blank body;
s4, impregnating the second blank in an impregnating solution to perform impregnating treatment, and drying to obtain a third blank, wherein the impregnating solution is nano SiC ceramic suspension or a mixture of polycarbosilane and nano SiC powder; the nano SiC ceramic suspension is a mixed solution of nano SiC, a solvent and a dispersing agent, and the concentration of the nano SiC in the nano SiC ceramic suspension is 10-40 vol%; in the mixed solution of the polycarbosilane and the nano SiC powder, the mass of the nano SiC powder is 5-15% of that of the polycarbosilane;
s5, sintering the third blank to obtain a silicon carbide ceramic sintered body;
s6, carrying out aluminizing in the silicon carbide sintered body to obtain the silicon carbide-aluminum composite material.
The further technical proposal comprises the following steps of S1, in parts by mass80-95 parts of silicon carbide powder and 5-20 parts of sintering aid; the grain diameter of the silicon carbide powder is 0.1-3 mu m; the sintering aid is Al 2 O 3 、Y 2 O 3 、MgO、CaO、TiO 2 、La 2 O 3 、AlN、B 4 C、C、SiO 2 The particle size of the sintering aid is 0.1-1 mu m, and the purity of the sintering aid is more than 99.5%; the dispersion solvent is at least one of deionized water, absolute ethyl alcohol and methanol.
The further technical proposal comprises the following steps that in the step S1, the technological parameters of ball milling comprise ball milling rotation speed of 200-400 rpm and ball milling time of 0.5-6 h; the drying process parameters comprise the drying temperature of 50-120 ℃ and the drying time of 3-24 h; the number of the screening meshes is 50-100 meshes. The purpose of the drying is to remove the dispersing solvent.
The further technical proposal comprises that the grain diameter of the silicon carbide spherical granulation powder is 10-100 mu m, thus ensuring good fluidity.
The further technical proposal comprises the step S2, wherein the printing parameters comprise a printing layer thickness of 50-300 mu m, a scraper speed of 1-6 cm/S and a glue saturation of 50-100%. The design structure may be in a cube shape, a cylindrical shape, etc., and may be designed by modeling software, and the present application is not particularly limited.
The further technical scheme includes that in step S3, the technological parameters of the curing treatment include: the curing temperature is 100-300 ℃, the heat preservation time is 0.5-3 h, and the second blank body is ensured to have better strength; the degreasing treatment comprises the following steps: heating to 300-600 ℃ at 0.5-10 ℃/min under the air atmosphere, keeping the temperature for 1-6 h, and then cooling to room temperature at 0.5-10 ℃/min.
In the step S4, the particle size of the nano SiC is 10-200 nm, the solvent is at least one of deionized water, absolute ethyl alcohol, acetone and methanol, the dispersing agent is at least one of citric acid, oxalic acid, sodium acrylate, potassium acrylate, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400 and polyethylene glycol 2000, and the mixing amount of the dispersing agent is 0.25-5% of the mass of the nano SiC;
the preparation method of the polycarbosilane and nano SiC powder mixed solution comprises the following steps: dissolving polycarbosilane in dimethylbenzene or normal hexane, adding nano SiC powder with the particle size of 10-200 nm, and uniformly mixing to obtain a mixture of the polycarbosilane and the nano SiC powder, wherein the mass ratio of the polycarbosilane to the dimethylbenzene or the normal hexane is 1:1-3;
the impregnation treatment includes: and standing the second blank in the nano SiC ceramic suspension or the mixture of the polycarbosilane and the nano SiC powder, vacuumizing to 10-100 Pa, controlling the infiltration time to be 0.5-5 h, and drying after the infiltration is finished to remove the solvent, wherein the drying temperature is 60-100 ℃ and the time is more than 8 hours.
