CN112010664B - High-thermal-conductivity transparent ceramic and preparation method thereof - Google Patents

High-thermal-conductivity transparent ceramic and preparation method thereof Download PDF

Info

Publication number
CN112010664B
CN112010664B CN202011098605.0A CN202011098605A CN112010664B CN 112010664 B CN112010664 B CN 112010664B CN 202011098605 A CN202011098605 A CN 202011098605A CN 112010664 B CN112010664 B CN 112010664B
Authority
CN
China
Prior art keywords
mass
parts
potassium
sand
transparent ceramic
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.)
Active
Application number
CN202011098605.0A
Other languages
Chinese (zh)
Other versions
CN112010664A (en
Inventor
麦文英
汪加武
叶建明
王礼
石献忠
黄大泱
卢佩玉
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.)
Overland Ceramics Co ltd
Original Assignee
Overland Ceramics Co ltd
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 Overland Ceramics Co ltd filed Critical Overland Ceramics Co ltd
Priority to CN202011098605.0A priority Critical patent/CN112010664B/en
Publication of CN112010664A publication Critical patent/CN112010664A/en
Application granted granted Critical
Publication of CN112010664B publication Critical patent/CN112010664B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • 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
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227Lanthanum oxide or oxide-forming salts thereof
    • 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
    • C04B2235/3427Silicates other than clay, e.g. water glass
    • C04B2235/3463Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
    • 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
    • C04B2235/3427Silicates other than clay, e.g. water glass
    • C04B2235/3463Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3481Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
    • 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
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/442Carbonates
    • 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
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/447Phosphates or phosphites, e.g. orthophosphate, hypophosphite
    • 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
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5276Whiskers, spindles, needles or pins
    • 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
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606Drying
    • 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
    • C04B2235/9607Thermal properties, e.g. thermal expansion coefficient
    • 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
    • C04B2235/9646Optical properties

Abstract

The invention relates to the field of ceramic production, and provides a high-thermal-conductivity transparent ceramic and a preparation method thereof, which are used for solving the problem that a ceramic plate is weak in thermal conductivity. The invention provides a high heat conduction transparent ceramic, which comprises: s10, taking 7-10 parts by mass of sodium sand, 5-8 parts by mass of potassium feldspar, 40-60 parts by mass of alumina powder, 1-3 parts by mass of high-potassium sand, 1-3 parts by mass of potassium-sodium feldspar, 0.5-2 parts by mass of barium carbonate, 10-12 parts by mass of cordierite and 1-3 parts by mass of calcium phosphate; s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing the alumina microspheres and the potassium titanate whiskers with a base material, and uniformly stirring to obtain precursor powder; s30, stamping the precursor powder to form a plate blank; s40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The light transmittance of the ceramic is improved, and the thickness and the heat conductivity of the ceramic are improved.

