CN113248258A - Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof - Google Patents

Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof Download PDF

Info

Publication number
CN113248258A
CN113248258A CN202110535695.3A CN202110535695A CN113248258A CN 113248258 A CN113248258 A CN 113248258A CN 202110535695 A CN202110535695 A CN 202110535695A CN 113248258 A CN113248258 A CN 113248258A
Authority
CN
China
Prior art keywords
phase
silicon carbide
powder
ceramic material
sic
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
Application number
CN202110535695.3A
Other languages
Chinese (zh)
Other versions
CN113248258B (en
Inventor
黄政仁
祝明
陈健
郑嘉棋
陈文辉
马宁宁
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.)
Shanghai Institute of Ceramics of CAS
Original Assignee
Shanghai Institute of Ceramics of CAS
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 Shanghai Institute of Ceramics of CAS filed Critical Shanghai Institute of Ceramics of CAS
Priority to CN202110535695.3A priority Critical patent/CN113248258B/en
Publication of CN113248258A publication Critical patent/CN113248258A/en
Application granted granted Critical
Publication of CN113248258B publication Critical patent/CN113248258B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24SSOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
    • F24S70/00Details of absorbing elements
    • F24S70/10Details of absorbing elements characterised by the absorbing material
    • F24S70/16Details of absorbing elements characterised by the absorbing material made of ceramic; made of concrete; made of natural stone
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3804Borides
    • C04B2235/3813Refractory metal borides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3817Carbides
    • C04B2235/3821Boron carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/421Boron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422Carbon
    • C04B2235/424Carbon black
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/40Solar thermal energy, e.g. solar towers
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/40Solar thermal energy, e.g. solar towers
    • Y02E10/46Conversion of thermal power into mechanical power, e.g. Rankine, Stirling or solar thermal engines

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Sustainable Development (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Sustainable Energy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Ceramic Products (AREA)

Abstract

The invention relates to a silicon carbide-based composite ceramic material with high spectral selectivity and a preparation method and application thereof; the silicon carbide-based composite ceramic material has a main phase of SiC and a second phase of TiB2And/or ZrB2(ii) a Preferably, the main phase content in the main phase and the second phase is 50vol% to 100 vol%; the second phase content is 0vol% to 50 vol%.

