CN114956831A - Reaction sintering silicon carbide ceramic and preparation method thereof - Google Patents
Reaction sintering silicon carbide ceramic and preparation method thereof Download PDFInfo
- Publication number
- CN114956831A CN114956831A CN202111079010.5A CN202111079010A CN114956831A CN 114956831 A CN114956831 A CN 114956831A CN 202111079010 A CN202111079010 A CN 202111079010A CN 114956831 A CN114956831 A CN 114956831A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- ink
- sintering
- powder
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- B33Y10/00—Processes of additive manufacturing
-
- 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
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- 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
- C04B2235/424—Carbon black
-
- 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
- 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
- C04B2235/425—Graphite
-
- 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
- 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
- C04B2235/428—Silicon
-
- 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
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
-
- 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
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of reaction sintering silicon carbide ceramic, which comprises four steps of preparing silicon carbide powder, preparing ink, preparing green compact and sintering the green compact, and belongs to the technical field of silicon carbide ceramic preparation. According to the preparation method of the reaction sintering silicon carbide ceramic, disclosed by the invention, the carbon source is directly introduced into the ink, so that the carbon content in the silicon carbide printing blank is greatly increased, the content of beta-silicon carbide generated in the final sintering blank is further greatly increased, the content of free silicon is further greatly reduced, and the density, the strength and the hardness of the silicon carbide ceramic are improved. Meanwhile, the phenomenon that the printed green body is insufficient in strength due to insufficient penetration depth of glue in the sintering process because the ink-jet glue is attached to the surface of the powder after the carbon powder is directly added into the powder is avoided.
Description
Technical Field
The invention relates to the technical field of silicon carbide ceramic preparation, in particular to reaction sintering silicon carbide ceramic and a preparation method thereof.
Background
Silicon carbide (SiC) has good thermal shock resistance and chemical stability, and thus has good application prospects under high temperature and extreme conditions. However, SiC ceramics are difficult to process to form products with complex shapes, and the traditional SiC ceramic preparation processes such as powder sintering and film deposition consolidation have a plurality of limitations, which influence the exertion of excellent performances such as high-temperature performance, environmental resistance, high strength and the like.
The 3D ink-jet printing technology is a new rapid forming technology at present, and has the advantages of rapidness, precision and capability of forming complex materials, but the compactness of the SiC ceramic prepared by the 3D ink-jet printing technology at present is poor, and the mechanical properties of the SiC ceramic product are influenced.
The reaction sintering silicon carbide is also called siliconizing sintering silicon carbide, and is a preparation method which utilizes liquid silicon at high temperature to permeate into the green body to react with carbon to generate silicon carbide and fill silicon in pores, the content of the silicon carbide in the product determines the final performance of a sample, and the higher the content of the silicon carbide in the green body is, the better the performance is. Wherein increasing the carbon content in the biscuit is an effective way to increase the silicon carbide content in the product.
The glue used by the 3D ink-jet printing technical method at present is generally liquid resin, and the carbon content of the glue is low; in addition, if the printing powder is directly introduced into the carbon powder, the carbon powder is easy to float on the surface of a printing surface in the powder laying process due to low density of the carbon powder, and the uniformity of the product is influenced; in addition, because the specific surface area of the carbon powder is far larger than that of the silicon carbide powder, the ink-jet glue can be absorbed by the carbon powder, so that the powder particles are difficult to bond together. In the prior art, a reaction sintering silicon carbide biscuit which is difficult to realize direct printing has a high carbon source, so that the content of silicon carbide in the blank which is directly sintered after printing is too low.
Disclosure of Invention
The invention aims to provide a preparation method of reaction sintering silicon carbide ceramic with high silicon carbide content and compact structure.
