CN115286394A - Preparation method of silicon carbide ceramic material for binder jet printing - Google Patents
Preparation method of silicon carbide ceramic material for binder jet printing Download PDFInfo
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- CN115286394A CN115286394A CN202210900589.5A CN202210900589A CN115286394A CN 115286394 A CN115286394 A CN 115286394A CN 202210900589 A CN202210900589 A CN 202210900589A CN 115286394 A CN115286394 A CN 115286394A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 51
- 239000011230 binding agent Substances 0.000 title claims abstract description 41
- 238000007639 printing Methods 0.000 title claims abstract description 40
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 235000015895 biscuits Nutrition 0.000 claims abstract description 46
- 238000005238 degreasing Methods 0.000 claims abstract description 27
- 238000005507 spraying Methods 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 238000005475 siliconizing Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000013461 design Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005469 granulation Methods 0.000 claims abstract description 5
- 230000003179 granulation Effects 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 31
- 229910052799 carbon Inorganic materials 0.000 claims description 30
- 230000008569 process Effects 0.000 claims description 21
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 16
- 229920001568 phenolic resin Polymers 0.000 claims description 16
- 239000005011 phenolic resin Substances 0.000 claims description 16
- 238000005336 cracking Methods 0.000 claims description 14
- 238000007598 dipping method Methods 0.000 claims description 14
- 238000001723 curing Methods 0.000 claims description 13
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
- 239000007833 carbon precursor Substances 0.000 claims description 11
- 229930195733 hydrocarbon Natural products 0.000 claims description 11
- 150000002430 hydrocarbons Chemical class 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 11
- 235000021355 Stearic acid Nutrition 0.000 claims description 10
- 238000004132 cross linking Methods 0.000 claims description 10
- 238000005470 impregnation Methods 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 10
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 239000008117 stearic acid Substances 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000000280 densification Methods 0.000 claims description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 9
- 230000008595 infiltration Effects 0.000 claims description 9
- 238000001764 infiltration Methods 0.000 claims description 9
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 9
- 239000007849 furan resin Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 238000005255 carburizing Methods 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920003257 polycarbosilane Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 239000011295 pitch Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 description 20
- 238000005516 engineering process Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- 238000010146 3D printing Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 238000013001 point bending Methods 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000110 selective laser sintering Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 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
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000007648 laser printing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/573—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 obtained by reaction sintering or recrystallisation
-
- 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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention relates to a preparation method of a silicon carbide ceramic material for binder jet printing. The preparation method comprises the following steps: adding a dispersing agent, a high carbon residue binder and a solvent into a powder containing carbon powder serving as a raw material to be mixed to obtain slurry; drying the slurry or carrying out spray granulation to obtain composite powder with the particle size of 20-250 mu m; selecting a spraying binder and setting printing parameters by taking the composite powder as a printing raw material, and performing binder spraying printing according to the design structure of the silicon carbide ceramic material to obtain a biscuit of the silicon carbide ceramic material; degreasing the ceramic material biscuit at high temperature to obtain a degreased biscuit sample; and carrying out siliconizing sintering on the degreased biscuit sample to obtain the adhesive spray-printed silicon carbide ceramic material.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a preparation method of a silicon carbide ceramic material for binder jet printing.
Background
The silicon carbide ceramic (SiC) material has good thermal conductivity, corrosion resistance and chemical resistance, low thermal expansion rate and durability. The high-purity SiC product can keep stable at the high temperature of more than 1200 ℃, and can be widely applied to a semiconductor diffusion process, normal-pressure CVD, LP-CVD and the like; the high-toughness silicon carbide can be applied to the fields of cutting tools, springs, engine parts and the like. However, silicon carbide ceramics also have the characteristics of easy oxidation, high melting rate and high light absorption. Compared with plastics or metals, the ceramic material has a fixed melting point, can be pasted after being melted by heating, and has a high melting point particularly for oxide ceramics, while carbide ceramics have no melting point and can be directly oxidized under a high-temperature condition. Silicon carbide can be oxidized into silicon dioxide, or other gases or directly decomposed under the action of laser, so that 3D printing cannot be directly carried out, and only a biscuit is printed and then sintered.