Description

Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof
Technical Field
The invention relates to a silicon carbide-based composite ceramic material with high spectral selectivity and a preparation method and application thereof, belonging to the technical field of solar thermal power generation.
Background
The exhaustion of energy and the pollution to the environment in the process of energy utilization are problems which need to be solved urgently by people at present. Solar energy is used as a novel clean energy source, is inexhaustible, and plays a very important role in solving the problem of energy crisis.
Solar energy can be effectively converted into electric energy which can be used by human beings through a solar thermal power generation technology. Among these, the heat absorber is a key component of a solar thermal power generation system, which transfers the energy of solar radiation to a heat transfer fluid, which is used for thermodynamic cycle power generation. However, due to the substantial heat losses (mainly thermal radiation, and also thermal and convection) in the actual heat transfer process, the solar energy received by the absorber is not completely transferred to the heat transfer fluid. Therefore, the development of absorber materials with high solar absorption coefficient α (0.3-2.5 μm) and low emissivity ε (2.5-16 μm) is one of the important issues to be solved in solar thermal power generation technology.
The silicon carbide ceramic has very high solar energy absorption coefficient, and simultaneously has excellent performances of high thermal conductivity, good high-temperature oxidation resistance, excellent high-temperature mechanical property and the like, so that the silicon carbide ceramic can be used as a solar energy heat absorption material. However, the high heat radiation properties of silicon carbide ceramics tend to dissipate the absorbed energy as heat radiation, which compromises its practical effectiveness in use. Therefore, the method has important significance for improving the spectral selectivity alpha/epsilon of the silicon carbide ceramic.
Disclosure of Invention
Aiming at the problem that the spectrum selectivity of the silicon carbide ceramic is too low when the silicon carbide ceramic is applied to a solar heat absorption material, the invention provides a silicon carbide complex phase ceramic material with high spectrum selectivity and a preparation method and application thereof.
In a first aspect, the invention provides a silicon carbide complex phase ceramic material with high spectral selectivity, wherein the main phase of the silicon carbide complex phase ceramic material is SiC, and the second phase is TiB2And/or ZrB2(ii) a Preferably, of said main and second phases, mainThe phase content is 50vol% -100 vol%; the second phase content is 0vol% to 50 vol%.
Selection of TiB2And ZrB2The spectral selectivity of silicon carbide ceramic as the second phase material is adjusted because it has a very low infrared emissivity. When the SiC is compounded with the silicon carbide, the advantages of high solar energy absorption rate, high heat conduction, excellent oxidation resistance and the like of the SiC and the low infrared radiance of a second phase can be integrated, so that the high spectrum selective solar heat absorber material with excellent comprehensive performance is prepared.
Preferably, the silicon carbide-based composite ceramic material further comprises a B-C system sintering aid; the content of the main phase and the second phase is 90-96 wt%; the B-C system sintering aid accounts for 4-10wt% of the total raw materials, and the sum of the components is 100%.
The spectral selectivity of the pure solid phase silicon carbide ceramic was 1.424. When the content of the second phase is more than 0 and less than or equal to 5vol percent, the emissivity of SiC is extremely low in a wave band of 11-13 mu m, and TiB2/ZrB2The emissivity of (a) is relatively high, which causes a small amount (0-5 vol%) of second phase recombination to exhibit an increase in emissivity of the composite material, resulting in a decrease in selectivity. When 5 vol% of TiB is doped2Then the spectrum selectivity of the complex phase ceramic is 1.403; when 5 vol% ZrB is doped2The spectral selectivity of the complex phase ceramic was 1.398, both of which were reduced compared to the pure solid phase silicon carbide ceramic. When the content of the second phase is less than or equal to 5 vol% and less than or equal to 50vol%, the spectral selectivity of the complex phase ceramic shows an upward trend. In particular, when the second phase is TiB2The spectral selectivity increases from 1.403 to 1.632 with increasing doping; when the second phase is ZrB2The spectral selectivity is improved from 1.398 to 1.549 with the increase of the doping amount.