In order to solve the above problems, the present invention provides a method for reaction sintering silicon carbide ceramics, comprising the steps of:
s1: preparing silicon carbide powder;
s2: preparing ink, stirring and mixing glue, a carbon source, an additive and a solvent to form a suspension, transferring the suspension into a ball mill for full ball milling to obtain a ball milling suspension, and filtering the ball milling suspension to obtain the ink;
s3: preparing a green body by adopting a 3D ink-jet method, laying a layer of silicon carbide powder in the step S1, spraying the ink in the step S2, after the ink is solidified, repeating the steps of laying silicon carbide powder and spraying the ink, and laying layer by layer to prepare the green body;
s4: and (4) sintering the green body, namely placing the green body in the step S3 into a high-temperature sintering furnace for siliconizing reaction sintering, and obtaining the reaction sintering silicon carbide ceramic after sintering.
Compared with the prior art, the carbon source is directly introduced into the ink, so that the carbon content in the silicon carbide printing blank is greatly increased, and the phenomenon that the strength of the printed blank is insufficient due to the fact that the penetration depth of glue in a sintering process is insufficient because the ink-jet glue is attached to the surface of powder after the carbon powder is directly added into the powder is avoided. In addition, the carbon source directly added into the glue can improve the carbon content in the glue, and also increases the carbon content in the final blank. The content of carbon in the printing blank body is increased, so that the content of the generated beta-silicon carbide in the final sintering blank body is greatly increased, and the content of free silicon in the final blank body is greatly reduced, thereby improving the density, strength and hardness of the silicon carbide ceramic.
Preferably, the silicon carbide powder in the step S1 is a mixed powder obtained by fully mixing silicon carbide powders with different particle sizes, wherein the particle size of the silicon carbide powder is 1-200 um, the purity is not less than 99%, and the bulk density is 1.2-2.0 g/cm 3 . The preparation of compact silicon carbide ceramic is facilitated by controlling the granularity, purity and bulk density of the silicon carbide powder.
Preferably, in the step S2, the mass percentage of the glue in the ink is 10% to 50%, the mass percentage of the carbon source is 10% to 50%, the mass percentage of the additive is 0.1% to 10%, and the balance is the solvent. The carbon content in the finally printed green body and the strength of the green body are controlled by controlling the mass percentage of the glue, the carbon source, the additive and the solvent, and finally the performance of the silicon carbide ceramic is improved.
Preferably, the carbon source in step S2 is selected from one or more of carbon black, graphene, and graphite. One or more of carbon black, graphene and graphite are selected as carbon sources to be added into the ink, because the carbon black, the graphene and the graphite have stable performance at normal temperature and do not react in the processes of forming a suspension with glue, an additive and a solvent and ball milling.
Preferably, the granularity of the carbon source in the step S2 is 20-500 nm. The carbon source with the nanometer particle size can better form a suspension with glue, additives and solvents.
Preferably, the glue in step S2 is selected from one or more of phenolic resin, furan resin, polyvinyl alcohol solution, and polyvinyl pyrrolidine solution. At least one of phenolic resin, furan resin, polyvinyl alcohol solution and polyvinyl pyrrolidine solution is selected as glue, so that the glue is easy to diffuse into the silicon carbide powder in the sintering process, and the strength of the sintered silicon carbide ceramic can be improved.
Preferably, the additive in step S2 is selected from one or more of tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate, BYK-160. One or more of tetramethyl ammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate and BYK-160 are added into the printing ink as additives, so that the comprehensive performance of the silicon carbide ceramic is improved.
Preferably, the solvent in step S2 is selected from one or more of absolute ethyl alcohol, ethylene glycol, acetone, and deionized water. One or more of absolute ethyl alcohol, ethylene glycol, acetone and deionized water is/are selected as a solvent, and can form a suspension with glue, a carbon source and an additive to form ink which is convenient for ink-jet printing.
Preferably, the mesh number of the filter screen used in the step S2 is 50 to 200 meshes. A filter screen with 50-200 meshes is used for filtering out large particles formed by insufficient ball milling in the ball milling process, so that the influence on the performance of the final silicon carbide ceramic caused by introducing the large particles into a ceramic blank in the ink-jet printing process is avoided.