Based on the characteristics, the preparation technology of the SiC ceramic and the composite material thereof combined with 3D printing becomes the main development direction of current research and application, and the 3D printing technology is an additive manufacturing technology which is completely different from the traditional material processing method. The 3D printing technology is based on three-dimensional digital model design, materials such as ceramic powder, resin, metal powder and the like are processed in a layering mode, stacked and bonded through a software layering discrete and numerical control forming system, and finally, a three-dimensional entity is manufactured through superposition forming. Compared with the traditional manufacturing method, the 3D printing technology saves raw materials, is easy to rapidly manufacture materials with complex structures, shortens the research and development period, and is more suitable for production of personalized products. The method is widely applied to the fields of biomedicine, tissue engineering, automobile parts, aerospace, micro-nano devices and the like.
At present, the method for 3D printing of SiC ceramics and composite materials thereof mainly comprises the following steps: fused Deposition Modeling (FDM), stereolithography (SL), layered Object Manufacturing (LOM), selective Laser Sintering (SLs), selective Laser Melting (SLM), direct write free forming (DIW), and the like. The FDM technology is low in printing speed and low in efficiency, and the forming precision is low; in the SL technology, because the silicon carbide powder has strong light absorption capacity, the silicon carbide powder must be modified, the requirements on organic binders are high, the cost is high, and only small-sized samples are printed at present; the LOM technology can only form face materials in a laminated mode, and the application range is small at present; the SLS technology has high requirements on equipment, and the solid content of the formed material is low; in the DIW technique, due to the existence of a large amount of solvent (water), the ceramic body is easy to crack in the drying process, and the large-size SiC ceramic material is not easy to prepare.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing a silicon carbide ceramic material by binder spray printing, so as to solve the problem that it is difficult to obtain a meter-level large-size complex-structure ceramic component in 3D printing manufacturing of high-precision complex-shape silicon carbide ceramic and its composite material.
Specifically, in a first aspect, the present invention provides a method for preparing a silicon carbide ceramic material for binder spray printing, comprising:
adding a dispersing agent, a high carbon residue binder and a solvent into the powder containing carbon as a raw material powder, and mixing to obtain slurry; drying the slurry or carrying out spray granulation to obtain composite powder with the particle size of 20-250 mu m;
selecting a spraying binder and setting printing parameters by taking the composite powder as a printing raw material, and performing binder spraying printing according to the design structure of the silicon carbide ceramic material to obtain a biscuit of the silicon carbide ceramic material;
degreasing the ceramic material biscuit at high temperature to obtain a degreased biscuit sample;
and carrying out siliconizing sintering on the degreased biscuit sample to obtain the adhesive spray-printed silicon carbide ceramic material.
Preferably, the carbon-containing powder is carbon powder, chopped carbon fiber powder, a mixed powder composed of carbon powder and chopped carbon fiber powder, or a mixed powder composed of carbon powder and/or chopped carbon fiber powder and silicon carbide powder.
Preferably, the dispersant comprises one or more of Stearic Acid (SA), n-butanol, polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB), sodium Dodecyl Sulfate (SDS), or Sodium Dodecyl Benzene Sulfonate (SDBS); the addition amount of the dispersant is controlled to be 0.1 to 0.5 weight percent of the mass of the carbon-containing powder.
Preferably, the high residual carbon binder comprises one or more of phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethyl methacrylate (PMMA), or epoxy resin; the addition amount of the binder is controlled to be 5-10 wt% of the mass of the carbon-containing powder.
Preferably, the solid content of the slurry obtained after ball milling is controlled to be 40 to 50wt%, preferably 40 to 45wt%.
Preferably, the spray binder is selected from a mixture of one or more of furan resin, phenolic resin, or pitch resin.
Preferably, the printing parameters include: the spraying amount of the adhesive is 75-85%, the spraying and scanning speed is 0.4-1 m/s, and the scanning distance is 0.1-0.5 mm; the thickness of the printed layer is controlled to be 0.1-0.5 mm.
Preferably, the degreasing temperature is controlled to be not higher than 1200 ℃, and is preferably 900-1100 ℃; the degreasing time is 12-48 h.
Preferably, the temperature of the siliconizing sintering is 1450-1750 ℃ and the time is 60-120 minutes.
Preferably, the preparation method further comprises at least one densification treatment after degreasing and before siliconizing and sintering; the densification treatment process comprises the following steps: high carbon residue solution impregnation treatment and/or chemical vapor infiltration treatment.