Preferably, the SiC-TiB produced2The spectrum selectivity alpha/epsilon of the complex phase ceramic material is as follows: 1.403-1.632; produced SiC-ZrB2The spectrum selectivity alpha/epsilon of the complex phase ceramic material is as follows: 1.398-1.549.
In a second aspect, the present invention provides a preparation method of the silicon carbide composite ceramic material with high spectral selectivity, including: mixing the raw materials of SiC powder and TiB2And/or ZrB2Adding the powder and the B-C system sintering aid into absolute ethyl alcohol, adding a binder, and performing ball milling to obtain slurry; drying, crushing and granulating the obtained slurry to obtain mixed powder; and (3) dry-pressing the mixed powder to form, and then performing cold isostatic pressing, negative pressure dewaxing and normal pressure sintering to obtain the composite ceramic block.
Preferably, the grain diameter of the SiC powder is 0.5-1 μm; the TiB2The particle size of the powder is 1-3 μm; the ZrB2The particle size of the powder is 1-3 μm. The finer the particle size of the powder is, the more favorable the sintering densification is, the content of air holes can be reduced, and the mechanical property, the thermal conductivity and the like of a sample are improved.
Preferably, in the B-C system sintering aid, the B source is B4C. At least one of B powder and boric acid; the C source is at least one of phenolic resin, fructose, amorphous carbon and carbon black.
Preferably, the binder is at least one of phenolic resin, PVA and PVB.
Preferably, the ball milling is planetary ball milling for 18-24 hours, so that the powder is as uniform and fine as possible, and sintering can be promoted.
Preferably, the dry pressing forming pressure is 10-20MPa, and the dwell time is 5-15 seconds.
Preferably, the cold isostatic pressure is 150-250MPa, and the pressure maintaining time is 1-3 minutes.
Preferably, the negative pressure dewaxing temperature is 900-.
Preferably, the normal pressure sintering temperature is 2000-2200 ℃, preferably 2100-2200 ℃; the heat preservation time at the highest temperature point is 0.5 to 2 hours; the normal pressure sintering atmosphere is argon atmosphere.
In a third aspect, the invention provides an application of the silicon carbide complex phase ceramic material with high spectral selectivity in a solar heat absorber material.
With increasing content of the second phase (>5 vol%), the spectral selectivity of the sample showed an upward trend; at the same second phase doping amount, TiB2The spectral selectivity is improved to be larger than ZrB2
The silicon carbide-based complex phase ceramic provided by the invention has high solar spectrum selectivity, has the advantages of high inherent thermal conductivity, excellent oxidation resistance and the like of silicon carbide ceramic, can be used as a solar heat absorber material in a solar heat power generation system, and breaks through the inherent application range, namely, is used as structural ceramic. The sintering method adopted by the invention is a solid-phase normal-pressure sintering method, can realize the production of large-batch products, and provides a foundation for the practical large-scale application of the products.
Drawings
FIG. 1 shows different amounts of TiB2And ZrB2The silicon carbide-based complex phase ceramic has spectral selectivity.
Detailed Description
The present invention is further described below in conjunction with the following embodiments, which are intended to illustrate and not to limit the present invention.
The invention selects TiB with low infrared emissivity2And ZrB2As a second phase, the spectral selectivity of the silicon carbide ceramic is adjusted by solid phase sintering. And the silicon carbide is used as a main phase, and the inherent excellent performances of the silicon carbide, such as high thermal conductivity, excellent oxidation resistance and the like, can be combined, so that the high spectrum selective solar heat absorber material with excellent comprehensive performance is prepared. And the sintering mode of normal pressure sintering provides a foundation for the large-scale production of products.
The following exemplary illustrates a method for preparing a silicon carbide-based complex phase ceramic with high solar spectrum selectivity provided by the present invention:
preparing raw materials, mixing the raw materials, and performing ball milling to obtain mixed slurry. Weighing SiC powder and TiB according to formula of high-spectrum selective silicon carbide ceramic2And/or ZrB2The powder is used as main raw material powder, and B-C system raw materials are added as sintering aids. The raw materials are weighed and then mixed into absolute ethyl alcohol, a binder is added, and then silicon carbide balls are added as ball milling media to be ball milled on a planetary ball mill for a period of time to obtain mixed slurry. Wherein, the grain diameter of the SiC powder can be 0.5-1 μm; TiB2The particle diameter of the powder canIs 1-3 μm; ZrB2The particle size of the powder can be 1-3 μm. The above SiC and TiB2/ZrB2The mass ratio of the main raw material powder to the total raw materials can be 90-96wt%, and in the part, the SiC dosage can be 50-100 vol%; TiB2/ZrB2The proportion of the dosage can be 0vol% to 50 vol%. The source B in the sintering aid can be B4C. One or more of B powder and boric acid, and C source can be one or more of phenolic resin, fructose, amorphous carbon and carbon black. The B-C system sintering aid accounts for 4-10wt% of the total raw materials. The binder is one or more of phenolic resin, PVA and PVB. The binder is added additionally and is used in an amount of about 2-10 wt% of the mass of the raw material. The mixing time can be 12-24 hours, preferably 18-24 hours, so as to obtain uniform and fine powder as far as possible and promote the sintering process.
Drying, crushing, granulating, dry pressing, cold isostatic pressing and other processes to obtain a green body sample. Wherein the drying condition can be drying at 60-100 deg.C for 12-36 hr. The crushing method can be manual grinding or mechanical crushing. The granulation method can be spray granulation or nylon sieving; the dry pressing forming pressure can be 10-20MPa, and the pressure maintaining time can be 5-15 seconds; the cold isostatic pressure can be 150-250MPa, and the pressure maintaining time can be 1-3 minutes.
And (4) dewaxing under negative pressure and sintering under normal pressure to obtain the high solar spectrum selectivity ceramic sample. Wherein the negative pressure dewaxing temperature can be 900-; the normal pressure sintering temperature can be 2000-2200 ℃, the temperature is preferably 2100-2200 ℃, and the holding time can be 0.5-2 hours.
The ceramic sample is processed into a wafer with the diameter of 35mm and the thickness of 3mm, and both sides of the wafer are ground flat to test the solar absorptivity (alpha) and the thermal emissivity (epsilon), and the spectral selectivity (alpha/epsilon) is calculated.
The test results are: the spectral selectivity of the pure solid phase silicon carbide ceramic was 1.424. When the content of the second phase is more than 0 and less than or equal to 5 vol%, the spectral selectivity shows a decreasing tendency. Because the emissivity of SiC is very low in the 11-13 μm band, while TiB2/ZrB2The emissivity of (A) is relatively high, which allows a small amount (0-5 vol%) of second phases to recombineThe composite emissivity then appears to increase, resulting in a decrease in selectivity. When 5 vol% of TiB is doped2Then the spectrum selectivity of the complex phase ceramic is 1.403; when 5 vol% ZrB is doped2The spectral selectivity of the complex phase ceramic was 1.398, both of which were reduced compared to the pure solid phase silicon carbide ceramic. When the content of the second phase is less than or equal to 5 vol% and less than or equal to 50vol%, the spectral selectivity of the complex phase ceramic shows an upward trend. In particular, when the second phase is TiB2The spectral selectivity increases from 1.403 to 1.632 with increasing doping; when the second phase is ZrB2The spectral selectivity is improved from 1.398 to 1.549 with the increase of the doping amount.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention.
Example 1
Preparing pure solid phase sintered silicon carbide ceramic. 188g of SiC powder is weighed as a raw material, 2g B4The C powder is a boron source, 4g of carbon black is used as one of carbon sources, and 20g of phenolic resin solution is added to be used as a binder and the carbon source to form all the raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.424 through testing and calculation.
Example 2
Preparation of a second phase of 5 vol% TiB2The silicon carbide-based composite ceramic. 150g of SiC powder and 11.1g of TiB were weighed2Is used as a main raw material, namely SiC accounts for 95 vol%, TiB2The content ratio was 5 vol%. 1.17g B was additionally added4The C powder is a boron source, 3.43g of carbon black is used as one of carbon sources, and 17.14g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.403 through testing and calculation.
Example 3
Preparation of a second phase of 5 vol% ZrB2The silicon carbide-based composite ceramic. 150g of SiC powder and 15.05g of ZrB were weighed2Is used as main raw material, namely SiC accounts for 95 vol%, ZrB2The content ratio was 5 vol%. 1.76g B was additionally added4The C powder is a boron source, 3.51g of carbon black is used as one of carbon sources, and 17.56g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.398 through testing and calculation.
Example 4
Preparation of a second phase of 15 vol% TiB2The silicon carbide-based composite ceramic. 135g of SiC powder and 33.5g of TiB were weighed2Is used as a main raw material, namely SiC accounts for 85vol percent of the SiC and TiB2The content ratio is 15 vol%. 1.79g B was additionally added4The C powder is a boron source, 3.59g of carbon black is used as one of carbon sources, and 17.93g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. Will be provided withAll the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.43 through testing and calculation.