The invention also provides a reaction sintering silicon carbide ceramic prepared by the preparation method.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a method for preparing reaction-sintered silicon carbide ceramic by a 3D ink-jet method, which comprises the following steps:
s1: preparing silicon carbide powder, wherein the silicon carbide powder is mixed powder obtained by fully mixing silicon carbide with different particle sizes, the particle size of the silicon carbide powder is 1-200 mu m, the purity is more than or equal to 99 percent, and the bulk density is 1.2-2.0 g/cm 3 . By controllingThe granularity, purity and bulk density of the silicon carbide powder are favorable for preparing compact silicon carbide ceramics.
S2: preparing ink, stirring and mixing glue, a carbon source, an additive and a solvent to form a suspension, transferring the suspension into a ball mill for full ball milling to obtain a ball milling suspension, and filtering the ball milling suspension to obtain the ink; wherein the glue is selected from one or more of phenolic resin, furan resin, polyvinyl alcohol solution and polyvinyl pyrrolidine solution; the carbon source is selected from one or more of carbon black, graphene and graphite, and the granularity of the carbon source is 20-500 nm; the additive is one or more selected from tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate and BYK-160; the solvent is one or more selected from anhydrous ethanol, ethylene glycol, acetone and deionized water.
The glue in the ink is easy to diffuse into the silicon carbide powder in the sintering process, the strength of the sintered silicon carbide ceramic can be improved, and carbon black, graphene and graphite with the particle size of nano level can better form a suspension with the glue, an additive and a solvent; the additives of tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate and BYK-160 can improve the comprehensive performance of the silicon carbide ceramic; the solvents of absolute ethyl alcohol, glycol, acetone and deionized water can form a suspension with glue, a carbon source and an additive to form ink which is convenient for ink-jet printing.
S3: preparing a green body by adopting a 3D ink-jet method, laying a layer of silicon carbide powder in the step S1, spraying the ink in the step S2, after the ink is solidified, repeating the steps of laying silicon carbide powder and spraying the ink, and laying and spraying multiple layers of silicon carbide powder and ink layer by layer according to the shape of the prefabricated ceramic to prepare the green body;
the 3D ink-jet method can be used for preparing green bodies with complex shapes, and the problem that SiC ceramics are difficult to process to form products with complex shapes is solved
S4: and (4) sintering the green body, namely placing the green body obtained in the step S3 in a high-temperature sintering furnace, carrying out siliconizing reaction sintering at the sintering temperature of 1450-1800 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering.
And (3) infiltrating liquid silicon at high temperature into the blank body to react with carbon to generate silicon carbide ceramic through high-temperature carburization reaction sintering.
In the disclosure, a 3D inkjet printing technology is introduced into the preparation of the reaction-sintered silicon carbide ceramic, and by directly introducing a carbon source into the ink, on the one hand, the carbon content in the silicon carbide printing green body is greatly increased, and the content of the generated beta-silicon carbide in the final sintered green body is greatly increased and the content of free silicon in the green body is greatly reduced, thereby improving the density, strength and hardness of the silicon carbide ceramic. On the other hand, the problem that the strength of a printed blank is reduced because the glue which is jetted is attached to the surface of the powder body after the carbon powder is directly added into the powder body and is difficult to permeate into the powder body in the sintering process is avoided.