Description

High-thermal-conductivity transparent ceramic and preparation method thereof
Technical Field
The invention relates to the field of ceramic production, in particular to high-thermal-conductivity transparent ceramic and a preparation method thereof.
Background
According to the definition in the national standard GB/T23266-2009 ceramic plate, the ceramic thin plate mentioned in the invention is made of clay and other inorganic non-metallic materials through the production processes of forming, high-temperature sintering and the like, and has the thickness of not more than 6mm and the area of not less than 1.62m2The plate-like ceramic article of (1). The ceramic thin plate needs to have higher heat conductivity in some use scenes, while the semi-permeable ceramic thin plate has certain disadvantage on the index, and has more damages and high construction and later maintenance costs in application.
The prior transparent ceramics often need higher roasting temperature to improve the light transmittance of the ceramics.
Disclosure of Invention
The invention solves the technical problem of poor heat-conducting property of the ceramic plate and provides the high-heat-conducting transparent ceramic.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the preparation method of the high-thermal-conductivity transparent ceramic comprises the following steps:
s10, taking 7-10 parts by mass of sodium sand, 5-8 parts by mass of potassium feldspar, 40-60 parts by mass of alumina powder, 1-3 parts by mass of high-potassium sand, 1-3 parts by mass of potassium-sodium feldspar, 0.5-2 parts by mass of barium carbonate, 3-5 parts by mass of alumina microspheres, 1-3 parts by mass of potassium titanate whiskers, 10-12 parts by mass of cordierite, 1-3 parts by mass of calcium phosphate, 0.05-0.1 part by mass of yttrium oxide, 0.01-0.05 part by mass of lanthanum oxide and 0.1-0.5 part by mass of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic.
The aluminum oxide powder is used as a main raw material, the existing formula is changed, the sintering temperature is improved, and a sintering aid is introduced: alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide, so that the light transmittance of the plate is improved as much as possible; the whisker and the alumina microsphere are matched to improve the heat-conducting property of the plate as much as possible.
The heat conductivity of the plate is improved, and meanwhile, the light transmittance of the plate is improved.
Preferably, in step S10, 8 to 10 parts by mass of sodium sand, 6 to 8 parts by mass of potassium feldspar, 50 to 60 parts by mass of alumina powder, 2 to 3 parts by mass of high-potassium sand, 2 to 3 parts by mass of potassium-sodium feldspar, 1 to 2 parts by mass of barium carbonate, 4 to 5 parts by mass of alumina microspheres, 2 to 3 parts by mass of potassium titanate whiskers, 11 to 12 parts by mass of cordierite, 2 to 3 parts by mass of calcium phosphate, 0.07 to 0.1 part by mass of yttrium oxide, 0.03 to 0.05 part by mass of lanthanum oxide, and 0.2 to 0.5 part by mass of magnesium oxide.
Preferably, in step S10, 8 parts by mass of sodium sand, 6 parts by mass of potassium feldspar, 50 parts by mass of alumina powder, 2 parts by mass of high-potassium sand, 2 parts by mass of potassium-sodium feldspar, 1 part by mass of barium carbonate, 4 parts by mass of alumina microspheres, 2 parts by mass of potassium titanate whiskers, 11 parts by mass of cordierite, 2 parts by mass of calcium phosphate, 0.07 part by mass of yttrium oxide, 0.03 part by mass of lanthanum oxide, and 0.2 part by mass of magnesium oxide.
Preferably, the particle size of the alumina powder is 10 to 30 nm. The particle size of the alumina powder is optimized to improve the light transmittance of the ceramic.
Preferably, the sintering time is 4-6 h.
Preferably, the preparation method of the alumina microspheres comprises the following steps:
taking 4-5.6 parts by mass of aluminum sulfate, 4.5-6.3 parts by mass of urea and 0.28-78 parts by mass of P1230.2;
mixing aluminum sulfate and urea, adding 25-35 parts by mass of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding an ethanol solution of P123, and continuously stirring for 1 hour to obtain a mixed solution;
and reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h.
Preferably, 4 parts by mass of aluminum sulfate, 4.5 parts by mass of urea and 4.78 parts by mass of P1230.2 are taken.
Preferably, the preparation method of the potassium titanate whisker comprises the following steps:
taking 30-40 parts by mass of stearic acid, 5-12 parts by mass of ethyl titanate and 10-15 parts by mass of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid, adding ethyl titanate after dropwise adding is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker. Can obtain layered potassium tetratitanate crystal whisker, which is combined with cordierite and alumina microsphere and can obviously improve the strength of transparent ceramic after high-temperature firing.
Preferably, 35 parts by mass of stearic acid, 10 parts by mass of ethyl titanate, and 11 parts by mass of a 20% potassium nitrate aqueous solution are taken.
