CN114394844A - Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic - Google Patents

Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic Download PDF

Info

Publication number
CN114394844A
CN114394844A CN202111621742.2A CN202111621742A CN114394844A CN 114394844 A CN114394844 A CN 114394844A CN 202111621742 A CN202111621742 A CN 202111621742A CN 114394844 A CN114394844 A CN 114394844A
Authority
CN
China
Prior art keywords
carbon
wood
silicon
waste
silicon carbide
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.)
Pending
Application number
CN202111621742.2A
Other languages
Chinese (zh)
Inventor
闫春泽
王长顺
陈安南
史玉升
吴思琪
聂翔
刘桂宙
欧阳震
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huazhong University of Science and Technology
Original Assignee
Huazhong University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Huazhong University of Science and Technology filed Critical Huazhong University of Science and Technology
Priority to CN202111621742.2A priority Critical patent/CN114394844A/en
Publication of CN114394844A publication Critical patent/CN114394844A/en
Pending legal-status Critical Current

Links

Images

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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
    • 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
    • C04B35/515—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
    • 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
    • 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
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • 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
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • C04B35/62209—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse using woody material, remaining in the 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
    • C04B2235/60—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
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • 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
    • C04B2235/65—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
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/658—Atmosphere during thermal 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Dispersion Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a method for preparing silicon carbide ceramic by waste 3D printing and the silicon carbide ceramic. The method comprises the following steps: sequentially carbonizing and crushing the wood waste to obtain wood carbon powder; mixing the wood carbon powder with a binder, and performing 3D printing and forming to obtain a wood carbon blank; dissolving carbon-containing waste in an organic solvent to obtain a carbon-containing solution, and immersing the wooden carbon blank in the carbon-containing solution for solution impregnation pyrolysis to obtain a wooden carbon preform; and evaporating silicon in the silicon-containing waste material by heating to obtain gas-phase silicon, and sintering the wood-carbon prefabricated body in the gas-phase silicon to obtain the silicon carbide ceramic. The invention comprehensively utilizes the wood waste, the carbon-containing waste and the silicon-containing waste with high efficiency, and prepares the silicon carbide by gas-phase reaction sintering of the silicon-containing waste, thereby solving the technical problems of high cost, impurity pollution, incapability of preparing silicon carbide ceramics with complex structures and the like at present.