Preferably, the high carbon residue solution impregnation treatment process comprises the following steps: putting the degreased biscuit sample into a carbon precursor solution with high residual carbon content for dipping, crosslinking and curing; then, converting the carbon precursor into cracked carbon through high-temperature cracking; repeating the processes of dipping, curing and cracking to obtain a biscuit sample after carburization; wherein the carbon precursor with high residual carbon content is at least one of phenolic resin, pitch resin, sucrose, furan resin or polycarbosilane resin; the time for dipping, crosslinking and curing is 12-36h, preferably 24h; the high-temperature cracking temperature is 900-1100 ℃, and the time is 1-2h; the number of times of repeating the dipping-curing-cracking process is 1-4 times.
Preferably, the chemical vapor infiltration treatment process comprises the following steps: at least one hydrocarbon gas is adopted as a carburizing medium, and the hydrocarbon gas is converted into carbon after high-temperature decomposition and polycondensation and is deposited in a porous degreased biscuit to obtain a biscuit sample after carburization; wherein the vapor infiltration treatment is carried out in a chemical vapor deposition device; controlling the flow rate of the hydrocarbon gas to be 200-300mL/min; the high-temperature decomposition and polycondensation temperature is 1000-1300 deg.C, and the time is 1-7 days.
In a second aspect, the invention provides a binder-jet-printed silicon carbide ceramic material obtained according to the preparation method.
Advantageous effects
The binder jet printing process provided by the invention comprises the following steps: (1) The silicon carbide ceramic and the composite material thereof with the magnitude of more than 2m can be manufactured; (2) The silicon carbide ceramic and the composite material thereof with the precision of 0.1mm can be manufactured; (3) The manufacture of the silicon carbide ceramic with the complex hollow structure and the composite material thereof can be realized.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative, and not a limitation of the present invention.
The adhesive jet printing technology (BJP) is a general Additive Manufacturing (AM) technology, and the printing process of the adhesive jet technology is to jet a liquid adhesive through a nozzle with the diameter of less than 50 micrometers to selectively bond powder in a thin layer, and the bonding process is repeated layer by layer. The principle of the technology is chemical reaction solidification, the material can be formed without heating in the spraying process, products with high precision and complex shapes can be manufactured by adopting various powder materials (metal, ceramic or polymer and the like), and the technology is suitable for 3D printing forming of silicon carbide ceramics with large size, high precision and complex shapes and composite materials thereof.
The laser printing layer-by-layer scanning is relatively easy to generate the defect of thermal stress caused by temperature gradient in the powder, the binder is sprayed and printed to simultaneously bond the powder in a large area, the stress is relatively small, the equipment is easy to realize large-scale, a printing support structure is not needed in the printing process, and the overall cost of the equipment is low.
The following is an exemplary description of a preparation method of the binder-jet printing silicon carbide ceramic material of the present invention, which mainly comprises the following steps.
(1) Preparing a powder raw material. Taking a carbon-containing powder as a raw material powder, adding a dispersing agent, a high-carbon-residue binder and a solvent, mixing, and performing ball milling to obtain slurry; drying the slurry or carrying out spray granulation to obtain the composite powder with good fluidity and the particle size of 20-250 mu m. The composite powder has small particle size and is easy to bond, so that the flowability is poor and the powder is inconvenient to spread; an excessively large particle size of the powder results in a decrease in reactivity and also in poor flowability.
The carbon-containing powder can be carbon powder, short carbon fiber powder, mixed powder consisting of carbon powder and short carbon fiber powder, or mixed powder consisting of carbon powder and/or short carbon fiber powder and silicon carbide powder. The content of the silicon carbide powder is more than 0 and less than 100wt% in the mixed powder consisting of the carbon powder and/or the chopped carbon fiber powder and the silicon carbide powder. In some embodiments, the particle size of the carbon powder can be controlled to be 0.1-1um; the length of the carbon fiber powder is 20-50 μm, the diameter is 3-5 μm, and the length-diameter ratio is 4-15; the grain diameter of the silicon carbide powder is 0.2-200um.