The high-thermal-conductivity transparent ceramic is prepared by the preparation method of the high-thermal-conductivity transparent ceramic.
The inventor finds that inorganic whiskers can improve the mechanical property of the ceramic in the research and development process of transparent ceramics for many years, but the light transmittance or the heat conductivity of the transparent ceramic is difficult to change, and common zinc oxide whiskers, magnesium oxide whiskers, aluminum borate whiskers, silicon carbide whiskers and the like are difficult to improve the light transmittance of the ceramic.
The inventor makes a great deal of attempts to improve the heat-conducting property and the light transmittance of the transparent ceramic, and finds that the combination of the alumina with a certain structure and the potassium titanate whisker has an obvious effect on improving the light transmittance of the ceramic material, can improve the heat-conducting property of the ceramic material at the same time and greatly improves the property of the transparent ceramic. Further, the inventors have found that the light transmittance of the ceramic can be further improved by using layered potassium titanate whiskers in combination with alumina microspheres.
Compared with the prior art, the invention has the beneficial effects that: the light transmittance of the ceramic is improved, and the thickness and the heat conductivity of the ceramic are improved.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1
A highly thermally conductive transparent ceramic comprising:
s10, taking 80g of sodium sand, 60g of potassium feldspar, 500g of alumina powder, 20g of high-potassium sand, 20g of potassium-sodium feldspar, 10g of barium carbonate, 40g of alumina microspheres, 20g of potassium titanate whiskers, 110g of cordierite, 20g of calcium phosphate, 0.70g of yttrium oxide, 0.30g of lanthanum oxide and 2g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h. The preparation method of the alumina microspheres comprises the following steps:
taking 40g of aluminum sulfate, 45g of urea and P1232 g;
mixing aluminum sulfate and urea, adding 250mL of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding 15mL of P123 ethanol solution, and continuously stirring for 1 hour to obtain a mixed solution;
and reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 35g of stearic acid, 10g of ethyl titanate and 11g of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dropwise adding, stirring for 1-2 h, standing, cooling, roasting at 550 ℃ for 2h, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
The aluminum oxide powder is used as a main raw material, the existing formula is changed, the sintering temperature is increased, and a sintering aid is introduced, so that the light transmittance of the plate is improved as much as possible; the whisker and the alumina microsphere are matched to improve the heat-conducting property of the plate as much as possible. The heat conductivity of the plate is improved, and meanwhile, the light transmittance of the plate is improved. The particle size of the alumina powder is optimized to improve the light transmittance of the ceramic. The layered potassium tetratitanate crystal whisker, combined with cordierite and alumina microsphere, can raise the strength of transparent ceramic obviously after high temperature sintering.
Example 2
A highly thermally conductive transparent ceramic comprising:
s10, taking 80g of sodium sand, 60g of potassium feldspar, 500g of alumina powder, 20g of high-potassium sand, 20g of potassium-sodium feldspar, 10g of barium carbonate, 40g of alumina microspheres, 20g of potassium titanate whiskers, 110g of cordierite, 20g of calcium phosphate, 0.70g of yttrium oxide, 0.30g of lanthanum oxide and 2g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h. The preparation method of the alumina microspheres comprises the following steps:
taking 40g of aluminum sulfate, 45g of urea and P1232 g;
mixing aluminum sulfate and urea, adding 250mL of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding 15mL of P123 ethanol solution, and continuously stirring for 1 hour to obtain a mixed solution;
and reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h.
The potassium titanate is potassium hexatitanate.
Example 3
A highly thermally conductive transparent ceramic comprising:
step S10, taking 100g of sodium sand, 80g of potassium feldspar, 600g of alumina powder, 30g of high-potassium sand, 30g of potassium-sodium feldspar, 20g of barium carbonate, 50g of alumina microspheres, 30g of potassium titanate whiskers, 120g of cordierite, 30g of calcium phosphate, 1g of yttrium oxide, 0.5g of lanthanum oxide and 5g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h. The preparation method of the alumina microspheres comprises the following steps:
taking 56g of aluminum sulfate, 63g of urea and P1232.8g;
mixing aluminum sulfate and urea, adding 350mL of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding 21mL of P123 ethanol solution, and continuously stirring for 1h to obtain a mixed solution;
and reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 35g of stearic acid, 10g of ethyl titanate and 11g of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dropwise adding, stirring for 1-2 h, standing, cooling, roasting at 550 ℃ for 2h, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Comparative example 1
A highly thermally conductive transparent ceramic comprising:
s10, taking 80g of sodium sand, 60g of potassium feldspar, 500g of alumina powder, 20g of high-potassium sand, 20g of potassium-sodium feldspar, 10g of barium carbonate, 60g of alumina microspheres, 110g of cordierite, 20g of calcium phosphate, 0.70g of yttrium oxide, 0.30g of lanthanum oxide and 2g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing the alumina microspheres, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h. The preparation method of the alumina microspheres comprises the following steps:
taking 40g of aluminum sulfate, 45g of urea and P1232 g;
mixing aluminum sulfate and urea, adding 250mL of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding 15mL of P123 ethanol solution, and continuously stirring for 1 hour to obtain a mixed solution;
and reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h.
Comparative example 2
A highly thermally conductive transparent ceramic comprising:
s10, taking 80g of sodium sand, 60g of potassium feldspar, 500g of alumina powder, 20g of high-potassium sand, 20g of potassium-sodium feldspar, 10g of barium carbonate, 60g of potassium titanate whisker, 110g of cordierite, 20g of calcium phosphate, 0.70g of yttrium oxide, 0.30g of lanthanum oxide and 2g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing potassium titanate whisker, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 35g of stearic acid, 10g of ethyl titanate and 11g of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dropwise adding, stirring for 1-2 h, standing, cooling, roasting at 550 ℃ for 2h, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Comparative example 3
A highly thermally conductive transparent ceramic comprising:
s10, taking 80g of soda sand, 60g of potassium feldspar, 500g of alumina powder, 20g of high-potassium sand, 20g of potassium-sodium feldspar, 10g of barium carbonate, 40g of flaky alumina, 20g of potassium titanate whisker, 110g of cordierite, 20g of calcium phosphate, 0.70g of yttrium oxide, 0.30g of lanthanum oxide and 2g of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing flaky alumina, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
and S40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain the high-thermal-conductivity transparent ceramic. The particle size of the alumina powder is 10-30 nm. The sintering time is 5 h.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 35g of stearic acid, 10g of ethyl titanate and 11g of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dropwise adding, stirring for 1-2 h, standing, cooling, roasting at 550 ℃ for 2h, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
The plate width of the sheet-shaped alumina particles is 0.5 to 5 μm, and the ratio of the plate width to the plate thickness of the sheet-shaped alumina particles is 5 to 8.
Examples of the experiments
The prepared product was subjected to a heat conductivity test using a heat conductivity tester, and the transmittance of the sample at a wavelength of 700nm (sample thickness polished to 5mm) was measured using an ultraviolet-visible spectrophotometer (model UV-2550, Shimadzu corporation).
TABLE 1 Properties of transparent ceramics according to respective embodiments
Figure DEST_PATH_IMAGE001
The sample used for the test of each example or comparative example had a thickness of 5mm, which was large. However, example 1 also achieves 40% transmittance at a thickness of 5mm, providing the possibility of further increasing the thickness of the transparent ceramic.
The light transmittance of examples 1 and 3 is high, depending on the content of sintering aid and alumina, which in combination with the sintering aid increases the light transmittance to around 40% for the bulk ceramic plate. The transmittance of examples 1 and 3 was significantly improved compared to the comparative examples, because the whiskers of the comparative examples had a certain antagonistic effect with other components of the existing formulation, and a balance between the thermal conductivity and the transmittance could not be established. The whisker structure of the ceramic brick in the embodiment 2 is different from that of the ceramic brick in the embodiment 1, only the alumina microspheres are adopted in the comparative example 1, and the alumina structures in the comparative examples 2 and 3 are different from that of the ceramic brick in the embodiment 1, so that the thermal conductivity of the ceramic brick can be improved only by the alumina with a certain structure and the whiskers with a certain structure, and meanwhile, the light transmittance of the ceramic brick is improved.
The above detailed description is specific to possible embodiments of the present invention, and the above embodiments are not intended to limit the scope of the present invention, and all equivalent implementations or modifications that do not depart from the scope of the present invention should be included in the present claims.