Description

Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic
Technical Field
The invention belongs to the technical field of silicon carbide ceramics, and particularly relates to a method for preparing silicon carbide ceramics by 3D printing of waste materials and the silicon carbide ceramics.
Background
The silicon carbide ceramic has the comprehensive qualities of good chemical stability, high thermal conductivity, low thermal expansion, high thermal shock resistance and the like, and is widely applied in the fields of aerospace, automobiles, chemical catalysis, heat exchange, electromagnetic absorption/shielding and the like. At present, the main synthesis routes of SiC ceramics include chemical vapor deposition, precursor impregnation and cracking, reaction infiltration and the like, and raw materials and equipment required by the methods are expensive, so a method capable of effectively reducing the raw material cost and the reaction temperature for producing silicon carbide is urgently needed, so that the economy and the application range of the silicon carbide ceramics are improved.
Human beings produce a large amount of solid waste in life and production processes. For example, wood is the most abundant renewable and sustainable resource in the world, plays an important role in production and life of people, and can be used for manufacturing appliances, furniture, buildings and the like. However, during the processing and production of wood products, wooden waste materials such as rice hulls, straw, fallen leaves, hay, branches, and wood chips are inevitably produced. Coal and oil belong to fossil energy, and are non-renewable resources formed by the evolution of organic matters for tens of millions or even billions of years, the oil is called industrial blood, the coal is called industrial grain, and with the increasing increase of mining, human beings face a serious resource shortage problem, however, residue wastes such as coal ash, petroleum asphalt, coal tar asphalt and the like generated in the utilization process of the petroleum and coal resources cause a serious environmental protection problem. Along with the development of the photovoltaic industry, a lot of silicon mud waste materials are inevitably generated in the silicon wafer cutting process, so that expensive crystalline silicon is lost, and meanwhile, serious environmental pollution is caused. With the proposal of the targets of carbon neutralization and carbon peak reaching, the recovery and utilization of resources also become an important emission reduction means. The key points of people's attention are to effectively improve the utilization rate of waste resources and the added value of products.
At present, research work has been carried out on the preparation of silicon carbide ceramics from solid wastes, for example 201711057626.6 discloses a method for preparing high-quality silicon carbide from diamond cutting wastes, the invention prepares silicon carbide powder by pressing silicon-containing diamond wire cutting wastes, high-purity carbon powder and a reducing agent into balls, and then carrying out high-temperature smelting, crushing and acid washing, thereby greatly utilizing the silicon-containing wastes. However, the invention still needs high-cost high-purity carbon source as reactant, and the pollution of impurities in the waste materials can not be avoided in the smelting process, so that a further purification process is needed, and the obtained silicon carbide powder needs to be further processed to obtain a component. 201710725687.9 discloses a method for preparing silicon carbide porous ceramics by using crystalline silicon cutting waste, the invention fully mixes the crystalline silicon cutting waste with carbon powder, ammonium salt and phenolic resin, then carries out dry pressing and forming, and finally carries out high temperature sintering to obtain the silicon carbide porous ceramics. However, the method cannot avoid the problem of impurity pollution in the waste materials, the quality of the silicon carbide ceramic is greatly reduced, and the silicon carbide ceramic with a complex structure cannot be prepared by dry pressing, and further machining is needed to meet the use requirement.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a method for preparing silicon carbide ceramic by 3D printing of waste materials and the silicon carbide ceramic, and aims to solve the technical problems that the existing silicon carbide ceramic with a complex structure is high in cost, polluted by impurities and incapable of being prepared by comprehensively utilizing wooden waste materials, carbon-containing waste materials and silicon-containing waste materials efficiently and sintering the silicon-containing waste materials through gas-phase reaction.
To achieve the above object, according to one aspect of the present invention, there is provided a method for preparing silicon carbide ceramic by 3D printing of waste material, comprising the steps of:
s1: sequentially carbonizing and crushing the wood waste to obtain wood carbon powder;
s2: mixing the wood carbon powder with a binder, and performing 3D printing and forming to obtain a wood carbon blank;
s3: dissolving carbon-containing waste in an organic solvent to obtain a carbon-containing solution, and immersing the wooden carbon blank in the carbon-containing solution for solution impregnation pyrolysis to obtain a wooden carbon preform;
s4: and evaporating silicon in the silicon-containing waste material by heating to obtain gas-phase silicon, and sintering the wood-carbon prefabricated body in the gas-phase silicon to obtain the silicon carbide ceramic.
Preferably, in step S1, the wood waste is one or more of rice hull, straw, fallen leaves, hay, branches, wood blocks and wood chips.
Preferably, the particle size of the wood carbon powder is 0.5-100 microns; the 3D printing and forming is three-dimensional photocuring forming, powder bed melting forming, material extrusion forming or binder spraying forming.
Preferably, the carbon-containing waste material is petroleum asphalt and/or coal tar pitch, and the organic solvent is one or more of gasoline, diesel oil, kerosene, xylene, toluene, carbon disulfide, carbon tetrachloride and n-hexane; the mass ratio of the carbon-containing waste to the organic solvent is (1-5): 5. here, a ratio lower than this ratio results in a lower solid content of the impregnation solution, and the mass after impregnation does not change much, and a ratio higher than this ratio makes it difficult to completely dissolve.
Preferably, the solution impregnation pyrolysis specifically comprises: and immersing the wood carbon blank into a carbon-containing solution, vacuumizing the carbon-containing solution to 0-200 Pa in a vacuum impregnation tank, maintaining the pressure for 15-60 min, moving the carbon-containing solution to a vacuum atmosphere carbonization furnace, introducing protective gas, heating the carbon-containing solution to 800-1200 ℃ at the heating rate of 0.1-5 ℃/min, and preserving the heat for 2-10 h to obtain the wood carbon preform.
Preferably, the method further comprises: adjusting the porosity of the woody carbon preform by repeating the step S3 for a greater number of times, the less the porosity of the woody carbon preform is, the more the step S3 is repeated, the porosity of the woody carbon preform is 35 to 80%.
Preferably, in step S4, the silicon-containing waste is silicon mud waste and/or coal ash; the mass ratio of the silicon-containing waste to the wood-carbon prefabricated body is (2.5-5.5): 1. the silicon mud waste is generated in the silicon wafer cutting process, and the silicon mud waste is derived from the waste in the photovoltaic silicon wafer cutting process.
The mass ratio of the silicon-containing waste to the wood-carbon prefabricated body is related to the silicon-containing waste, when the silicon-containing waste is silicon mud waste, a silicon simple substance occupies a large proportion, and a small mass ratio of 2.5 is selected according to the silicon-carbon metering ratio: 1, when the silicon-containing waste material is coal ash, the silicon dioxide accounts for a large proportion, and a large mass proportion of 5.5: 1, if a mixture of the two is used, an intermediate ratio may be selected.