In the step S5, sintering treatment is carried out in an atmosphere furnace; when the infiltration liquid is nano SiC ceramic suspension, the sintering process includes: heating to 1200-1600 ℃ at 10-20 ℃/min under argon atmosphere, heating to 1800-2100 ℃ at 5-10 ℃/min, preserving heat for 1-12 h, sintering, and cooling to room temperature at 5-10 ℃/min;
when the impregnating solution is a mixed solution of polycarbosilane and nano SiC powder, the sintering treatment comprises the following steps: under the argon atmosphere, heating to 1100-1300 ℃ at 1-5 ℃/min, preserving heat for 1-3 h, carrying out pyrolysis treatment on polycarbosilane, heating to 1800-2100 ℃ at 5-10 ℃/min, preserving heat for 1-12 h, carrying out high-temperature sintering, and cooling to room temperature at 5-10 ℃/min.
The further technical scheme includes that the step S6 is carried out in an infiltration furnace, and the step S6 includes: vacuumizing the infiltration furnace to below 10Pa, heating to 650-800 ℃ at 5-10 ℃/min, preserving heat for 5-10 min, introducing high-purity nitrogen or argon to 1-4 MPa, preserving heat for 30-120 min, and cooling to room temperature at 5-10 ℃/min.
In a second aspect, the present application provides a silicon carbide-aluminium composite material prepared by the method of the first aspect.
By the technical scheme of the application, the following beneficial effects can be brought:
1. in the powder preparation stage, nano-micron silicon carbide powder and sintering aid are adopted, and the powder is prepared through a spray granulation method, so that the powder has good fluidity, good sintering activity and the strength of a degreased blank body is improved.
2. The silicon carbide blank sprayed and printed by the binder is impregnated with the nano SiC ceramic suspension or the mixture of the polycarbosilane and the nano SiC powder, so that the compactness of the silicon carbide ceramic is improved, the sintering is promoted, and meanwhile, the pyrolysis process is avoided; in addition, when the mixture liquid of the polycarbosilane and the nano SiC powder is impregnated, due to the addition of nano SiC particles, the generation of thermal stress in the pyrolysis process is relieved and reduced, and the blank body is prevented from being damaged.
3. The ceramic sample is prepared by using the binder jet 3D printing technology, so that the ceramic component with large size, complex shape and silicon carbide is easier to prepare, a die is not needed, the cost is low, the period is short, and further, the density and the thermal conductivity and the mechanical property of the ceramic component can be improved by aluminizing.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely, and it is apparent that the described embodiments are some, but not all, embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
Example 1
The embodiment of the application provides a preparation method of a first binder jet printing silicon carbide-aluminum composite material, which comprises the following specific steps:
1. 85 parts by weight of silicon carbide powder with the grain diameter of 0.2 mu m and 10 parts by weight of Al with the grain diameter of 0.2 mu m are weighed 2 O 3 5 parts by weight of Y having a particle diameter of 0.5 μm 2 O 3 Absolute ethyl alcohol is adopted as a dispersing solvent, ball milling is carried out for 3 hours at the rotating speed of 250rpm, the mixture is uniformly mixed, then the mixture is dried for 6 hours at the temperature of 60 ℃ and then passes through a 50-mesh screen, and finally, the spherical silicon carbide granulating powder with the average particle size of 35 mu m is prepared through spray granulation.
2. Placing the 35 mu m silicon carbide spherical granulating powder obtained in the step 1 into a model exone invent+ printer, and setting printing parameters as follows: the thickness of the printed layer was set to 90 μm, the doctor blade speed was set to 3cm/s, and the glue saturation was 80%, to prepare a first green body. The printed structure is a square of 5cm by 10 cm.
3. Removing residual powder from the first blank, curing the first blank at 180 ℃ for 0.5h, and degreasing the cured first blank in air, wherein the method specifically comprises the following steps of: heating to 500 ℃ at 2 ℃/min, keeping the temperature for 3 hours, and then cooling to room temperature at 2 ℃/min to obtain a second blank.