In some embodiments, the dispersant may include one or more of Stearic Acid (SA), n-butanol, polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB), sodium Dodecyl Sulfate (SDS), or Sodium Dodecyl Benzene Sulfonate (SDBS); the addition amount of the dispersant can be controlled to be 0.1 to 0.5 weight percent of the carbon powder containing quality. The dosage of the dispersant is too small, and a better powder dispersion effect cannot be achieved; if the amount of the dispersant is too much, the gas generated in the subsequent degreasing process is too much, and pores are easily generated in the ceramic body.
In some embodiments, the high carbon residue binder comprises one or more of phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethylmethacrylate (PMMA), or epoxy resin; the addition amount of the binder can be controlled to be 5-10 wt% of the carbon powder (5-10% of the binder when the powder is 100).
The solvent may be water or ethanol. The ball milling parameters can be as follows: taking SiC balls as grinding balls, wherein the ball-milling rotating speed is 300-1000rpm, and the ball-milling time is 12-24h. Preferably, the solid content of the slurry obtained after ball milling can be controlled to be 40 to 50wt%, preferably 40 to 45wt%. The solid content is too low, and powder in the slurry is easy to settle; too high a solids content can make subsequent spray granulation difficult.
(2) And (4) adhesive jet printing. Taking the composite powder prepared in the step (1) as a printing raw material, selecting one or a mixture of more of furan resin, phenolic resin and asphalt resin as a spraying binder, and setting printing parameters: the spraying amount of the adhesive is 75-85%, the spraying scanning speed is 0.4-1 m/s, and the scanning interval is 0.1-0.5 mm. The binder spraying amount is the ratio of the volume occupied by the binder solution in the powder gap to the pore volume. And (4) carrying out binder jet printing according to the design structure of the silicon carbide ceramic material to obtain the silicon carbide ceramic material biscuit with a complex shape. In some embodiments, the printed layer thickness can be controlled to be 0.1 to 0.5mm.
(3) And (6) degreasing. And (3) carrying out high-temperature degreasing on the ceramic material biscuit obtained by the adhesive jet printing in the step (2) to obtain a degreased biscuit sample. Wherein, the degreasing temperature is controlled to be not higher than 1200 ℃, and is preferably 900-1100 ℃; the degreasing time is 12-48 h.
In some embodiments, the porosity of the degreased biscuit sample can be controlled to be 40% to 80%, preferably 60% to 80%; the pore size distribution is 0.01-20 μm, preferably 0.05-20 μm; the density is 0.4 to 1.6g/cm 3 Preferably 0.4 to 1.3g/cm 3 (ii) a The equivalent carbon density is 0.40-0.96 g/cm 3 Preferably 0.40 to 0.84g/cm 3 。
(4) And (5) siliconizing and sintering. Placing the degreased biscuit sample obtained in the step (3) at 1450-1750 ℃ for siliconizing for 60-120 minutes to obtain the biscuit with the density of 2.70-3.10 g/cm 3 The high-density silicon carbide ceramic material.
In some embodiments, according to the material performance requirement, the degreased biscuit sample obtained in step (3) may be subjected to high carbon residue solution immersion treatment and/or chemical vapor infiltration treatment, and then subjected to high temperature degreasing again, so as to increase the density of the sample. At least one densification treatment is carried out between degreasing and siliconizing sintering, and the steps can be repeated as required.
The specific process of the high carbon residue solution impregnation treatment can be as follows: putting the degreased biscuit sample into a carbon precursor solution with high residual carbon content for dipping, crosslinking and curing; then, converting the carbon precursor into cracked carbon through high-temperature cracking; and repeating the processes of dipping, curing and cracking to obtain the biscuit sample after carburization. Wherein the carbon precursor with high residual carbon content can be at least one of phenolic resin, pitch resin, sucrose, furan resin or polycarbosilane resin; the time for the impregnation and crosslinking curing can be 12-36h, preferably 24h; the high-temperature cracking temperature can be 900-1100 ℃, and the time can be 1-2h; the number of times the impregnation-curing-cracking process is repeated may be 1 to 4 times.
The specific process of the chemical vapor infiltration treatment can be as follows: at least one hydrocarbon gas is used as a carburizing medium, and the hydrocarbon gas is converted into carbon and deposited in the porous degreased biscuit after pyrolysis and polycondensation to obtain a biscuit sample after carburization. Wherein the vapor infiltration treatment can be carried out in a chemical vapor deposition apparatus; the hydrocarbon gas is selected from at least one of hydrocarbon gas compounds; controlling the flow rate of the hydrocarbon gas to be 200-300mL/min; the high-temperature decomposition and polycondensation temperature is 1000-1300 deg.C, and the time is 1-7 days.