Preferably, the step S4 is specifically: the method comprises the following steps of (1) keeping the temperature of silicon-containing waste materials in an oven at 100-200 ℃ for 10-24 h, drying, laying the dried silicon-containing waste materials at the bottom of a crucible, and placing a wood-carbon prefabricated body on a supporting body in the crucible; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas or vacuumizing, heating to 1300-1800 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 2-5 h to obtain the silicon carbide ceramic.
In accordance with another aspect of the present invention, a silicon carbide ceramic is provided.
Preferably, the porosity of the silicon carbide ceramic is 2-70%.
In general, at least the following advantages can be obtained by the above technical solution contemplated by the present invention compared to the prior art.
(1) The method comprises the steps of adopting wood waste, carbon-containing waste and silicon-containing waste as raw materials, processing the wood waste to obtain wood carbon powder, forming a wood carbon blank body by adopting a 3D printing technology, wherein the wood carbon blank body has a certain porosity, immersing the wood carbon blank body into an organic solution in which the carbon-containing waste is dissolved, and performing solution impregnation pyrolysis to ensure that carbon enters pores of the wood carbon blank body and densify the wood carbon blank body, so that the porosity of the wood carbon blank body is changed. Then the silicon-containing waste material is sintered in a gas phase reaction manner to obtain the silicon carbide part with controllable macrostructure. The method realizes the efficient comprehensive and reasonable application of the wood waste, the carbon-containing waste and the silicon-containing waste, the used raw materials are cheap and easily available waste materials, the environmental pollution can be greatly reduced after the waste materials are recycled, the production cost of silicon carbide is reduced, the utilization rate of waste resources and the added value of products are effectively improved, and the sustainable development is promoted. Meanwhile, the problem that complex special-shaped parts of the silicon carbide ceramic are difficult to process can be effectively solved by adopting a 3D printing technology, the silicon carbide parts with required structures are formed according to requirements, and the application range of the silicon carbide ceramic is further expanded.
(2) According to the method, the porosity of the wood-based carbon preform is adjusted by repeating the step S3 for more times, the porosity of the wood-based carbon preform is smaller when the step S3 is repeated for more times, and the porosity of the wood-based carbon preform is 35-80%. The porosity of the wood carbon blank can be regulated and controlled by controlling the frequency of the process in the impregnation pyrolysis stage of the carbon-containing solution, so that the wood carbon preform with the porosity meeting the requirement is obtained.
(3) In the gas-phase reaction sintering process of the silicon-containing waste material in the step S4, an overhead sintering scheme is adopted, silicon in the silicon-containing waste material is evaporated through heating to obtain a gas-phase silicon source, namely, the dried silicon-containing waste material is laid at the bottom of a crucible, and a wood-carbon prefabricated body is placed on a support body in the crucible, so that the gas-phase silicon source reacts with the wood-carbon prefabricated body, the wood-carbon prefabricated body is prevented from directly contacting with the silicon-containing waste material, and the silicon carbide is prevented from being polluted by impurities in the silicon-containing waste material.
(4) According to the scheme of 3D printing of the wood waste, dipping and pyrolysis of the carbon-containing waste and gas phase reaction sintering of the silicon-containing waste, the silicon carbide ceramic with good comprehensive performance can be obtained without adopting high-purity raw materials, and each step is based on a corresponding scientific principle, so that the feasibility is high. 3D prints and is a material forming technology based on the principle of discrete-piling up, need not complicated mould, as long as according to the three-dimensional data file of model alright drive 3D printer work required part of shaping, do benefit to and realize high-performance complicated carborundum's high efficiency, low carbon, green preparation and application, 3D prints and is a "material increase" processing mode, compares in traditional "subtract material" processing, but the integral shaping complex structure part, realizes that the raw materials can cyclic utilization, has further reduced the material cost. The 3D printing technology used by the invention has wide coverage, and the corresponding 3D printing technology can be selected according to actual requirements so as to meet the diversified preparation and application of large, medium and small-size complex silicon carbide components.
Drawings
FIG. 1 is a flow chart of a method for preparing silicon carbide ceramic by 3D printing of waste materials according to a preferred embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The method for preparing the silicon carbide ceramic through 3D printing of the waste materials comprises the steps of firstly using wood carbon powder obtained after wood waste materials are carbonized and mechanically crushed as a raw material for 3D printing, then forming a wood carbon blank body with a required structure through 3D printing, obtaining a wood carbon prefabricated body with controllable porosity after dipping and pyrolysis of a carbon-containing waste material solution, and finally obtaining the silicon carbide ceramic through gas phase reaction sintering of silicon-containing waste materials.
Referring to fig. 1, the method specifically includes the following steps:
s1: sequentially carbonizing and crushing the wood waste to obtain wood carbon powder;
the wood waste is preferably one or more of rice hulls, straws, fallen leaves, hay, branches, wood blocks and wood chips.
The carbonization comprises the following steps: and (3) placing the wood waste into a carbonization furnace, introducing nitrogen or argon as protective gas, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 5 hours to obtain wood carbon, and mechanically crushing and screening to obtain the wood carbon powder.
The particle size of the wood carbon powder is preferably 0.5-100 microns.
S2: mixing the wood carbon powder with a binder, and performing 3D printing and forming to obtain a wood carbon blank;
the binder is preferably one or more of nylon powder, polyether sulfone powder, epoxy resin powder, liquid epoxy resin AB glue, liquid phenolic resin and photosensitive resin.
Mixing the binder and the wood carbon powder, and forming a wood carbon blank by adopting a 3D printing technology; the 3D printing technique is preferably stereolithography, powder bed melting, material extrusion, binder jetting.
S3: dissolving carbon-containing waste in an organic solvent to obtain a carbon-containing solution, and immersing the wooden carbon blank in the carbon-containing solution for solution impregnation pyrolysis to obtain a wooden carbon preform;
the carbon-containing waste material is preferably petroleum asphalt and/or coal tar pitch, and the organic solvent is preferably one or more of gasoline, diesel oil, kerosene, xylene, toluene, carbon disulfide, carbon tetrachloride and n-hexane; the mass ratio of the carbon-containing waste to the organic solvent is preferably (1-5): 5; and fully mixing the carbon-containing waste material and the organic solvent, and then putting the mixture into an ultrasonic device to obtain a carbon-containing solution.