4. Placing the second blank in a mixed solution of polycarbosilane and nano SiC powder, vacuumizing to 100Pa, and impregnating for 0.5h, wherein the preparation method of the mixed solution of polycarbosilane and nano SiC powder comprises the following steps: dissolving polycarbosilane in n-hexane, adding nano SiC powder with the particle size of 50nm, and uniformly mixing to obtain a mixture of the polycarbosilane and the nano SiC powder, wherein the mass ratio of the polycarbosilane to the n-hexane is 1:2, and the doping amount of the nano SiC powder is 5% (relative to the mass of the polycarbosilane); and then placing the impregnated second blank body in a baking oven at 60 ℃ for baking for 12 hours to remove the n-hexane, and obtaining a third blank body.
5. And (3) placing the third blank in an atmosphere furnace, heating to 1100 ℃ at 2 ℃/min, preserving heat for 2 hours, carrying out pyrolysis treatment on polycarbosilane, heating to 1850 ℃ at 5 ℃/min, preserving heat for 2 hours, carrying out high-temperature sintering, and cooling to room temperature at 10 ℃/min, wherein argon is selected as a protective atmosphere in the whole process, and obtaining the silicon carbide ceramic sintered body with 86% density.
6. Placing the silicon carbide ceramic sintered body and the aluminum block into an infiltration furnace, vacuumizing the high-temperature furnace to below 10Pa, heating to 750 ℃ at 10 ℃/min, preserving heat for 10min, then introducing high-purity nitrogen to 3MPa, preserving heat for 60min continuously, and cooling to room temperature at 10 ℃/min.
The density of the silicon carbide-aluminum composite material prepared in the embodiment is 98.3% measured by an Archimedes drainage method, the bending strength of the silicon carbide-aluminum composite material prepared in the embodiment is 420.2+/-16.8 MPa and the fracture toughness is 6.21+/-0.34 MPa.m measured by a three-point bending resistance method 1/2 The thermal conductivity was 180.2 W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has higher density and excellent thermo-mechanical property.
Example 2
The embodiment of the application provides a preparation method of a first binder jet printing silicon carbide-aluminum composite material, which comprises the following specific steps:
1. 90 parts by weight of silicon carbide powder with the grain diameter of 0.2 mu m and 5 parts by weight of B with the grain diameter of 0.2 mu m are weighed 4 C and 5 parts by weight of C with the particle size of 1 mu m, adopting absolute ethyl alcohol as a dispersing solvent, firstly carrying out ball milling for 3 hours at the rotating speed of 250rpm, uniformly mixing, then drying for 6 hours at the temperature of 60 ℃, then passing through a 50-mesh screen, and finally carrying out spray granulation to obtain the silicon carbide spherical granulating powder with the average particle size of 30 mu m.
2. Placing the 30 mu m silicon carbide spherical granulating powder obtained in the step 1 into a printer with the model of exone invent+ and setting printing parameters as follows: the thickness of the printed layer was set to 90 μm, the doctor blade speed was set to 3cm/s, and the glue saturation was 80%, to prepare a first green body. The printed structure is a square of 5cm by 10 cm.
3. Removing residual powder from the first blank, curing the first blank at 180 ℃ for 0.5h, and degreasing the cured first blank in air, wherein the method specifically comprises the following steps of: heating to 500 ℃ at 2 ℃/min, keeping the temperature for 3 hours, and then cooling to room temperature at 2 ℃/min to obtain a second blank.
4. Placing the second blank in a mixed solution of polycarbosilane and nano SiC powder, vacuumizing to 100Pa, and impregnating for 0.5h, wherein the preparation method of the mixed solution of polycarbosilane and nano SiC powder comprises the following steps: dissolving polycarbosilane in n-hexane, adding nano SiC powder with the particle size of 50nm, and uniformly mixing to obtain a mixture of the polycarbosilane and the nano SiC powder, wherein the mass ratio of the polycarbosilane to the n-hexane is 1:2, and the doping amount of the nano SiC powder is 5% (relative to the mass of the polycarbosilane); and then placing the impregnated second blank body in a baking oven at 60 ℃ for baking for 12 hours to remove the n-hexane, and obtaining the silicon carbide blank body 3.