Claims (8)

1. The preparation method of the high-thermal-conductivity transparent ceramic is characterized by comprising the following steps:
s10, taking 7-10 parts by mass of sodium sand, 5-8 parts by mass of potassium feldspar, 40-60 parts by mass of alumina powder, 1-3 parts by mass of high-potassium sand, 1-3 parts by mass of potassium-sodium feldspar, 0.5-2 parts by mass of barium carbonate, 3-5 parts by mass of alumina microspheres, 1-3 parts by mass of potassium titanate whiskers, 10-12 parts by mass of cordierite, 1-3 parts by mass of calcium phosphate, 0.05-0.1 part by mass of yttrium oxide, 0.01-0.05 part by mass of lanthanum oxide and 0.1-0.5 part by mass of magnesium oxide;
s20, mixing soda sand, potassium feldspar, alumina powder, high-potassium sand, potassium-sodium feldspar, barium carbonate, calcium phosphate and cordierite, preparing slurry by adopting wet ball milling, drying and crushing to obtain a base material; mixing alumina microspheres, potassium titanate whiskers, yttrium oxide, lanthanum oxide and magnesium oxide with a base material, and uniformly stirring to obtain precursor powder;
s30, stamping the precursor powder to form a plate blank;
s40, drying the plate blank until the water content is lower than 1%, and then sintering the plate blank in a kiln at 1600-1700 ℃ to obtain high-thermal-conductivity transparent ceramic;
the preparation method of the alumina microspheres comprises the following steps:
taking 4-5.6 parts by mass of aluminum sulfate, 4.5-6.3 parts by mass of urea and 0.28-78 parts by mass of P1230.2;
mixing aluminum sulfate and urea, adding 25-35 parts by mass of water, stirring until the aluminum sulfate and the urea are completely dissolved, adding an ethanol solution of P123, and continuously stirring for 1 hour to obtain a mixed solution;
reacting the mixed solution at 150-200 ℃ for 12h, cooling, filtering, washing, drying, and roasting at 500-600 ℃ for 4 h;
the preparation method of the potassium titanate whisker comprises the following steps:
taking 30-40 parts by mass of stearic acid, 5-12 parts by mass of ethyl titanate and 10-15 parts by mass of a 20% potassium nitrate aqueous solution;
dropwise adding 20% potassium nitrate aqueous solution into molten stearic acid, adding ethyl titanate after dropwise adding is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
2. The method for preparing a transparent ceramic with high thermal conductivity according to claim 1, wherein in step S10, 8 to 10 parts by mass of sodium sand, 6 to 8 parts by mass of potassium feldspar, 50 to 60 parts by mass of alumina powder, 2 to 3 parts by mass of high potassium sand, 2 to 3 parts by mass of potassium-sodium feldspar, 1 to 2 parts by mass of barium carbonate, 4 to 5 parts by mass of alumina microspheres, 2 to 3 parts by mass of potassium titanate whiskers, 11 to 12 parts by mass of cordierite, 2 to 3 parts by mass of calcium phosphate, 0.07 to 0.1 part by mass of yttrium oxide, 0.03 to 0.05 part by mass of lanthanum oxide, and 0.2 to 0.5 part by mass of magnesium oxide.
3. The method for preparing a transparent ceramic with high thermal conductivity according to claim 2, wherein in step S10, 8 parts by mass of soda sand, 6 parts by mass of potassium feldspar, 50 parts by mass of alumina powder, 2 parts by mass of high-potassium sand, 2 parts by mass of potassium-sodium feldspar, 1 part by mass of barium carbonate, 4 parts by mass of alumina microspheres, 2 parts by mass of potassium titanate whiskers, 11 parts by mass of cordierite, 2 parts by mass of calcium phosphate, 0.07 part by mass of yttrium oxide, 0.03 part by mass of lanthanum oxide, and 0.2 part by mass of magnesium oxide.
4. The method for preparing a transparent ceramic with high thermal conductivity according to claim 1, wherein the alumina powder has a particle size of 10 to 30 nm.
5. The method for preparing the transparent ceramic with high thermal conductivity according to claim 1, wherein the firing time is 4-6 hours.
6. The method for preparing transparent ceramic with high thermal conductivity according to claim 1, wherein the aluminum sulfate is taken in an amount of 4 parts by mass, the urea is taken in an amount of 4.5 parts by mass, and the P1230.2 parts by mass.
7. The method for producing a transparent ceramic having high thermal conductivity according to claim 1, wherein 35 parts by mass of stearic acid, 10 parts by mass of ethyl titanate, and 11 parts by mass of a 20% potassium nitrate aqueous solution are taken.
8. The high thermal conductivity transparent ceramic is characterized by being prepared by the preparation method of the high thermal conductivity transparent ceramic according to any one of claims 1 to 7.
CN202011098605.0A 2020-10-14 2020-10-14 High-thermal-conductivity transparent ceramic and preparation method thereof Active CN112010664B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011098605.0A CN112010664B (en) 2020-10-14 2020-10-14 High-thermal-conductivity transparent ceramic and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011098605.0A CN112010664B (en) 2020-10-14 2020-10-14 High-thermal-conductivity transparent ceramic and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112010664A CN112010664A (en) 2020-12-01
CN112010664B true CN112010664B (en) 2021-02-12