Example 5
Preparation of a second phase of 15 vol% ZrB2The silicon carbide-based composite ceramic. 135g of SiC powder and 45.41g of ZrB were weighed2Is used as a main raw material, namely SiC accounts for 85 vol% of the SiC and ZrB2The content ratio is 15 vol%. 1.92g B was additionally added4The C powder is a boron source, 3.84g of carbon black is used as one of carbon sources, and 19.19g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.43 through testing and calculation.
Example 6
Preparation of a second phase of 25 vol% TiB2The silicon carbide-based composite ceramic. Weighing 120g of SiC powder and 56.25g of TiB2Is used as a main raw material, namely SiC accounts for 75 vol% of the SiC and TiB2The content ratio is 25 vol%. 1.88g B was additionally added4The C powder is a boron source, 3.75g of carbon black is used as one of carbon sources, and 18.75g of phenolic resin solution is added to be used as a binder and the carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtainTo a mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample was measured and calculated to be 1.499.
Example 7
Preparation of a second phase of 25 vol% ZrB2The silicon carbide-based composite ceramic. Weighing 120g of SiC powder and 76.25g of ZrB2Is taken as a main raw material, namely SiC accounts for 75 vol% of the SiC and ZrB2The content ratio is 25 vol%. 2.09g B was additionally added4The C powder is a boron source, 4.18g of carbon black is used as one of carbon sources, and 20.88g of phenolic resin solution is added to be used as a binder and the carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.464 by testing and calculation.
Example 8
Preparation of a second phase of 35 vol% TiB2The silicon carbide-based composite ceramic. Weighing 100g of SiC powder, 75.72g of TiB2Is used as a main raw material, namely SiC accounts for 65vol percent and TiB2The content ratio was 35 vol%. 1.87g B was additionally added4The C powder is a boron source, 3.74g of carbon black is used as one of carbon sources, and 18.69g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. Dry pressing the mixed powder at 15MPa for 15 seconds, cold isostatic pressing at 200MPa for 3 minAnd (5) obtaining a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.525 through testing and calculation.
Example 9
Preparation of a second phase of 35 vol% ZrB2The silicon carbide-based composite ceramic. Weighing 100g of SiC powder, 102.64g of ZrB2As the main raw material, namely SiC accounting for 65 vol% of the two, ZrB2The content ratio was 35 vol%. 2.16g B was additionally added4The C powder is a boron source, 4.31g of carbon black is used as one of carbon sources, and 21.56g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.476 after testing and calculation.
Example 10
Preparation of a second phase of 50vol% TiB2The silicon carbide-based composite ceramic. Weighing 85g of SiC powder, 119.53g of TiB2Is used as a main raw material, namely SiC accounts for 50vol% of the SiC and TiB2The content ratio is 50 vol%. 2.18g B was additionally added4The C powder is a boron source, 4.35g of carbon black is used as one of carbon sources, and 21.76g of phenolic resin solution is added to be used as a binder and a carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. The green body sample is subjected to negative pressure dewaxing after being subjected to heat preservation at 900 ℃ for 0.5 hour, and then subjected to normal pressure sintering after being subjected to heat preservation at 2200 ℃ for 1 hourAnd obtaining a ceramic sample. The spectral selectivity of the sample is 1.632 through testing and calculation.
Example 11
Preparation of a second phase of 50vol% ZrB2The silicon carbide-based composite ceramic. Weighing 85g of SiC powder and 162.03g of ZrB2Is taken as a main raw material, namely SiC accounts for 50vol% of the SiC and ZrB2The content ratio is 50 vol%. 2.63g B was additionally added4The C powder is a boron source, 5.26g of carbon black is used as one of carbon sources, and 26.28g of phenolic resin solution is added to be used as a binder and the carbon source to form all raw materials. All the raw materials are added into a proper amount of absolute ethyl alcohol, and ball milling is carried out on a planet ball mill for 24 hours to obtain mixed slurry. Drying, crushing, sieving and granulating to obtain mixed powder. And (3) dry-pressing the mixed powder at the pressure of 15MPa for 15 seconds, and then carrying out cold isostatic pressing at the pressure of 200MPa for 3 minutes to obtain a blank sample. And (3) carrying out negative pressure dewaxing on the blank sample at the temperature of 900 ℃ for 0.5 hour, and then carrying out normal pressure sintering at the temperature of 2200 ℃ for 1 hour to obtain the ceramic sample. The spectral selectivity of the sample is 1.549 by testing and calculation.