5. And (3) placing the third blank in an atmosphere furnace, heating to 1200 ℃ at 2 ℃/min, preserving heat for 2 hours, carrying out pyrolysis treatment on polycarbosilane, heating to 1900 ℃ at 5 ℃/min, preserving heat for 2 hours, carrying out high-temperature sintering, and cooling to room temperature at 10 ℃/min, wherein argon is selected as a protective atmosphere in the whole process, and obtaining the silicon carbide ceramic sintered body with the density of 81%.
6. Placing the silicon carbide ceramic sintered body and the aluminum block into an infiltration furnace, vacuumizing the high-temperature furnace to below 10Pa, heating to 750 ℃ at 10 ℃/min, preserving heat for 10min, then introducing high-purity nitrogen to 3MPa, preserving heat for 60min continuously, and cooling to room temperature at 10 ℃/min.
The density of the silicon carbide-aluminum composite material prepared in the embodiment is 99.3% measured by an Archimedes drainage method, the bending strength of the silicon carbide-aluminum composite material prepared in the embodiment is 370.6+/-25.1 MPa and the fracture toughness is 7.62+/-0.42 MPa.m measured by a three-point bending resistance method 1/2 The thermal conductivity was 190.8W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has higher density and excellent thermo-mechanical property.
Example 3
The embodiment of the application provides a preparation method of a first binder jet printing silicon carbide-aluminum composite material, which comprises the following specific steps:
1. 80 parts by weight of silicon carbide powder with the grain diameter of 1 mu m and 5 parts by weight of Al with the grain diameter of 0.2 mu m are weighed 2 O 3 5 parts by weight of Y having a particle diameter of 0.5 μm 2 O 3 5 parts by weight of MgO with the grain size of 0.5 mu m and 5 parts by weight of CaO with the grain size of 1 mu m are uniformly mixed by adopting absolute ethyl alcohol as a dispersion solvent and ball milling time of 3 hours at the rotating speed of 350rpm, then are dried for 6 hours at the temperature of 60 ℃ and then pass through a 50-mesh screen, and finally are subjected to spray granulation to obtain the silicon carbide spherical granulating powder with the average grain size of 30 mu m.
2. Placing the 30 mu m silicon carbide spherical granulating powder obtained in the step 1 into a printer with the model of exone invent+ and setting printing parameters as follows: the thickness of the printed layer was set to 90 μm, the doctor blade speed was set to 3cm/s, and the glue saturation was 80%, to prepare a first green body. The printed structure is a square of 5cm by 10 cm.
3. Removing residual powder from the first blank, curing the first blank at 180 ℃ for 0.5h, and degreasing the cured first blank in air, wherein the method specifically comprises the following steps of: heating to 500 ℃ at 2 ℃/min, keeping the temperature for 3 hours, and then cooling to room temperature at 2 ℃/min to obtain a second blank.
4. Placing the second blank body in a nano SiC suspension with the concentration of 30vol%, vacuumizing to 100Pa, and impregnating for 0.5h, wherein the nano SiC ceramic suspension is a mixed solution of nano SiC, a solvent and a dispersing agent, the solvent of the nano SiC suspension is deionized water, the dispersing agent is polyethylene glycol 2000, and the doping amount of the dispersing agent is 1% of the mass of the nano SiC. And then placing the impregnated blank body in a 60 ℃ oven for drying for 24 hours to remove deionized water, and obtaining a third blank body.
5. And (3) placing the third blank in an atmosphere furnace, heating to 1600 ℃ at 15 ℃/min, then heating to 1750 ℃ at 5 ℃/min, preserving heat for 3 hours, performing high-temperature sintering, and cooling to room temperature at 10 ℃/min, wherein argon is selected as a protective atmosphere in the whole process, and obtaining the silicon carbide sintered body with the density of 88.7%.