Example one
1) Preparing silicon carbide powder, wherein the silicon carbide powder is formed by mixing silicon carbide ceramic powder with the granularity of 50um, 100um and 150um respectively, the purity of the mixed silicon carbide ceramic powder is more than or equal to 99 percent, and the bulk density is 1.6g/cm 3 ；
2) Preparing ink, namely stirring and mixing 40%, 30%, 5% and 25% of phenolic resin, carbon black, BYK-160 and absolute ethyl alcohol by mass percentage to form suspension, wherein the particle size of the carbon black is 500 nm; transferring the suspension into a ball mill for full ball milling to fully mix the carbon source, the glue and the additive to obtain ball milling suspension; filtering the ball-milling suspension by using a filter screen of 100 meshes to obtain ink, wherein the viscosity of the ink is 5mPa & s;
3) preparing a green body, namely paving a layer of silicon carbide powder in the step 1) by adopting a 3D ink-jet method, then spraying the ink in the step 2), after the ink is solidified, repeatedly paving the silicon carbide powder in the step 1) and the ink in the step 2), and spraying multiple layers of silicon carbide powder and ink according to the shape of the prefabricated ceramic to finally prepare the green body;
4) sintering the green body, namely placing the green body prepared in the step 3) into a high-temperature sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1600 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering. The performance parameters of the resulting silicon carbide ceramic are set forth in Table 1.
Example two
1) Preparing silicon carbide powder, wherein the silicon carbide powder is formed by mixing silicon carbide ceramic powder with the granularity of 3um, 50um and 200um respectively, the purity of the mixed silicon carbide ceramic powder is more than or equal to 99 percent, and the bulk density is 2g/cm 3 ；
2) Preparing ink, namely stirring and mixing furan resin, graphene, ammonium polyacrylate, ethylene glycol and ethanol according to the mass percentage concentration of 30%, 5%, 30% and 5% to form turbid liquid, wherein the granularity of the graphene is 20 nm; transferring the suspension into a ball mill for full ball milling to fully mix the carbon source, the glue and the additive to obtain ball milling suspension; filtering the ball-milling suspension by using a 50 filter screen to obtain ink, wherein the viscosity of the ink is 10mPa & s;
3) preparing a green body, namely paving a layer of silicon carbide powder in the step 1) by adopting a 3D ink-jet method, then spraying the ink in the step 2), after the ink is solidified, repeatedly paving the silicon carbide powder in the step 1) and the ink in the step 2), and spraying multiple layers of silicon carbide powder and ink according to the shape of the prefabricated ceramic to finally prepare the green body;
4) sintering the green body, namely placing the green body prepared in the step 3) in a high-temperature sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1450 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering. The performance parameters of the resulting silicon carbide ceramic are set forth in Table 1.
EXAMPLE III
1) Preparing silicon carbide powder, wherein the silicon carbide powder is formed by mixing silicon carbide ceramic powder with the granularity of 30um, 90um, 150um and 180um respectively, the purity of the mixed silicon carbide ceramic powder is more than or equal to 99 percent, and the bulk density is 1.4g/cm 3 ；
2) Preparing ink, namely stirring and mixing polyvinyl alcohol solution, graphite, polyvinyl pyrrolidine and water according to the mass percentage concentration of 50%, 30%, 1% and 19.9% to form turbid liquid, wherein the granularity of the graphite is 200 nm; transferring the suspension into a ball mill for full ball milling to fully mix the carbon source, the glue and the additive to obtain ball milling suspension; filtering the ball-milling suspension by using a filter screen with 200 meshes to obtain ink, wherein the viscosity of the ink is 18mPa & s;
3) preparing a green body, namely paving a layer of silicon carbide powder in the step 1) by adopting a 3D ink-jet method, then spraying the ink in the step 2), after the ink is solidified, repeatedly paving the silicon carbide powder in the step 1) and the ink in the step 2), and spraying multiple layers of silicon carbide powder and ink according to the shape of the prefabricated ceramic to finally prepare the green body;
4) sintering the green body, namely placing the green body prepared in the step 3) into a high-temperature sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1800 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering. The performance parameters of the resulting silicon carbide ceramic are set forth in Table 1.