The solution impregnation pyrolysis comprises the following steps: placing the wood carbon blank body into a carbon-containing solution, vacuumizing the vacuum impregnation tank to 0-200 Pa, maintaining the pressure for 15-60 min, moving the vacuum impregnation tank to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the vacuum impregnation tank to 800-1200 ℃ at a heating rate of 0.1-5 ℃/min, preserving the temperature for 2-10 h to obtain a wood carbon preform, and adjusting the porosity of the wood carbon preform by repeating the step S3 for more times, wherein the porosity of the wood carbon preform is smaller as the number of times of repeating the step S3 is larger, and the porosity of the wood carbon preform is 35-80%.
S4: and evaporating silicon in the silicon-containing waste material by heating to obtain gas-phase silicon, and sintering the wood-carbon prefabricated body in the gas-phase silicon to obtain the silicon carbide ceramic.
The silicon-containing waste is preferably silicon mud waste and/or coal ash; the mass ratio of the silicon-containing waste to the wood-carbon prefabricated body is (2.5-5.5): 1.
the gas phase reaction sintering comprises the following steps: putting the silicon-containing waste into an oven with the temperature of 100-200 ℃ for heat preservation for 10-24 h for drying; then, a certain amount of silicon-containing waste material is paved at the bottom of the crucible, and the wood-carbon prefabricated body is placed on a support body, placed in the crucible and covered by a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas or vacuumizing, heating to 1300-1800 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 2-5 h to obtain the silicon carbide.
The porosity of the silicon carbide is preferably 2-70%.
The technical scheme of the invention is explained in detail by the following specific examples:
example 1
S1: putting the straws in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 5 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 50 microns.
S2: selecting nylon powder as a binder, mixing the nylon powder with wood carbon powder, designing a required model, and carrying out fusion forming through a powder bed to obtain a wood carbon blank; the pores of the printed wood carbon blank are 60 to 70 percent.
S3: dissolving petroleum asphalt in gasoline to obtain a carbon-containing solution, wherein the mass ratio of the petroleum asphalt to the carbon-containing solution is 1: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank body in a carbon-containing waste solution, vacuumizing the vacuum impregnation tank to 200Pa, maintaining the pressure for 15min, moving the vacuum impregnation tank to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the wood carbon blank body to 800 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 2h to obtain the wooden carbon preform with the porosity of 80%.
S4: selecting silicon mud waste materials, wherein the mass ratio of the silicon mud waste materials to the wood carbon prefabricated body is 2.5: 1, putting the silicon mud waste into a drying oven at 100 ℃ for heat preservation for 24 hours for drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1300 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2h to obtain the silicon carbide with the porosity of 70%.
Example 2
S1: putting the rice hull into a carbonization furnace, introducing argon as protective gas, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 5 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 0.5 micron.
S2: selecting photosensitive resin as a binder, mixing the binder with wood carbon powder, designing a required model, and performing three-dimensional photocuring forming to obtain a wood carbon blank;
s3: dissolving coal tar pitch into diesel oil to obtain a carbon-containing solution, wherein the mass ratio of the coal tar pitch to the diesel oil is 5: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wood carbon blank into a carbon-containing waste solution, vacuumizing the solution to 0Pa in a vacuum impregnation tank, maintaining the pressure for 60min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 800 ℃ at the heating rate of 0.1 ℃/min, and preserving the temperature for 10h to obtain a wood carbon preform with the porosity of 35%.
S4: selecting coal ash, wherein the mass ratio of the coal ash to the wood carbon preform is 5.5: 1, putting the silicon mud waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1800 ℃ at the heating rate of 10 ℃/min, and preserving heat for 5 hours to obtain the silicon carbide with the porosity of 2%.
Example 3
S1: putting the wood blocks into a carbonization furnace, introducing argon as protective gas, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 5 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 100 microns.
S2: selecting liquid phenolic resin as a binder, designing a required model, and mixing and forming the binder and wood carbon powder by binder injection to obtain a wood carbon blank;
s3: dissolving petroleum asphalt in dimethylbenzene to obtain a carbon-containing solution, wherein the mass ratio of the petroleum asphalt to the carbon-containing solution is 2: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 100Pa in a vacuum impregnation tank, maintaining the pressure for 30min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1200 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 5h to obtain a wooden carbon preform with the porosity of 50%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 1: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to a mass ratio of 4: 1, putting the silicon-containing waste into a drying oven at 150 ℃ for heat preservation for 16h for drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1600 ℃ at the heating rate of 5 ℃/min, and preserving heat for 3h to obtain the silicon carbide with the porosity of 21%.
Example 4
S1: placing the wood chips in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 3 hours to obtain wood carbon, and mechanically crushing and sieving to obtain wood carbon powder with the particle size of 1 micron.
S2: selecting liquid phenolic resin as a binder, mixing the binder with wood carbon powder, designing a required model, and extruding and forming materials to obtain a wood carbon blank;
s3: dissolving coal tar pitch in toluene to obtain a carbon-containing solution, wherein the mass ratio of the coal tar pitch to the toluene is 3: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 200Pa in a vacuum impregnation tank, maintaining the pressure for 60min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1000 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 2h to obtain a wooden carbon preform with the porosity of 60%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 2: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to the mass ratio of 3.5: 1, putting the silicon-containing waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1500 ℃ at the heating rate of 10 ℃/min, and preserving heat for 5 hours to obtain the silicon carbide with the porosity of 36%.
Example 5
S1: placing the wood chips in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 3 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 30 microns.
S2: selecting polyether sulfone powder as a binder, mixing the polyether sulfone powder with wood carbon powder, designing a required model, and carrying out melt forming through a powder bed to obtain a wood carbon blank;
s3: dissolving coal tar pitch in n-hexane to obtain a carbon-containing solution, wherein the mass ratio of the coal tar pitch to the n-hexane is 5: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 100Pa in a vacuum impregnation tank, maintaining the pressure for 30min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1000 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 2h to obtain the wooden carbon preform with the porosity of 80%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 1: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to the mass ratio of 3.5: 1, putting the silicon-containing waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1500 ℃ at the heating rate of 10 ℃/min, and preserving heat for 3h to obtain the silicon carbide with the porosity of 70%.
Example 6