6. Placing the silicon carbide ceramic sintered body and the aluminum block into an infiltration furnace, vacuumizing the infiltration furnace to below 10Pa, heating to 750 ℃ at 10 ℃/min, preserving heat for 10min, then introducing high-purity nitrogen to 3MPa, preserving heat for 60min, and then cooling to room temperature at 10 ℃/min.
The density of the silicon carbide-aluminum composite material prepared in the embodiment is 99.8% measured by an Archimedes drainage method, the bending strength of the silicon carbide-aluminum composite material prepared in the embodiment is 382.6+/-42.6 MPa and the fracture toughness is 8.28+/-0.36 MPa.m measured by a three-point bending resistance method 1/2 Thermal conductivity is 195.5 W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has higher density and excellent thermo-mechanical property.
Example 4
The embodiment of the application provides a preparation method of a first binder jet printing silicon carbide-aluminum composite material, which comprises the following specific steps:
1. 85 parts by weight of silicon carbide powder with the grain diameter of 0.2 mu m and 10 parts by weight of Al with the grain diameter of 0.2 mu m are weighed 2 O 3 5 parts by weight of Y having a particle diameter of 0.5 μm 2 O 3 Absolute ethyl alcohol is adopted as a dispersing solvent, ball milling is carried out for 3 hours at the rotating speed of 250rpm, the mixture is uniformly mixed, then the mixture is dried for 6 hours at the temperature of 60 ℃ and then passes through a 50-mesh screen, and finally, the spherical silicon carbide granulating powder with the average particle size of 35 mu m is prepared through spray granulation.
2. Placing the 35 mu m silicon carbide spherical granulating powder obtained in the step 1 into an exone inovent+ printer, and setting printing parameters as follows: the thickness of the printed layer was set to 90 μm, the doctor blade speed was set to 3cm/s, and the glue saturation was 80%, to prepare a first green body. The printed structure is a square of 5cm by 10 cm. 3. Removing residual powder from the first blank, curing the first blank at 180 ℃ for 0.5h, and degreasing the cured first blank in air, wherein the method specifically comprises the following steps of: heating to 500 ℃ at 2 ℃/min, keeping the temperature for 3 hours, and then cooling to room temperature at 2 ℃/min to obtain a second blank.
4. Placing the second blank body in a nano SiC suspension with the concentration of 30vol%, vacuumizing to 100Pa, and impregnating for 0.5h, wherein the nano SiC ceramic suspension is a mixed solution of nano SiC, a solvent and a dispersing agent, the solvent of the nano SiC suspension is deionized water, the dispersing agent is polyethylene glycol 2000, and the doping amount is 1% of the mass of the nano SiC. And then placing the impregnated second blank body in a baking oven at 60 ℃ for baking for 24 hours to remove deionized water, and obtaining a third blank body.
5. And (3) placing the third blank in an atmosphere furnace, heating to 1600 ℃ at 15 ℃/min, then heating to 1850 ℃ at 5 ℃/min, preserving heat for 3 hours, performing high-temperature sintering, and cooling to room temperature at 10 ℃/min, wherein argon is selected as a protective atmosphere in the whole process, and obtaining the silicon carbide ceramic sintered body with the density of 84.2%.
6. Placing the silicon carbide ceramic sintered body and the aluminum block into an infiltration furnace, vacuumizing the infiltration furnace to below 10Pa, heating to 750 ℃ at 10 ℃/min, preserving heat for 10min, then introducing high-purity nitrogen to 3MPa, preserving heat for 60min, and then cooling to room temperature at 10 ℃/min.
The density of the silicon carbide-aluminum composite material prepared in the embodiment is 99.6% measured by an Archimedes drainage method, the bending strength of the silicon carbide-aluminum composite material prepared in the embodiment is 405.3+/-35.6 MPa and the fracture toughness is 8.62+/-0.49 MPa.m measured by a three-point bending resistance method 1/2 A thermal conductivity of 203.5 W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has higher density and excellent thermo-mechanical property.