Claims (10)

1. The silicon carbide complex phase ceramic material with high spectral selectivity is characterized in that the main phase of the silicon carbide complex phase ceramic material is SiC, and the second phase is TiB2And/or ZrB2(ii) a Preferably, the main phase content in the main phase and the second phase is 50vol% to 100 vol%; the second phase content is 0vol% to 50 vol%.
2. The silicon carbide composite ceramic material with high spectral selectivity of claim 1, further comprising a B-C system sintering aid; the content of the main phase and the second phase is 90-96 wt%; the B-C system sintering aid accounts for 4-10wt% of the total raw materials, and the sum of the components is 100%.
3. The silicon carbide composite ceramic material with high spectral selectivity of claim 1 or 2, wherein the SiC-TiB is prepared2The spectrum selectivity alpha/epsilon of the complex phase ceramic material is as follows: 1.403-1.632; produced SiC-ZrB2The spectrum selectivity alpha/epsilon of the complex phase ceramic material is as follows: 1.398-1.549.
4. A method for preparing a silicon carbide composite ceramic material with high spectral selectivity according to any one of claims 1 to 3, comprising: mixing the raw materials of SiC powder and TiB2And/or ZrB2Adding the powder and the B-C system sintering aid into absolute ethyl alcohol, adding a binder, and performing ball milling to obtain slurry; drying, crushing and granulating the obtained slurry to obtain mixed powder; and (3) dry-pressing the mixed powder to form, and then performing cold isostatic pressing, negative pressure dewaxing and normal pressure sintering to obtain the composite ceramic block.
5. The production method according to claim 4, wherein the particle size of the SiC powder is 0.5 to 1 μm; the TiB2The particle size of the powder is 1-3 μm; the ZrB2The particle size of the powder is 1-3 μm.
6. The method according to claim 4 or 5, wherein the B source in the B-C system sintering aid is B4C. At least one of B powder and boric acid; the C source is at least one of phenolic resin, fructose, amorphous carbon and carbon black.
7. The method of any one of claims 4-6, wherein the binder is at least one of phenolic resin, PVA, and PVB.
8. The production method according to any one of claims 4 to 7, wherein the dry-press molding pressure is 10 to 20MPa, and the dwell time is 5 to 15 seconds; the cold isostatic pressure is 150-250MPa, and the pressure maintaining time is 1-3 minutes.
9. The preparation method according to any one of claims 4 to 8, wherein the negative pressure dewaxing temperature is 900-1100 ℃, and the holding time is 0.5-2 hours; the normal pressure sintering temperature is 2000-2200 ℃, and the preferable temperature is 2100-2200 ℃; the heat preservation time at the highest temperature point is 0.5 to 2 hours; the normal pressure sintering atmosphere is argon atmosphere.
10. Use of a silicon carbide composite ceramic material with high spectral selectivity according to any one of claims 1 to 3 in a solar thermal absorber material.
CN202110535695.3A 2021-05-17 2021-05-17 Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof Active CN113248258B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110535695.3A CN113248258B (en) 2021-05-17 2021-05-17 Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110535695.3A CN113248258B (en) 2021-05-17 2021-05-17 Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN113248258A true CN113248258A (en) 2021-08-13
CN113248258B CN113248258B (en) 2022-09-06