S1: placing the wood chips in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 3 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 60 microns.
S2: selecting epoxy resin powder as a binder, mixing the epoxy resin powder with wood carbon powder, designing a required model, and carrying out fusion forming through a powder bed to obtain a wood carbon blank;
s3: dissolving coal tar pitch in n-hexane to obtain a carbon-containing solution, wherein the mass ratio of the coal tar pitch to the n-hexane is 5: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 100Pa in a vacuum impregnation tank, maintaining the pressure for 60min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1000 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 2h to obtain a wooden carbon preform with the porosity of 50%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 0.5: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to the mass ratio of 3.5: 1, putting the silicon-containing waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1500 ℃ at the heating rate of 10 ℃/min, and preserving heat for 3h to obtain the silicon carbide with the porosity of 21%.
Example 7
S1: placing the wood chips in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 3 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 60 microns.
S2: selecting epoxy resin AB glue as a binder, mixing the epoxy resin AB glue with wood carbon powder, designing a required model, and carrying out fusion forming through a powder bed to obtain a wood carbon blank;
s3: dissolving petroleum asphalt in carbon tetrachloride to obtain a carbon-containing solution, wherein the mass ratio of the petroleum asphalt to the carbon tetrachloride is 2: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 0Pa in a vacuum impregnation tank, maintaining the pressure for 60min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1000 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 2h to obtain a wooden carbon preform with the porosity of 60%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 2: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to the mass ratio of 3.5: 1, putting the silicon-containing waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1500 ℃ at the heating rate of 10 ℃/min, and preserving heat for 3h to obtain the silicon carbide with the porosity of 36%.
Example 8
S1: placing the wood chips in a carbonization furnace, introducing nitrogen as protective gas, heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 3 hours to obtain wood carbon, and mechanically crushing and sieving to obtain the wood carbon powder with the particle size of 0.5 micron.
S2: selecting liquid epoxy resin as a binder, mixing the liquid epoxy resin with wood carbon powder, designing a required model, and extruding and forming materials to obtain a wood carbon blank;
s3: dissolving petroleum asphalt in dimethylbenzene to obtain a carbon-containing solution, wherein the mass ratio of the petroleum asphalt to the carbon-containing solution is 5: and 5, fully mixing and then placing in an ultrasonic device to obtain the carbon-containing waste solution. And (3) placing the wooden carbon blank into a carbon-containing waste solution, vacuumizing the solution to 0Pa in a vacuum impregnation tank, maintaining the pressure for 60min, moving the solution to a vacuum atmosphere carbonization furnace, introducing a protective atmosphere, heating the solution to 1000 ℃ at the heating rate of 1 ℃/min, and preserving the temperature for 2h to obtain a wooden carbon preform with the porosity of 35%.
S4: selecting silicon mud waste and coal ash, wherein the mass ratio of the silicon mud waste to the coal ash is 2: 1, and mixing the silicon-containing waste and the wood-carbon prefabricated body according to the mass ratio of 3.5: 1, putting the silicon-containing waste into a drying oven at 200 ℃ for heat preservation for 12h and drying; laying the wood carbon prefabricated body on the bottom of the crucible, placing the wood carbon prefabricated body on a support body, placing the support body in the crucible, and covering the support body with a cover; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas, heating to 1500 ℃ at the heating rate of 10 ℃/min, and preserving heat for 3h to obtain the silicon carbide with the porosity of 2%.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A method for preparing silicon carbide ceramic by 3D printing of waste materials is characterized by comprising the following steps:
s1: sequentially carbonizing and crushing the wood waste to obtain wood carbon powder;
s2: mixing the wood carbon powder with a binder, and performing 3D printing and forming to obtain a wood carbon blank;
s3: dissolving carbon-containing waste in an organic solvent to obtain a carbon-containing solution, and immersing the wooden carbon blank in the carbon-containing solution for solution impregnation pyrolysis to obtain a wooden carbon preform;
s4: and evaporating silicon in the silicon-containing waste material by heating to obtain gas-phase silicon, and sintering the wood-carbon prefabricated body in the gas-phase silicon to obtain the silicon carbide ceramic.
2. The method of claim 1, wherein in step S1, the wood waste is one or more of rice hulls, straw, fallen leaves, hay, branches, wood pieces, and wood chips.
3. The method according to claim 1 or 2, wherein the particle size of the wood carbon powder is 0.5 to 100 μm; the 3D printing and forming is three-dimensional photocuring forming, powder bed melting forming, material extrusion forming or binder spraying forming.
4. The method of claim 1, wherein the carbon-containing waste material is petroleum pitch and/or coal tar pitch, and the organic solvent is one or more of gasoline, diesel, kerosene, xylene, toluene, carbon disulfide, carbon tetrachloride, and n-hexane; the mass ratio of the carbon-containing waste to the organic solvent is (1-5): 5.
5. the method of claim 1, wherein the solution dip pyrolysis specifically comprises: and immersing the wood carbon blank into a carbon-containing solution, vacuumizing the carbon-containing solution to 0-200 Pa in a vacuum impregnation tank, maintaining the pressure for 15-60 min, moving the carbon-containing solution to a vacuum atmosphere carbonization furnace, introducing protective gas, heating the carbon-containing solution to 800-1200 ℃ at the heating rate of 0.1-5 ℃/min, and preserving the heat for 2-10 h to obtain the wood carbon preform.
6. The method of claim 5, wherein the method further comprises: adjusting the porosity of the woody carbon preform by repeating the step S3 for a greater number of times, the less the porosity of the woody carbon preform is, the more the step S3 is repeated, the porosity of the woody carbon preform is 35 to 80%.
7. The method of claim 1, wherein in step S4, the silicon-containing waste is silicon sludge waste and/or coal ash; the mass ratio of the silicon-containing waste to the wood-carbon prefabricated body is (2.5-5.5): 1.
8. the method according to claim 1, wherein the step S4 is specifically: the method comprises the following steps of (1) keeping the temperature of silicon-containing waste materials in an oven at 100-200 ℃ for 10-24 h, drying, laying the dried silicon-containing waste materials at the bottom of a crucible, and placing a wood-carbon prefabricated body on a supporting body in the crucible; and (3) putting the crucible into a vacuum atmosphere sintering furnace, introducing protective gas or vacuumizing, heating to 1300-1800 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 2-5 h to obtain the silicon carbide ceramic.
9. A silicon carbide ceramic prepared according to the method of any one of claims 1-8.
10. The silicon carbide ceramic according to claim 9, wherein the silicon carbide ceramic has a porosity of 2 to 70%.
CN202111621742.2A 2021-12-28 2021-12-28 Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic Pending CN114394844A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111621742.2A CN114394844A (en) 2021-12-28 2021-12-28 Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111621742.2A CN114394844A (en) 2021-12-28 2021-12-28 Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic

Publications (1)

Publication Number Publication Date
CN114394844A true CN114394844A (en) 2022-04-26

Family

ID=81228342

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111621742.2A Pending CN114394844A (en) 2021-12-28 2021-12-28 Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic

Country Status (1)

Country Link
CN (1) CN114394844A (en)

Citations (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1049082A (en) * 1964-04-16 1966-11-23 Siemens Planiawerke Ag An electrical heating element of silicon carbide and a method of making such a heating element
US4154787A (en) * 1977-07-25 1979-05-15 Coors Porcelain Company Method for manufacturing silicon carbide bodies
JPS6325273A (en) * 1986-07-17 1988-02-02 イ−グル工業株式会社 Manufacture of silicon carbide-carbonaceous composite formed body
JPH0558731A (en) * 1991-09-04 1993-03-09 Kawasaki Steel Corp Production of carbon fiber reinforced carbon composite material consisting of two kinds of carbons having internal structures different from each other in parent phase
US6051096A (en) * 1996-07-11 2000-04-18 Nagle; Dennis C. Carbonized wood and materials formed therefrom
US20030132540A1 (en) * 2002-01-11 2003-07-17 Gardner Slade H. Method of forming ecoceramic-based silicon-carbide tooling for composites and method for forming composites using same
CN1617840A (en) * 2001-12-12 2005-05-18 申克碳化技术股份有限公司 Method for the production of a carbon or ceramic component
CN1850730A (en) * 2006-05-26 2006-10-25 中国科学院上海硅酸盐研究所 Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology
US20090209405A1 (en) * 2008-02-19 2009-08-20 University Of Central Florida Research Foundation, Inc. Method for Synthesizing Bulk Ceramics and Structures from Polymeric Ceramic Precursors
WO2010133641A2 (en) * 2009-05-19 2010-11-25 Skz-Kfe Ggmbh Kunststoff-Forschung Und -Entwicklung Method for producing a sic ceramic component
CN102442826A (en) * 2011-09-30 2012-05-09 景德镇陶瓷学院 Silicon carbide composite ceramic prepared by using photovoltaic silicon cutting wastes and manufacturing method thereof
CN102503430A (en) * 2011-09-23 2012-06-20 中国科学院上海硅酸盐研究所 Method for preparing reaction-sintered silicon carbide ceramic by improved tape casting process
CN102898165A (en) * 2012-11-07 2013-01-30 宜昌科博耐火材料有限公司 SiSiC high-temperature ceramic furnace bottom plate for annular furnace and preparation method for bottom plate
CN103359736A (en) * 2013-07-17 2013-10-23 海南大学 Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar
CN103803982A (en) * 2014-02-27 2014-05-21 中原工学院 Preparation method of rice hull stacked porous silicon carbide
CN104230367A (en) * 2014-09-10 2014-12-24 武汉科技大学 SiC-ZrC-ZrB2 nano complex phase ceramic modified C/C composite material and preparation method thereof
CN105565814A (en) * 2015-11-30 2016-05-11 陕西聚洁瀚化工有限公司 Method for producing silicon carbide (SiC) ceramics by polysilicon wire-electrode cutting scraps
CN106977235A (en) * 2017-04-07 2017-07-25 东北大学 A kind of method for preparing Si SiC antioxidant coatings in carbon material surface
DE102016004060A1 (en) * 2016-04-08 2017-10-12 Markus Holzbach Process for producing silicided articles and these silicated articles
CN107879757A (en) * 2017-11-21 2018-04-06 北京林业大学 A kind of preparation method of toughness reinforcing lignin-base silicon carbide woodceramics base substrate
WO2018177294A1 (en) * 2017-03-27 2018-10-04 储晞 Method, apparatus, and system for producing silicon-containing product by utilizing silicon mud byproduct of cutting silicon material with diamond wire
CN110171976A (en) * 2019-05-27 2019-08-27 华中科技大学 The preparation method and product of SiC base ceramic part based on increasing material manufacturing
CN112093801A (en) * 2020-05-11 2020-12-18 武汉科技大学 Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof
CN112877778A (en) * 2021-03-12 2021-06-01 哈尔滨晶彩材料科技有限公司 Protective special-shaped graphite crucible and using method thereof
CN113248272A (en) * 2021-05-11 2021-08-13 广州三的投资管理企业（有限合伙） Preparation method and application of carbon-ceramic friction material
CN113387724A (en) * 2021-06-10 2021-09-14 西北工业大学 High-temperature-resistant long-life composite coating on surface of carbon/carbon composite material and preparation method thereof
CN113788701A (en) * 2021-09-07 2021-12-14 华中科技大学 Preparation method and product of 3D printing lignocellulose derived silicon carbide ceramic