Example 5
Example 5 is a comparative example to example 1, with the other parameters being exactly the same process, except that: in the step 4, the degreased blank body 2 is placed in a mixed solution only filled with polycarbosilane, nano SiC is not added, the vacuum is pumped to 100Pa, and the mixture is impregnated for 0.5h, wherein in the polycarbosilane mixed solution, the polycarbosilane is as follows: the mass of the n-hexane is 1:2. After sintering, a silicon carbide sintered body having a density of 80.2% was obtained, and significant cracks were generated.
The density of the silicon carbide-aluminum composite material prepared by the embodiment is 95.3% measured by an Archimedes drainage method, and the bending strength of the silicon carbide-aluminum composite material prepared by the embodiment is 306.8 +/-56.3 MPa measured by a three-point bending resistance method, and the silicon carbide-aluminum composite material is brokenThe fracture toughness is 5.35+/-0.46 MPa.m 1/2 The thermal conductivity was 148.9W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has lower density and poorer thermo-mechanical property.
Example 6
Example 6 is a comparative example to example 4, the other parameters being exactly the same process, except that: example 6 step 4 of impregnating the nano SiC suspension was omitted and a silicon carbide sintered body having a density of 64.5% was obtained after sintering. This example illustrates that not doing the treatment of impregnating the SiC suspension is detrimental to improving the density of the silicon carbide sintered body.
The density of the silicon carbide-aluminum composite material prepared in the embodiment is 87.5% measured by an Archimedes drainage method, the bending strength of the silicon carbide-aluminum composite material prepared in the embodiment is 283.4 +/-35.7 MPa and the fracture toughness is 3.64+/-0.51 MPa.m measured by a three-point bending resistance method 1/2 The thermal conductivity was 78.4 W.m -1 ·K -1 The silicon carbide-aluminum composite material part prepared by the embodiment has lower density and poorer thermo-mechanical property.
Example 7
Example 7 is a comparative example to example 4, the other parameters being exactly the same process, except that: example 7 the step 6 of the aluminizing process was omitted, the density of the silicon carbide material obtained in the present example was 84.2% as measured by the Archimedes drainage method, the flexural strength of the silicon carbide material obtained in the present example was 170.5.+ -. 39.4MPa as measured by the three-point bending resistance method, and the fracture toughness was 3.05.+ -. 0.26 MPa.m 1/2 The thermal conductivity was 56.2 W.m -1 ·K -1 That is, it is explained that the silicon carbide material component prepared without infiltration of aluminum in this embodiment has lower density and poorer thermo-mechanical properties.
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
While the application has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the application. Therefore, the protection scope of the application is subject to the protection scope of the claims.
Claims (10)
1. A method for preparing a silicon carbide-aluminum composite material by binder jet printing, which is characterized by comprising the following steps:
s1, weighing silicon carbide powder, a sintering aid and a dispersing solvent to form a mixture, and sequentially performing ball milling, drying, sieving and spray granulation on the mixture to obtain silicon carbide spherical granulating powder;
s2, taking the silicon carbide spherical granulating powder as a printing raw material, and performing binder jet printing according to preset printing parameters and preset design structures to obtain a first blank;
s3, removing residual powder, curing and degreasing the first blank body to obtain a second blank body;
s4, impregnating the second blank in an impregnating solution to perform impregnating treatment, and drying to obtain a third blank, wherein the impregnating solution is nano SiC ceramic suspension or a mixture of polycarbosilane and nano SiC powder; the nano SiC ceramic suspension is a mixed solution of nano SiC, a solvent and a dispersing agent, and the concentration of the nano SiC in the nano SiC ceramic suspension is 10-40 vol%; in the mixed solution of the polycarbosilane and the nano SiC powder, the mass of the nano SiC powder is 5-15% of that of the polycarbosilane;
s5, sintering the third blank to obtain a silicon carbide ceramic sintered body;
s6, carrying out aluminizing in the silicon carbide sintered body to obtain the silicon carbide-aluminum composite material.