Family

ID=77182373

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110535695.3A Active CN113248258B (en) 2021-05-17 2021-05-17 Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN113248258B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114933484A (en) * 2022-06-14 2022-08-23 武汉科技大学 Toughened SiC-based high-temperature ceramic composite material and preparation method thereof

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0372708A1 (en) * 1988-11-10 1990-06-13 United Kingdom Atomic Energy Authority A method of producing a silicon carbide-based body
US5032550A (en) * 1989-10-13 1991-07-16 Aluminum Company Of America High impact resistant ceramic composite
US20090048087A1 (en) * 2006-05-22 2009-02-19 Zhang Shi C High-density pressurelessly sintered zirconium diboride/silicon carbide composite bodies and a method for producing the same
WO2011063422A1 (en) * 2009-11-23 2011-05-26 Applied Nanostructured Solutions, Llc Ceramic composite materials containing carbon nanotube-infused fiber materials and methods for production thereof
JP2014047105A (en) * 2012-08-31 2014-03-17 Shinano Denki Seiren Kk Method for producing silicon carbide powder
US8995055B1 (en) * 2011-11-21 2015-03-31 The United States Of America As Represented By The Secretary Of The Navy Angular and spectral selective absorber in ultrathin metamaterials
JP2016132607A (en) * 2015-01-21 2016-07-25 新日鐵住金株式会社 Ceramic composite material and manufacturing method therefor
CN106083057A (en) * 2016-06-13 2016-11-09 中国科学院上海硅酸盐研究所 A kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof
CN106083058A (en) * 2016-06-13 2016-11-09 中国科学院上海硅酸盐研究所 A kind of silicon carbide-based complex phase pressure-sensitive ceramic material and preparation method thereof
CN106478105A (en) * 2016-09-26 2017-03-08 西安交通大学 A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon
US20180127630A1 (en) * 2012-09-24 2018-05-10 Purdue Research Foundation High emissivity materials and methods of manufacture
US20210088259A1 (en) * 2015-12-07 2021-03-25 Carbo Ceramics Inc. Ceramic particles for use in a solar power tower

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0372708A1 (en) * 1988-11-10 1990-06-13 United Kingdom Atomic Energy Authority A method of producing a silicon carbide-based body
US5032550A (en) * 1989-10-13 1991-07-16 Aluminum Company Of America High impact resistant ceramic composite
US20090048087A1 (en) * 2006-05-22 2009-02-19 Zhang Shi C High-density pressurelessly sintered zirconium diboride/silicon carbide composite bodies and a method for producing the same
WO2011063422A1 (en) * 2009-11-23 2011-05-26 Applied Nanostructured Solutions, Llc Ceramic composite materials containing carbon nanotube-infused fiber materials and methods for production thereof
US8995055B1 (en) * 2011-11-21 2015-03-31 The United States Of America As Represented By The Secretary Of The Navy Angular and spectral selective absorber in ultrathin metamaterials
JP2014047105A (en) * 2012-08-31 2014-03-17 Shinano Denki Seiren Kk Method for producing silicon carbide powder
US20180127630A1 (en) * 2012-09-24 2018-05-10 Purdue Research Foundation High emissivity materials and methods of manufacture
JP2016132607A (en) * 2015-01-21 2016-07-25 新日鐵住金株式会社 Ceramic composite material and manufacturing method therefor
US20210088259A1 (en) * 2015-12-07 2021-03-25 Carbo Ceramics Inc. Ceramic particles for use in a solar power tower
CN106083057A (en) * 2016-06-13 2016-11-09 中国科学院上海硅酸盐研究所 A kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof
CN106083058A (en) * 2016-06-13 2016-11-09 中国科学院上海硅酸盐研究所 A kind of silicon carbide-based complex phase pressure-sensitive ceramic material and preparation method thereof
CN106478105A (en) * 2016-09-26 2017-03-08 西安交通大学 A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon

Non-Patent Citations (8)