Patent Citations (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1049082A (en) * 1964-04-16 1966-11-23 Siemens Planiawerke Ag An electrical heating element of silicon carbide and a method of making such a heating element
US4154787A (en) * 1977-07-25 1979-05-15 Coors Porcelain Company Method for manufacturing silicon carbide bodies
JPS6325273A (en) * 1986-07-17 1988-02-02 イ−グル工業株式会社 Manufacture of silicon carbide-carbonaceous composite formed body
JPH0558731A (en) * 1991-09-04 1993-03-09 Kawasaki Steel Corp Production of carbon fiber reinforced carbon composite material consisting of two kinds of carbons having internal structures different from each other in parent phase
US6051096A (en) * 1996-07-11 2000-04-18 Nagle; Dennis C. Carbonized wood and materials formed therefrom
CN1617840A (en) * 2001-12-12 2005-05-18 申克碳化技术股份有限公司 Method for the production of a carbon or ceramic component
US20030132540A1 (en) * 2002-01-11 2003-07-17 Gardner Slade H. Method of forming ecoceramic-based silicon-carbide tooling for composites and method for forming composites using same
CN1850730A (en) * 2006-05-26 2006-10-25 中国科学院上海硅酸盐研究所 Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology
US20090209405A1 (en) * 2008-02-19 2009-08-20 University Of Central Florida Research Foundation, Inc. Method for Synthesizing Bulk Ceramics and Structures from Polymeric Ceramic Precursors
WO2010133641A2 (en) * 2009-05-19 2010-11-25 Skz-Kfe Ggmbh Kunststoff-Forschung Und -Entwicklung Method for producing a sic ceramic component
CN102503430A (en) * 2011-09-23 2012-06-20 中国科学院上海硅酸盐研究所 Method for preparing reaction-sintered silicon carbide ceramic by improved tape casting process
CN102442826A (en) * 2011-09-30 2012-05-09 景德镇陶瓷学院 Silicon carbide composite ceramic prepared by using photovoltaic silicon cutting wastes and manufacturing method thereof
CN102898165A (en) * 2012-11-07 2013-01-30 宜昌科博耐火材料有限公司 SiSiC high-temperature ceramic furnace bottom plate for annular furnace and preparation method for bottom plate
CN103359736A (en) * 2013-07-17 2013-10-23 海南大学 Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar
CN103803982A (en) * 2014-02-27 2014-05-21 中原工学院 Preparation method of rice hull stacked porous silicon carbide
CN104230367A (en) * 2014-09-10 2014-12-24 武汉科技大学 SiC-ZrC-ZrB2 nano complex phase ceramic modified C/C composite material and preparation method thereof
CN105565814A (en) * 2015-11-30 2016-05-11 陕西聚洁瀚化工有限公司 Method for producing silicon carbide (SiC) ceramics by polysilicon wire-electrode cutting scraps
DE102016004060A1 (en) * 2016-04-08 2017-10-12 Markus Holzbach Process for producing silicided articles and these silicated articles
WO2018177294A1 (en) * 2017-03-27 2018-10-04 储晞 Method, apparatus, and system for producing silicon-containing product by utilizing silicon mud byproduct of cutting silicon material with diamond wire
CN106977235A (en) * 2017-04-07 2017-07-25 东北大学 A kind of method for preparing Si SiC antioxidant coatings in carbon material surface
CN107879757A (en) * 2017-11-21 2018-04-06 北京林业大学 A kind of preparation method of toughness reinforcing lignin-base silicon carbide woodceramics base substrate
CN110171976A (en) * 2019-05-27 2019-08-27 华中科技大学 The preparation method and product of SiC base ceramic part based on increasing material manufacturing
CN112093801A (en) * 2020-05-11 2020-12-18 武汉科技大学 Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof
CN112877778A (en) * 2021-03-12 2021-06-01 哈尔滨晶彩材料科技有限公司 Protective special-shaped graphite crucible and using method thereof
CN113248272A (en) * 2021-05-11 2021-08-13 广州三的投资管理企业（有限合伙） Preparation method and application of carbon-ceramic friction material
CN113387724A (en) * 2021-06-10 2021-09-14 西北工业大学 High-temperature-resistant long-life composite coating on surface of carbon/carbon composite material and preparation method thereof
CN113788701A (en) * 2021-09-07 2021-12-14 华中科技大学 Preparation method and product of 3D printing lignocellulose derived silicon carbide ceramic