The silicon carbide ceramic material prepared by the preparation method provided by the invention comprises the following steps: the relative density is more than or equal to 99 percent; the silicon content is 10-58 vol%; the density is 2.70-3.10 g/cm 3 (ii) a The three-point bending strength is 200-460 MPa; the elastic modulus is 200-400 GPa; fracture toughness of 2.0-4.0 MPam 1/2 (ii) a The thermal conductivity is 110-200W/mK; coefficient of thermal expansion (RT-400) 3.0-4.0X 10 -6 。
The present invention will be described in detail by way of examples. It should also be understood that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adjustments made by those skilled in the art in light of the above disclosure are within the scope of the present invention, and that the specific process parameters and the like described in the following examples are only examples of suitable ranges, i.e., those skilled in the art can select from the suitable ranges described herein, and are not intended to be limited to the specific values listed below.
Example 1
(1) Preparing a powder raw material. Adding the powder C into Sodium Dodecyl Benzene Sulfonate (SDBS), phenolic resin and an alcohol solvent, mixing, and performing ball milling to obtain slurry; spraying and granulating the slurry to obtain composite powder with the particle size of 100um and good fluidity; wherein the mass of the C powder is 100g, the addition amount of the SDBS is 0.2wt% (0.2 g) of the C powder, the addition amount of the binder phenolic resin is 10wt% (10 g) of the C powder, and the solid content of the slurry is 45wt%.
(2) And (4) adhesive jet printing. Taking the composite powder prepared in the step (1) as a printing raw material, selecting furan resin as a spraying binder, and setting printing parameters: the binder spraying amount was 80%, the spraying scanning speed was 0.5m/s, and the scanning pitch was 0.4mm. Carrying out binder jet printing according to the design structure of the silicon carbide ceramic composite material to obtain a silicon carbide ceramic material biscuit with a complex shape; wherein the printed layer thickness is 0.2mm.
(3) And (6) degreasing. And (3) degreasing the ceramic biscuit obtained by the adhesive jet printing in the step (2) at high temperature to obtain a degreased biscuit sample. Wherein the degreasing temperature is 1200 ℃, and the degreasing time is 24h; the obtained sample had a porosity of 78%, an average pore diameter of 3 μm and an equivalent carbon density of 0.40g/cm 3 。
(4) And (5) siliconizing and sintering. And (4) placing the degreased biscuit sample obtained in the step (3) at 1550 ℃ for siliconizing for 60 minutes to obtain the high-density silicon carbide ceramic material.
Through tests, the silicon carbide ceramic material obtained in the embodiment has the following characteristics: the relative density is more than or equal to 99 percent; silicon content 58vol%; density 2.70g/cm 3 (ii) a The three-point bending strength is 210MPa; the elastic modulus is 220GPa; fracture toughness 2.0MPam 1/2 (ii) a The thermal conductivity is 120W/mK; coefficient of thermal expansion (RT-400) 4.0X 10 -6 。
Example 2
Steps (1) to (3) were conducted in example 1.
(4) And (4) dipping. Putting the degreased biscuit sample into alcohol solution of phenolic resin for dipping, crosslinking and curing; and then, converting the carbon precursor into cracked carbon through high-temperature cracking to obtain the biscuit sample subjected to carburization. Wherein the volume ratio of the phenolic resin to the alcohol is 1:1; the time for dipping, crosslinking and curing is 24h; the pyrolysis temperature is 1000 ℃ and the time is 1h. After the impregnation is finished, the degreasing operation in the step (3) is carried out again, and the obtained sample has the porosity of 60 percent, the average pore diameter of 0.85um and the equivalent carbon density of 0.60g/cm 3 。
(5) And (5) siliconizing and sintering. And (4) placing the degreased biscuit sample obtained in the step (4) at 1600 ℃ for siliconizing for 120 minutes to obtain the high-density silicon carbide ceramic material.
Through tests, the silicon carbide ceramic material obtained in the embodiment has the following characteristics: the relative density is more than or equal to 99 percent; silicon content 38vol%; density 2.88g/cm 3 (ii) a The three-point bending strength is 250MPa; the elastic modulus is 230GPa; fracture toughness 2.2MPam 1/2 (ii) a The thermal conductivity is 160W/mK; coefficient of thermal expansion (RT-400) 4.0X 10 -6 。
Example 3
Steps (1) to (3) were conducted in accordance with example 2.