Example four
1) Preparing silicon carbide powder, wherein the silicon carbide powder is formed by mixing silicon carbide ceramic powder with the granularity of 5um, 30um, 60um, 80um and 100um respectively, the purity of the mixed silicon carbide ceramic powder is more than or equal to 99 percent, and the bulk density is 2g/cm 3 ；
2) Preparing ink, namely stirring and mixing a polyvinyl pyrrolidine solution, a carbon source, triethyl phosphate and deionized water according to the mass percentage concentration of 50%, 10% and 30% to form turbid liquid, wherein the carbon source is prepared from graphene with the granularity of 50 nanometers and graphite 1 with the granularity of 150 nm: 1, mixing; transferring the suspension into a ball mill for full ball milling to fully mix the carbon source, the glue and the additive to obtain ball milling suspension; filtering the ball-milling suspension by using a filter screen of 150 meshes to obtain ink, wherein the viscosity of the ink is 20mPa & s;
3) preparing a green body, namely paving a layer of silicon carbide powder in the step 1) by adopting a 3D ink-jet method, then spraying the ink in the step 2), after the ink is solidified, repeatedly paving the silicon carbide powder in the step 1) and the ink in the step 2), and spraying multiple layers of silicon carbide powder and ink according to the shape of the prefabricated ceramic to finally prepare the green body;
4) sintering the green body, namely placing the green body prepared in the step 3) into a high-temperature sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1500 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering. The performance parameters of the resulting silicon carbide ceramic are set forth in Table 1.
EXAMPLE five
1) Preparing silicon carbide powder, wherein the silicon carbide powder is formed by mixing silicon carbide ceramic powder with the granularity of 100um, 150um and 200um respectively, the purity of the mixed silicon carbide ceramic powder is more than or equal to 99 percent, and the bulk density is 1.2g/cm 3 ；
2) Preparing ink, namely stirring and mixing glue, a carbon source, an additive and a solvent according to the mass percentage concentration of 30%, 40%, 5% and 25% to form suspension, wherein the glue is prepared from phenolic resin, furan resin and polyvinyl alcohol solution according to the mol ratio of 2:1:1, mixing a carbon source, an additive and a solvent, wherein the carbon source is formed by mixing carbon black with the granularity of 400 nanometers, graphene with the granularity of 20 nanometers and graphite with the granularity of 200 nanometers according to the molar ratio of 1:3:2, the additive is formed by mixing tetramethyl ammonium hydroxide, ammonium polyacrylate, herring oil and castor oil according to the molar ratio of 3:2:1:1, and the solvent is formed by mixing ethylene glycol and deionized water according to the molar ratio of 1: 2; transferring the suspension into a ball mill for full ball milling to fully mix the carbon source, the glue and the additive to obtain ball milling suspension; filtering the ball-milling suspension by using a filter screen of 200 meshes to obtain ink, wherein the viscosity of the ink is 13mPa & s;
3) preparing a green body, namely paving a layer of silicon carbide powder in the step 1) by adopting a 3D ink-jet method, then spraying the ink in the step 2), after the ink is solidified, repeatedly paving the silicon carbide powder in the step 1) and the ink in the step 2), and spraying multiple layers of silicon carbide powder and ink according to the shape of the prefabricated ceramic to finally prepare the green body;
4) sintering the green body, namely placing the green body prepared in the step 3) into a high-temperature sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1600 ℃, and obtaining the reaction sintering silicon carbide ceramic after sintering. The performance parameters of the resulting silicon carbide ceramic are set forth in Table 1.
TABLE 13 performance of the ink-jet method for preparing reaction-sintered silicon carbide ceramics
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (10)
1. A preparation method of reaction sintering silicon carbide ceramic comprises the following steps:
s1: preparing silicon carbide powder;
s2: preparing ink, stirring and mixing glue, a carbon source, an additive and a solvent to form a suspension, transferring the suspension into a ball mill for full ball milling to obtain a ball milling suspension, and filtering the ball milling suspension to obtain the ink;
s3: preparing a green body by adopting a 3D ink-jet method, laying a layer of silicon carbide powder in the step S1, spraying the ink in the step S2, after the ink is solidified, repeating the steps of laying silicon carbide powder and spraying the ink, and laying layer by layer to prepare the green body;
s4: and (4) sintering the green body, namely placing the green body in the step S3 into a high-temperature sintering furnace for siliconizing reaction sintering, and obtaining the reaction sintering silicon carbide ceramic after sintering.