2. The method according to claim 1, wherein in step S1, 80 to 95 parts by mass of the silicon carbide powder and 5 to 20 parts by mass of the sintering aid are calculated; the grain diameter of the silicon carbide powder is 0.1-3 mu m; the sintering aid is Al 2 O 3 、Y 2 O 3 、MgO、CaO、TiO 2 、La 2 O 3 、AlN、B 4 C、C、SiO 2 The particle size of the sintering aid is 0.1-1 mu m, and the purity of the sintering aid is more than 99.5%; the dispersion solvent is at least one of deionized water, absolute ethyl alcohol and methanol.
3. The method according to claim 1, wherein in the step S1, the process parameters of the ball milling include a ball milling rotation speed of 200-400 rpm and a ball milling time of 0.5-6 h; the drying process parameters comprise the drying temperature of 50-120 ℃ and the drying time of 3-24 h; the number of the screening meshes is 50-100 meshes.
4. The method according to claim 1, wherein the silicon carbide spherical granulated powder has a particle diameter of 10 to 100 μm.
5. The method according to claim 1, wherein in step S2, the printing parameters include a printing layer thickness of 50-300 μm, a doctor blade speed of 1-6 cm/S, and a glue saturation of 50-100%.
6. The method according to claim 1, wherein in step S3, the process parameters of the curing process include: the curing temperature is 100-300 ℃, and the heat preservation time is 0.5-3 h; the degreasing treatment comprises the following steps: heating to 300-600 ℃ at 0.5-10 ℃/min under the air atmosphere, keeping the temperature for 1-6 h, and then cooling to room temperature at 0.5-10 ℃/min.
7. The method according to claim 1, wherein in the step S4, the nano SiC has a particle size of 10-200 nm, the solvent is at least one of deionized water, absolute ethyl alcohol, acetone and methanol, the dispersant is at least one of citric acid, oxalic acid, sodium acrylate, potassium acrylate, polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400 and polyethylene glycol 2000, and the mixing amount of the dispersant is 0.25-5% of the mass of the nano SiC;
the preparation method of the polycarbosilane and nano SiC powder mixed solution comprises the following steps: dissolving polycarbosilane in dimethylbenzene or normal hexane, adding nano SiC powder with the particle size of 10-200 nm, and uniformly mixing to obtain a mixture of the polycarbosilane and the nano SiC powder, wherein the mass ratio of the polycarbosilane to the dimethylbenzene or the normal hexane is 1:1-3;
the impregnation treatment includes: and standing the second blank in the nano SiC ceramic suspension or the mixture of the polycarbosilane and the nano SiC powder, vacuumizing to 10-100 Pa, controlling the infiltration time to be 0.5-5 h, and drying after the infiltration is finished, wherein the drying temperature is 60-100 ℃.
8. The method according to claim 1, wherein in step S5, the sintering process is performed in an atmosphere furnace; when the infiltration liquid is nano SiC ceramic suspension, the sintering process includes: heating to 1200-1600 ℃ at 10-20 ℃/min under argon atmosphere, heating to 1800-2100 ℃ at 5-10 ℃/min, preserving heat for 1-12 h, and cooling to room temperature at 5-10 ℃/min;
when the impregnating solution is a mixed solution of polycarbosilane and nano SiC powder, the sintering treatment comprises the following steps: under the argon atmosphere, the temperature is raised to 1100-1300 ℃ at 1-5 ℃/min, the heat is preserved for 1-3 h, the temperature is raised to 1800-2100 ℃ at 5-10 ℃/min, the heat is preserved for 1-12 h, and the temperature is lowered to the room temperature at 5-10 ℃/min.
9. The method of claim 1, wherein step S6 is performed in an infiltration furnace, step S6 comprising: vacuumizing the infiltration furnace to below 10Pa, heating to 650-800 ℃ at 5-10 ℃/min, preserving heat for 5-10 min, introducing high-purity nitrogen or argon to 1-4 MPa, preserving heat for 30-120 min, and cooling to room temperature at 5-10 ℃/min.
10. A silicon carbide-aluminium composite material, prepared by the method of any one of claims 1 to 9.
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