Non-Patent Citations (12)

* Cited by examiner, † Cited by third party
Title
JUN-MIN QIAN ET AL.: "Porous SiC ceramics fabricated by reactive infiltration of gaseous silicon into charcoal", 《CERAMIC INTERNATIONAL》, vol. 30, no. 6, 10 March 2004 (2004-03-10), pages 948, XP004516837, DOI: 10.1016/j.ceramint.2003.11.001 *
严自力等: "碳化硅木质陶瓷的研究进展", 《硅酸盐学报》 *
严自力等: "碳化硅木质陶瓷的研究进展", 《硅酸盐学报》, no. 12, 15 December 2008 (2008-12-15), pages 1797 - 1802 *
刘景林: "利用自结合碳化硅制造的结构材料", 《耐火与石灰》 *
刘景林: "利用自结合碳化硅制造的结构材料", 《耐火与石灰》, no. 05, 10 October 2007 (2007-10-10), pages 27 *
吴添: "激光3D打印碳化硅陶瓷粉末及反应熔渗工艺的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
吴添: "激光3D打印碳化硅陶瓷粉末及反应熔渗工艺的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 7, 15 July 2020 (2020-07-15), pages 16 - 18 *
孙一唐 等译: "《金属和合金的化学热处理手册》", 上海科学技术出版社, pages: 174 - 326 *
朱振峰等: "生物模板法制备多孔陶瓷的研究进展", 《材料导报》 *
朱振峰等: "生物模板法制备多孔陶瓷的研究进展", 《材料导报》, no. 21, 10 November 2009 (2009-11-10), pages 50 - 54 *
金星等: "晶体硅金刚线切割废料制备高纯氮化硅", 《应用化学》 *
金星等: "晶体硅金刚线切割废料制备高纯氮化硅", 《应用化学》, no. 11, 10 November 2018 (2018-11-10), pages 95 - 102 *

Similar Documents

Publication Publication Date Title
CN100395211C (en) Method for preparing porous silicon carbide ceramic with high porosity
CN108865195B (en) Method for preparing high-strength carbon material from biomass
EP3227109B1 (en) Process for making densified carbon articles by three dimensional printing
CN100374367C (en) Technical method and schedule for preparation of foam carbon material used asphalt as raw material
CN109970038B (en) Method for producing mesocarbon microbeads by using medium-low temperature coal tar as raw material
CN107010985A (en) A kind of Carbon fibe enhancing ceramic matrix friction material of the phase containing Ti3SiC2 and preparation method thereof
CN108383100B (en) CH (physical channel)4/N2Preparation method of carbon molecular sieve for separation
CN107399983A (en) A kind of silicon carbide reaction-sintered foamed ceramics and preparation method thereof
CN113307646B (en) High-heat-conductivity and high-purity graphite-based composite material and preparation method thereof
CN104817337A (en) Multi-scale-structure SiC/C porous composite ceramic and preparation method thereof
CN109110759A (en) A kind of preparation method of nitrogen, boron codope porous carbon materials
CN110846718B (en) Method for preparing silicon carbide nano crystal whisker by utilizing mixed silicon source
KR101257458B1 (en) Manufacturing Method of Sintered SiC Regenerative Materials From Silicon Sludge
CN110550618A (en) Device and method for recovering tail gas of CVI/CVD (chemical vapor deposition/chemical vapor deposition) process
CN113716975B (en) Method for preparing wood biomass porous silicon carbide through 3D printing and porous silicon carbide
CN114394844A (en) Method for preparing silicon carbide ceramic by 3D printing of waste and silicon carbide ceramic
CN103253671B (en) Method for preparing SiC nanowire
CN1640847A (en) Simple carbon/carborundum composite material manufacturing method
Wu et al. Effect of ZrC content on the properties of biomorphic C–ZrC–SiC composites prepared using hybrid precursors of novel organometallic zirconium polymer and polycarbosilane
CN105780123A (en) Hafnium-carbide nanometer whiskers and preparing method thereof
CN114804073A (en) Biomass carbon nanotube and preparation method and application thereof
CN117945775B (en) C (C)fPreparation method of ZrC ceramic composite material
CN117509638B (en) Method and system for continuously preparing silicon-carbon material by coupling organic solid waste and silicon-rich solid waste
CN114984766B (en) Preparation method of carbon film with self-adhesion performance and obtained carbon film
CN109553084A (en) A method of the high-intensitive blocky porous charcoal of pyrolysis preparation

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20220426