2. The method for preparing reaction-sintered silicon carbide ceramic according to claim 1, wherein the silicon carbide powder in step S1 is a mixed powder obtained by mixing silicon carbide powders of different particle sizes, the particle size of the silicon carbide powder is 1 to 200 μm, the purity is not less than 99%, and the bulk density is 1.2 to 2.0g/cm 3 。
3. The method for preparing reaction-sintered silicon carbide ceramic according to claim 1, wherein the ink prepared in step S2 contains 10 to 50% by mass of glue, 10 to 50% by mass of carbon source, 0.1 to 10% by mass of additive, and the balance solvent.
4. The method for preparing reaction-sintered silicon carbide ceramic according to claim 1, wherein the carbon source in step S2 is selected from one or more of carbon black, graphene and graphite.
5. The method of claim 4, wherein the carbon source in step S2 has a particle size of 20-300 nm.
6. The method of claim 1, wherein the glue in step S2 is selected from one or more of phenolic resin, furan resin, polyvinyl alcohol solution, and polyvinyl pyrrolidine solution.
7. The method as claimed in claim 1, wherein the additive in step S2 is selected from one or more of tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate, BYK-160.
8. The method of claim 1, wherein the solvent used in step S2 is selected from one or more of absolute ethyl alcohol, ethylene glycol, acetone, and deionized water.
9. The method for producing reaction-sintered silicon carbide ceramic according to claim 1, wherein the number of mesh filters used in step S2 is 50 to 200 mesh.
10. A reaction-sintered silicon carbide ceramic produced by the production method according to claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111079010.5A CN114956831B (en) | 2021-09-15 | 2021-09-15 | Reaction sintering silicon carbide ceramic and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111079010.5A CN114956831B (en) | 2021-09-15 | 2021-09-15 | Reaction sintering silicon carbide ceramic and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114956831A true CN114956831A (en) | 2022-08-30 |
| CN114956831B CN114956831B (en) | 2023-08-11 |
Family
ID=82974765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111079010.5A Active CN114956831B (en) | 2021-09-15 | 2021-09-15 | Reaction sintering silicon carbide ceramic and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114956831B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116854478A (en) * | 2023-07-20 | 2023-10-10 | 四川硅旺新材料科技有限公司 | Preparation method of reaction sintering silicon carbide |
| CN117886609A (en) * | 2024-03-15 | 2024-04-16 | 广东佛山市陶瓷研究所控股集团股份有限公司 | Silicon carbide ceramic material and preparation method and application thereof |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150069649A1 (en) * | 2007-04-04 | 2015-03-12 | The Exone Company | Powder Particle Layerwise Three-Dimensional Printing Process |
| US20160144573A1 (en) * | 2014-11-25 | 2016-05-26 | Seiko Epson Corporation | Method and apparatus for producing three-dimensionally shaped object and three-dimensionally shaped object |
| CN107098714A (en) * | 2017-04-26 | 2017-08-29 | 西安交通大学 | A kind of types of silicon carbide-based ceramics method for manufacturing parts based on 3DP increases material manufacturing technologies |
| CN108290390A (en) * | 2015-11-24 | 2018-07-17 | 西格里碳素欧洲公司 | The 3D printing of ceramic component |
| WO2018206250A1 (en) * | 2017-05-10 | 2018-11-15 | Ceramtec Gmbh | Additive manufacturing of metal matrix composite materials |