(4) And (4) dipping. The first densification treatment was the same as in example 2; after the first densification treatment, the impregnation in the step (4) and the degreasing in the step (3) are carried out again, and the porosity of the sample obtained after the second densification treatment is 46%, the average pore diameter is 0.35um, and the equivalent carbon density is 0.84g/cm 3 。
(5) And (5) siliconizing and sintering. And (4) placing the degreased biscuit sample obtained in the step (4) at 1750 ℃ for siliconizing for 60 minutes to obtain the high-density silicon carbide ceramic material.
Through tests, the silicon carbide ceramic material obtained in the embodiment has the following characteristics: the relative density is more than or equal to 99 percent; silicon content 10vol%; density 3.10g/cm 3 (ii) a The three-point bending strength is 450MPa; the elastic modulus is 400GPa; fracture toughnessSex 2.5MPam 1/2 (ii) a The thermal conductivity is 170W/mK; coefficient of thermal expansion (RT-400) 4.0X 10 -6 。
Example 4
(1) Preparing a powder raw material. Adding stearic acid SA, phenolic resin and an alcohol solvent into the C powder and the SiC powder, mixing, and performing ball milling to obtain slurry; spraying and granulating the slurry to obtain composite powder with the particle size of 100 mu m and good fluidity; wherein the content of the C powder is 45wt%, the content of the silicon carbide powder is 55w%, the total mass of the C powder and the silicon carbide powder is 100g, the addition amount of the dispersant stearic acid SA is 0.2wt% (0.2 g) of the total mass of the powder, the addition amount of the binder is 10wt% (10 g) of the total mass of the powder, and the solid content of the slurry is 45wt%.
(2) And (4) adhesive jet printing. Taking the composite powder prepared in the step (1) as a printing raw material, selecting furan resin as a spraying binder, and setting printing parameters: the binder spraying amount was 85%, the spraying scanning speed was 0.4m/s, and the scanning pitch was 0.5mm. Carrying out binder jet printing according to the design structure of the silicon carbide ceramic and the composite material thereof to obtain a silicon carbide ceramic biscuit with a complex shape; wherein the printed layer thickness is 0.5mm.
(3) And (6) degreasing. And (3) carrying out high-temperature degreasing on the ceramic biscuit obtained by the adhesive jet printing in the step (2) to obtain a degreased biscuit sample. Wherein the degreasing temperature is 1200 ℃, and the degreasing time is 12h; the obtained sample had a porosity of 58%, a pore diameter of 5 μm, and a density of 1.15g/cm 3 。
(4) And (4) dipping. Putting the degreased biscuit sample into alcohol solution of phenolic resin for dipping, crosslinking and curing; and then, converting the carbon precursor into cracked carbon through high-temperature cracking to obtain a carburized biscuit sample. Wherein the volume ratio of the phenolic resin to the alcohol is 1:1; the time for dipping, crosslinking and curing is 24h; the pyrolysis temperature is 1100 ℃, and the time is 1h. After the impregnation is finished, the degreasing operation in the step (3) is carried out again, the porosity of the obtained sample is 48 percent, the average pore diameter is 0.75um, and the density of the sample is 1.40g/cm 3 . The second densification is carried out again in the steps (4) and (3) to obtain a sample with the porosity of 40 percent, the average pore diameter of 0.50um and the density of 1.60g/cm 3 Equivalent carbon densityThe degree is 0.82g/cm 3 。
(5) And (5) siliconizing and sintering. And (5) carrying out siliconizing treatment on the degreased biscuit sample obtained in the step (4) at 1600 ℃ for 120 minutes to obtain the high-density silicon carbide ceramic material.