Family

ID=73527911

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011098605.0A Active CN112010664B (en) 2020-10-14 2020-10-14 High-thermal-conductivity transparent ceramic and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112010664B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112441845B (en) * 2020-12-16 2022-07-22 广东欧文莱陶瓷有限公司 Preparation method of low-color-difference ceramic
CN113443924B (en) * 2021-09-02 2021-11-26 广东欧文莱陶瓷有限公司 Ceramic sheet and preparation method thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306943A (en) * 2008-06-27 2008-11-19 王昕� Fine-crystal transparent alumina ceramic of high straight-line luminous transmittance and method for preparing same
CN102839413B (en) * 2012-09-18 2015-04-08 武汉理工大学 Method for preparing ultrathin layered K2Ti4O9 crystal whiskers
CN104355651B (en) * 2014-10-16 2016-08-24 佛山市禾才科技服务有限公司 A kind of high intensity semi permeability ceramic material and the preparation method of ceramic thin plate
CN106673030B (en) * 2015-11-05 2018-01-16 中国石油化工股份有限公司大连石油化工研究院 A kind of alumina hollow ball and preparation method thereof
CN105819862A (en) * 2016-04-25 2016-08-03 岳西县吉奥电子器件有限公司 Potassium titanate whisker toughened silicon carbide-based ceramic circuit board substrate material and preparation method thereof

Also Published As

Publication number Publication date
CN112010664A (en) 2020-12-01

Similar Documents

Publication Publication Date Title
CN112010664B (en) High-thermal-conductivity transparent ceramic and preparation method thereof
CN100491285C (en) Alumina ceramic and preparation method thereof
CN100486932C (en) High-purity corundum pouring material containing nano calcium carbonate and preparation method thereof
CN112299833B (en) High-strength high-toughness mullite ceramic sheet and preparation method thereof
CN104829218B (en) Bimodal active alumina micropowder and preparation method
CN107434410B (en) Preparation method of cordierite ceramic powder
CN105294138A (en) Doublet aluminum oxide micropowder and preparation method thereof
CN112794707B (en) High-whiteness and high-strength light-transmitting ceramic tile and preparation method thereof
CN114988886B (en) Preparation method of high-purity alpha-alumina powder capable of being sintered at low temperature
CN105254282A (en) Preparation method of architectural ceramic material
CN114507014A (en) Snowflake crystal particle, preparation method thereof and preparation method of positioning crystal flower polished glazed brick
CN111498883A (en) Preparation method of large-primary-crystal high-purity calcined α -alumina micropowder
CN108046620B (en) A method of it is prepared by magnesite light burnt powder containing chrome-magnesite
CN104177070B (en) The preparation method that crystallite zirconium aluminium compound mill is situated between
CN111019648A (en) Molten salt method preparation method of oxysalt or oxynitride fluorescent powder
CN102491788B (en) Fast-fired composite-phase microcrystal matt surface glaze slip and application thereof
CN110590389A (en) Silicon nitride whisker-aluminum nitride-corundum ternary composite ceramic material using natural minerals as raw materials and preparation method thereof
CN112250461A (en) High-strength transparent ceramic and preparation method thereof
CN102503459A (en) High-grade cordierite-mullite refractory material for ceramic kiln and production process thereof
CN103496951B (en) Preparation method of low-temperature sintered high-strength ultrathin ceramic tile
CN102951899B (en) Cordierite material prepared by utilizing rare earth tailing and manufacturing method thereof
CN107619262A (en) A kind of Bone China and preparation method thereof
CN102503455B (en) Castable cordierite-mullite refractory material and production technique thereof
CN106430984A (en) Method for preparing microcrystal wollastonite glass from wollastonite
CN105481382A (en) Preparation method of cordierite fireproof material

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