* Cited by examiner, † Cited by third party
Title
CHRISTOS C.AGRAFIOTIS等: "Evaluation of porous silicon carbide monolithic honeycombs as volumetric receivers/collectors of concentrated solar radiation", 《SOLAR ENERGY MATERIALS AND SOLAR CELLS》 *
DILETTA SCITI等: "Suitability of ultra-refractory diboride ceramics as absorbers for solar energy applications", 《SOLAR ENERGY MATERIALS AND SOLAR CELLS》 *
HELENE ARENA等: "effect of TiC incorporation on the optical properties and oxidation resistance of SiC ceramics", 《SOLAR ENERGY MATERIALS AND SOLAR CELLS》 *
KP RANJITH 等: "Development of ZrB 2 -Based Single Layer Absorber Coating and Molten Salt Corrosion of Bulk ZrB 2 –SiC Ceramic for Concentrated Solar Power Application", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 *
MALLIK, M等: "EFFECT OF PARTICULATE VOLUME FRACTION ON MECHANICAL PROPERTIES OF PRESSURELESS SINTERED ZrB2-SiC ULTRA-HIGH TEMPERATURE CERAMIC COMPOSITES", 《PROCESSING AND PROPERTIES OF ADVANCED CERAMICS AND COMPOSITES II》 *
N.AZZALI 等: "Spectral emittance of ceramics for high temperature solar receivers", 《SOLAR ENERGY》 *
凌兴珠等: "原材料特性对SiC-TiB2复合陶瓷性能的影响", 《中南工业大学学报》 *
施浩良: "ZrB2/SiC复合粉末制备及其烧结性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114933484A (en) * 2022-06-14 2022-08-23 武汉科技大学 Toughened SiC-based high-temperature ceramic composite material and preparation method thereof
CN114933484B (en) * 2022-06-14 2023-08-18 武汉科技大学 Toughened SiC-based high-temperature ceramic composite material and preparation method thereof

Also Published As

Publication number Publication date
CN113248258B (en) 2022-09-06

Similar Documents

Publication Publication Date Title
CN106478105A (en) A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon
CN100377378C (en) Method for preparing Bi-Sb-Te series thermoelectric material
CN102633505A (en) Method for preparing high-purity MAX-phase ceramic powder
CN111455205B (en) Preparation method of high-thermal-conductivity low-expansion Diamond-Cu composite material with sandwich structure
CN109553419A (en) A kind of air pressure solid-phase sintering boron carbide complex phase ceramic and preparation method thereof
CN102502539A (en) Method for preparing yttrium-doped nano aluminum nitride powder
CN101565308B (en) Silicon nitride ceramics enhanced by boron nitride nanotube and preparation method thereof
CN108588838B (en) method for preparing SnSe polycrystalline block with high thermoelectric performance
CN112794719A (en) Normal pressure sintered anti-irradiation silicon carbide ceramic material and preparation method thereof
CN113248258B (en) Silicon carbide-based composite ceramic material with high spectral selectivity and preparation method and application thereof
CN110436930A (en) A kind of high-performance nano SiC ceramic and its preparation method and application
CN114573346A (en) Rare earth high-entropy aluminate ceramic selective emitter for thermophotovoltaic and preparation method and application thereof
CN102653470B (en) Cr2AlC ceramic target and preparation method thereof by vacuum hot pressing
CN113354418B (en) High-performance aluminum nitride ceramic substrate prepared by vacuum hot-pressing sintering method and preparation method
CN101724907B (en) Method for preparing single-phase nano crystalline Mn3(Cu0.5Ge0.5)N negative thermal expansion bulk material
CN105642884A (en) Preparation method for Bi-Te-based thermoelectric material with core-shell structure
CN107935598B (en) Low-temperature sintering method of high-performance silicon carbide ceramic material
CN115073186B (en) Silicon nitride ceramic sintered body and preparation method thereof
CN115433007A (en) Solar spectrum wide-frequency absorption material and preparation method thereof
CN108232259B (en) Preparation method of medium-temperature solid fuel cell electrolyte material
CN103642495B (en) Luminescent material with core-shell structure and preparation method thereof
Zhang et al. Effect of Sm2O3 on microstructure and high-temperature stability of MgAl2O4-Si3N4 ceramic for solar thermal absorber
CN104946918A (en) New method for quickly preparing AgInSe2 based thermoelectric material
CN101486564B (en) Preparation of boron nitride nano tube enhanced alumina ceramic
CN111410537B (en) Boron carbide-based complex phase ceramic material with linear conductive characteristic and preparation method thereof

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