| CN108947494A (en) * | 2018-07-09 | 2018-12-07 | 天津大学 | A kind of ceramic material increasing material manufacturing method |
| CN110330351A (en) * | 2019-07-26 | 2019-10-15 | 华中科技大学 | A kind of preparation method and product of SiC fiber reinforcement SiC ceramic base part |
| WO2019221999A1 (en) * | 2018-05-18 | 2019-11-21 | Arconic Inc. | Binder jet sintering additives and methods of use thereof |
| WO2020037054A1 (en) * | 2018-08-14 | 2020-02-20 | William Marsh Rice University | Distortion mitigation during sintering of ceramics through the incorporation of ceramic precursor solutions |
| CN111132953A (en) * | 2017-09-28 | 2020-05-08 | 西格里碳素欧洲公司 | Ceramic component |
| RU2735471C1 (en) * | 2019-09-25 | 2020-11-02 | Акционерное общество «Обнинское научно-производственное предприятие «Технология» им. А.Г.Ромашина» | Method of obtaining articles of complex shape based on reaction-bonded silicon carbide |
| CN112521130A (en) * | 2019-08-28 | 2021-03-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of ceramic part based on 3D printing technology |
| CN113135757A (en) * | 2021-04-29 | 2021-07-20 | 华中科技大学 | Ceramic primary blank forming method based on microwave in-situ sintering and product |
-
2021
- 2021-09-15 CN CN202111079010.5A patent/CN114956831B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150069649A1 (en) * | 2007-04-04 | 2015-03-12 | The Exone Company | Powder Particle Layerwise Three-Dimensional Printing Process |
| US20160144573A1 (en) * | 2014-11-25 | 2016-05-26 | Seiko Epson Corporation | Method and apparatus for producing three-dimensionally shaped object and three-dimensionally shaped object |
| CN108290390A (en) * | 2015-11-24 | 2018-07-17 | 西格里碳素欧洲公司 | The 3D printing of ceramic component |
| CN107098714A (en) * | 2017-04-26 | 2017-08-29 | 西安交通大学 | A kind of types of silicon carbide-based ceramics method for manufacturing parts based on 3DP increases material manufacturing technologies |
| WO2018206250A1 (en) * | 2017-05-10 | 2018-11-15 | Ceramtec Gmbh | Additive manufacturing of metal matrix composite materials |
| CN111132953A (en) * | 2017-09-28 | 2020-05-08 | 西格里碳素欧洲公司 | Ceramic component |
| WO2019221999A1 (en) * | 2018-05-18 | 2019-11-21 | Arconic Inc. | Binder jet sintering additives and methods of use thereof |
| CN108947494A (en) * | 2018-07-09 | 2018-12-07 | 天津大学 | A kind of ceramic material increasing material manufacturing method |
| WO2020037054A1 (en) * | 2018-08-14 | 2020-02-20 | William Marsh Rice University | Distortion mitigation during sintering of ceramics through the incorporation of ceramic precursor solutions |
| CN110330351A (en) * | 2019-07-26 | 2019-10-15 | 华中科技大学 | A kind of preparation method and product of SiC fiber reinforcement SiC ceramic base part |
| CN112521130A (en) * | 2019-08-28 | 2021-03-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of ceramic part based on 3D printing technology |
| RU2735471C1 (en) * | 2019-09-25 | 2020-11-02 | Акционерное общество «Обнинское научно-производственное предприятие «Технология» им. А.Г.Ромашина» | Method of obtaining articles of complex shape based on reaction-bonded silicon carbide |
| CN113135757A (en) * | 2021-04-29 | 2021-07-20 | 华中科技大学 | Ceramic primary blank forming method based on microwave in-situ sintering and product |
Non-Patent Citations (5)
| Title |
|---|
| CORSON L. CRAMER等: "Properties of SiC- Si made via binder jet 3D printing of SiC powder, carbon addition, and silicon melt infiltration", 《JOURNAL OF AMERICAN CERAMIC SOCIETY》 * |