Through tests, the silicon carbide ceramic material obtained in the embodiment has the following characteristics: the relative density is more than or equal to 99 percent; silicon content 15vol%; density 3.08g/cm 3 (ii) a The three-point bending strength is 430MPa; the elastic modulus is 350GPa; fracture toughness 2.3MPam 1/2 (ii) a The thermal conductivity is 160W/mK; coefficient of thermal expansion (RT-400) 4.0X 10 -6 。
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (13)
1. A preparation method of a silicon carbide ceramic material for binder jet printing is characterized by comprising the following steps:
adding a dispersing agent, a high carbon residue binder and a solvent into the powder containing carbon as a raw material powder, and mixing to obtain slurry; drying the slurry or carrying out spray granulation to obtain composite powder with the particle size of 20-250 mu m;
selecting a spraying binder and setting printing parameters by taking the composite powder as a printing raw material, and performing binder spraying printing according to the design structure of the silicon carbide ceramic material to obtain a biscuit of the silicon carbide ceramic material;
degreasing the ceramic material biscuit at high temperature to obtain a degreased biscuit sample;
and carrying out siliconizing sintering on the degreased biscuit sample to obtain the adhesive spray-printed silicon carbide ceramic material.
2. The preparation method according to claim 1, wherein the carbon-containing powder is carbon powder, chopped carbon fiber powder, a mixed powder of carbon powder and chopped carbon fiber powder, or a mixed powder of carbon powder and/or chopped carbon fiber powder and silicon carbide powder.
3. The method according to claim 1 or 2, wherein the dispersant comprises one or more of Stearic Acid (SA), n-butanol, polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB), sodium Dodecyl Sulfate (SDS), or Sodium Dodecylbenzenesulfonate (SDBS); the addition amount of the dispersant is controlled to be 0.1 to 0.5 weight percent of the mass of the carbon-containing powder.
4. The method of any one of claims 1-3, wherein the high carbon residue binder comprises one or more of phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethyl methacrylate (PMMA), or epoxy resin; the addition amount of the binder is controlled to be 5-10 wt% of the mass of the carbon-containing powder.
5. The method according to any one of claims 1 to 4, wherein the slurry obtained after ball milling has a solids content of 40 to 50 wt.%, preferably 40 to 45 wt.%.
6. The method of any one of claims 1-5, wherein the spray binder is selected from a mixture of one or more of furan resin, phenolic resin, or pitch resin.
7. The production method according to any one of claims 1 to 6, wherein the printing parameters include: the spraying amount of the adhesive is 75-85%, the spraying and scanning speed is 0.4-1 m/s, and the scanning distance is 0.1-0.5 mm; the thickness of the printed layer is controlled to be 0.1-0.5 mm.
8. The method according to any one of claims 1 to 7, wherein the degreasing temperature is controlled to be not higher than 1200 ℃, preferably 900 to 1100 ℃; the degreasing time is 12 to 48h.
9. The preparation method according to any one of claims 1 to 8, wherein the siliconizing sintering temperature is 1450 to 1750 ℃ and the time is 60 to 120 minutes.
10. The production method according to any one of claims 1 to 9, further comprising at least one densification treatment after degreasing and before siliconizing sintering; the densification treatment process comprises the following steps: high carbon residue solution impregnation treatment and/or chemical vapor infiltration treatment.
11. The preparation method according to claim 10, wherein the high carbon residue solution impregnation treatment process comprises: putting the degreased biscuit sample into a carbon precursor solution with high residual carbon content for dipping, crosslinking and curing; then, converting the carbon precursor into cracked carbon through high-temperature cracking; repeating the processes of dipping, curing and cracking to obtain a biscuit sample after carburization; wherein the carbon precursor with high residual carbon content is at least one of phenolic resin, pitch resin, sucrose, furan resin or polycarbosilane resin; the time for the impregnation and crosslinking curing is 12-36h, and is preferably 24h; the high temperature cracking temperature is 900-1100 deg.C, and the time is 1-2h; the number of times of repeating the dipping-curing-cracking process is 1 to 4 times.
12. The preparation method according to claim 10, wherein the chemical vapor infiltration treatment process comprises the following steps: at least one hydrocarbon gas is used as a carburizing medium, and the hydrocarbon gas is converted into carbon and deposited in the porous degreased biscuit after pyrolysis and polycondensation to obtain a biscuit sample after carburization; wherein the vapor infiltration treatment is carried out in a chemical vapor deposition apparatus; controlling the flow rate of the hydrocarbon gas to be 200-300mL/min; the high-temperature decomposition and polycondensation temperature is 1000-1300 deg.C, and the time is 1-7 days.
13. A binder-jet printed silicon carbide ceramic material obtained by the production method according to any one of claims 1 to 12.
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Application publication date: 20221104 |