| CORSON L. CRAMER等: "Properties of SiC- Si made via binder jet 3D printing of SiC powder, carbon addition, and silicon melt infiltration", 《JOURNAL OF AMERICAN CERAMIC SOCIETY》, vol. 104, no. 11, 19 June 2021 (2021-06-19) * |
| 王子晨等: "液相渗硅制备碳化硅/石墨复合陶瓷材料", 《陶瓷学报》 * |
| 王子晨等: "液相渗硅制备碳化硅/石墨复合陶瓷材料", 《陶瓷学报》, no. 05, 15 October 2016 (2016-10-15) * |
| 蔡嘉伟等: "间接3D陶瓷打印技术：文献综述（英文）", JOURNAL OF CENTRAL SOUTH UNIVERSITY, vol. 28, no. 4 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116854478A (en) * | 2023-07-20 | 2023-10-10 | 四川硅旺新材料科技有限公司 | Preparation method of reaction sintering silicon carbide |
| CN117886609A (en) * | 2024-03-15 | 2024-04-16 | 广东佛山市陶瓷研究所控股集团股份有限公司 | Silicon carbide ceramic material and preparation method and application thereof |
| CN117886609B (en) * | 2024-03-15 | 2024-05-28 | 广东佛山市陶瓷研究所控股集团股份有限公司 | Silicon carbide ceramic material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114956831B (en) | 2023-08-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114956831B (en) | Reaction sintering silicon carbide ceramic and preparation method thereof | |
| JP7099739B2 (en) | Method for manufacturing porous silicon carbide ceramic carrier | |
| CN109987941B (en) | High-entropy ceramic composite material with oxidation resistance and preparation method and application thereof | |
| CN112521130B (en) | Preparation method of ceramic part based on 3D printing technology | |
| CN110467467B (en) | Bulk silicon carbide polymer precursor ceramic and blending and cracking preparation method | |
| CN112521131B (en) | High-solid-phase-content alumina photosensitive ceramic material and preparation method thereof | |
| CN101913873A (en) | Method for making support body of porous ceramic filter pipe capable of improving strength and pore connectivity | |
| CN112830798B (en) | Preparation method of boron carbide granulation powder for pressureless sintering | |
| US4929404A (en) | Graphitic or carbonaceous moldings and processes for producing the same | |
| CN113458387A (en) | 3D printing gradient ceramic metal material and preparation method thereof | |
| CN109384437B (en) | Hybrid fiber cement-based composite material for 3D printing and preparation method thereof | |
| CN103833034A (en) | Method for preparation of silicon carbide slurry with nano-carbontube and graphene as carbon sources | |
| KR101618736B1 (en) | Isotropic graphite article and and method of manufacturing the same | |
| CN113718124B (en) | Preparation method of bicrystal gradient hard alloy | |
| CN111875404A (en) | Preparation method of silicon carbide slurry applied to free direct-write forming technology | |
| CN105367054A (en) | Preparation method for gel-casting system-based zirconium dioxide ball-milling medium | |
| CN105347396A (en) | Preparation method for zirconium dioxide ball-milling medium | |
| CN106823844A (en) | Porous membrane and preparation method thereof | |
| CN108706974A (en) | A kind of ramet superhigh temperature ceramics and preparation method thereof of normal pressure solid-phase sintering densification hafnium solid solution | |
| CN116354729B (en) | SiC ceramic part and preparation method and application thereof | |
| CN109266941B (en) | Plate-shaped tungsten carbide-cobalt alloy and preparation method thereof | |
| CN105347792A (en) | Preparation method of zirconium dioxide ball-milling medium based on aqueous gel system | |
| CN108484209A (en) | A kind of ceramic membrane and its preparation process | |
| CN116283251B (en) | Alumina ceramic and preparation method and application thereof | |
| CN104086183B (en) | The controlled porous Si of a kind of porosity3N4Preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |