WO2019093781A1 - Composition de magnésie à conductivité thermique élevée et céramique de magnésie - Google Patents

Composition de magnésie à conductivité thermique élevée et céramique de magnésie Download PDF

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WO2019093781A1
WO2019093781A1 PCT/KR2018/013526 KR2018013526W WO2019093781A1 WO 2019093781 A1 WO2019093781 A1 WO 2019093781A1 KR 2018013526 W KR2018013526 W KR 2018013526W WO 2019093781 A1 WO2019093781 A1 WO 2019093781A1
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mgo
magnesia
ceramics
high thermal
composition
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안철우
한병동
최종진
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한국기계연구원
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    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped 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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped 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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • the present invention relates to a magnesia (MgO) composition and a magnesia (MgO) ceramics prepared through the same. More specifically, the present invention relates to a titanium oxide (TiO 2 ), a niobium oxide (Nb 2 O 5 ), a zirconium oxide (ZrO 2), or alumina (Al 2 O 3) were added to, 1300 °C to at 1400 °C enables the sintering of the magnesia (MgO) composition, which the magnesia (MgO) ceramic having a high thermal conductivity characteristic prepared by .
  • TiO 2 titanium oxide
  • Nb 2 O 5 niobium oxide
  • ZrO 2 zirconium oxide
  • Al 2 O 3 alumina
  • alumina Al 2 O 3
  • Al 2 O 3 a low thermal conductive oxide ceramic material
  • the thermal conductivity of alumina (Al 2 O 3 ) is somewhat lower than 20-35 W / mK, it is necessary to improve the thermal conductivity of a low-cost oxide heat-radiating material in order to improve the life of a product using a low-
  • nitride materials are being used as excellent thermally conductive ceramic materials.
  • Nitrides such as aluminum nitride (AIN) and silicon nitride (Si 3 N 4 ) show a high thermal conductivity of 100 W / mK or more, but they are very expensive, have a very high sintering temperature of 1800 ° C. or higher, There are disadvantages. Therefore, it is not suitable as a general heat-dissipating substrate material requiring price competitiveness.
  • Magnesia (MgO) has a thermal conductivity of 30-60 W / mK higher than alumina (Al 2 O 3 ).
  • alumina (Al 2 O 3 ) is sintered at about 1500 ° C.
  • magnesia (MgO) has a disadvantage of sintering at a temperature higher than 1700 ° C., so that it is necessary to improve the sintering condition of magnesia (MgO).
  • MgO magnesia
  • Examples of researches for lowering the sintering temperature of magnesia (MgO) without considering the thermal conductivity property include adding a composition composed of lithium fluoride (LiF) and bismuth oxide (Bi 2 O 3 ), which are additives to magnesia (MgO) It is known that the sintering temperature can be lowered to 1500 DEG C or less. It has also been reported that sintering at 1400 ° C or lower is possible when a glass material is added as a low temperature sintering additive. (Registered patent KR10-1417445)
  • sinterability is improved through addition of a donor oxide which is known through research results of (K, Na) NbO 3 (KNN), SrTiO 3 (ST) and BaTiO 3 (BT) , And the sintering temperature of magnesia (MgO) can be lowered to a temperature lower than 1500 ° C.
  • the addition of an oxide that acts as a donor to such an oxide promotes grain growth due to ionic vacancies, dislocations, stacking faults, and twins. Such promotion of grain growth can improve the sinterability of the material. (Composition Design for Growth of Single Crystal by Abnormal Grain Growth in Modified Potassium Sodium Niobate Ceramics, Cryst. Growth Des. 16, page 6586-6592, 2016)
  • An object of the present invention is to provide a magnesia (MgO) composition and a magnesia (MgO) ceramics simultaneously having low temperature sintering ( ⁇ 1500 ° C) and high thermal conductivity characteristics.
  • sintering of magnesia is enhanced by adding an oxide additive which can act as a donor in magnesia (MgO), and sintering is possible at a low temperature lower than 1500 ° C.
  • the donor is an oxide including ions having a higher valence than Mg 2 + ions, and typically includes Nb 5 + , Ti 4 + , Zr 4 + , Al 3 +, and the like.
  • a high thermal conductive magnesia (MgO) composition according to an embodiment of the present invention includes MgO + x wt.% TiO 2 , MgO + y wt.% Nb 2 O 5 , (3) MgO + z wt.% ZrO 2 , or (4) MgO + w wt.% Al 2 O 3 (Where x, y, z and w satisfy 0 ⁇ x, y, z, w? 10.0 in the above equations (1) to (4).
  • a method for manufacturing a high thermal conductivity magnesia (MgO) ceramic comprising the steps of: (a) adding and mixing oxides to magnesia (MgO) Preparing a composition; (b) drying said composition; (c) sintering the composition.
  • MgO magnesia
  • low temperature sintering through sinterability improvement is achieved through the addition of one or more oxides that can act as a donor.
  • the MgO ceramics substrate composition according to the present invention has a high thermal conductivity while allowing magnesia (MgO) having a high thermal conductivity to be sintered at a temperature lower than 1500 ° C, thereby allowing the magnesia (MgO) So that it can be applied as a substrate material.
  • MgO magnesia
  • FIG. 1 is a graph showing changes in thermal diffusivity of a specimen obtained by adding titanium dioxide (TiO 2 ) to magnesia (MgO).
  • Nb 2 O 5 niobium pentoxide
  • MgO magnesia
  • ZrO 2 zirconium oxide
  • MgO magnesia
  • FIG. 4 is a graph showing changes in thermal diffusivity of a specimen sintered by adding a composition of 0.3 wt% titanium dioxide (TiO 2 ), 0.3 wt% niobium oxide (Nb 2 O 5 ), and zirconium oxide (ZrO 2 ) to magnesia
  • TiO 2 titanium dioxide
  • Nb 2 O 5 0.3 wt% niobium oxide
  • ZrO 2 zirconium oxide
  • Fig. 6 is a graph showing the relationship between the specimen prepared from the composition of magnesia (MgO) + 2.0 wt.% Titanium dioxide (TiO 2 ) and the specimen prepared from the composition of magnesia (MgO) + 2.0 wt.% Zirconium oxide (ZrO 2 ) And the surface of the sintered body was observed with an electron microscope.
  • magnesia (MgO) composition and the magnesia (MgO) ceramics according to the present invention will be described in detail.
  • the high thermal conductivity magnesia (MgO) composition according to the present invention comprises MgO + x wt.% TiO 2 , MgO + y wt.% Nb 2 O 5 , MgO + z wt.% ZrO 2, or equation (4) MgO + w wt. % Al 2 O 3 ( in the above formulas (1) to (4), x, y, z, w is 0 ⁇ x, y, z , w? 10.0).
  • alumina is used as a heat-radiating oxide substrate material.
  • Alumina (Al 2 O 3 ) can be sintered at 1500 ° C. and is inexpensive and has been used as a typical heat-dissipating oxide substrate material.
  • the thermal conductivity of alumina (Al 2 O 3 ) is somewhat low, 20-35 W / mK, and it is necessary to improve the thermal conductivity of the low-cost oxide heat-radiating material in order to improve the life of the product using low- cost heat-
  • the magnesia (MgO) according to the present invention is similar in price to alumina (Al 2 O 3 ) but has a relatively high thermal diffusivity and thermal conductivity.
  • the magnesia (MgO) according to the present invention has excellent resistance to alkali and electric insulation at high temperatures, exhibits high thermal conductivity, and has high light transmittance, and can be used for heat resistant materials, air insulating materials, high temperature optical materials, lighting materials and the like.
  • the high thermal conductivity of 30-60 W / mK shows a possibility of being used as a heat-dissipating oxide substrate material, but a high sintering temperature of 1700 DEG C or more has been a problem. Accordingly, in order to enhance the competitiveness of the magnesia (MgO), sintering at a sintering temperature of 1500 ° C or lower of alumina (Al 2 O 3 ) needs to be possible.
  • titanium dioxide TiO 2
  • niobium oxide Nb 2 O 5
  • zirconium oxide ZrO 2
  • / or alumina Al 2 O 3
  • the high thermal conductivity magnesia (MgO) composition comprises MgO + x wt.% TiO 2 , MgO + y wt.% Nb 2 O 5 , MgO + z wt. ZrO 2, or equation (4) MgO + w wt. % Al 2 O 3 ( in the above formulas (1) to (4), x, y, z, w is 0 ⁇ x, y, z, w ⁇ 10.0).
  • x in the equation (1) is 0 ⁇ x? 10.0
  • y in the equation (2) is 0 ⁇ y? 5.0
  • z in the equation (3) and w in the equation (4) may satisfy a range of 0 ⁇ w? 0.8.
  • y may satisfy a range of 0 ⁇ y ≤ 1.0.
  • magnesia (MgO) (MgO) ceramics sintered at 1700 deg. C even when the sintered body is sintered at 1400 deg. C to 1400 deg.
  • the specimen sintered at 1400 ° C. is a magnesia (MgO) ceramics.
  • the magnesia (MgO) ceramics according to the present invention is sintered at 1400 ° C It can be seen that the thermal diffusivity of the magnesia (MgO) ceramics sintered at 1700 ° C is similar.
  • the high thermal conductive magnesia (MgO) composition according to the present invention has the formula (5) MgO + 0.3 wt.% TiO 2 + 0.3 wt.% Nb 2 O 5 + zwt.% ZrO 2 .
  • z satisfies a range of 0 ⁇ z? 0.05.
  • the MgO ceramics according to the present invention exhibit significantly higher thermal diffusivity than the MgO ceramics sintered at 1700 ° C in the case where 0 wt.% To 0.05 wt.% Or less of MgO is added.
  • the thermal diffusivity of the magnesia (MgO) ceramics according to the present invention is increased Able to know.
  • the method for manufacturing a high thermal conductivity magnesia (MgO) ceramic according to the present invention comprises the steps of: (a) adding and mixing oxides to magnesia (MgO) to prepare a composition according to any one of claims 1 to 4; (b) drying said composition; And (c) sintering the composition.
  • MgO magnesia
  • low-temperature sintering through sinterability improvement is achieved through the addition of one or more oxides that can act as a donor .
  • the oxide is TiO 2, Nb 2 O 5, ZrO 2, Ga 2 O 3, Mn 2 O 3, Fe 2 O 3, SnO 2, MnO 2, SiO 2, V 2 O 5, Ta 2 O 4 , Sb 2 O 5, or Al 2 O 3 .
  • the oxide is TiO 2, Nb 2 O 5, ZrO 2, or Al 2 O 3 ≪ / RTI >
  • the step (c) may be performed at a sintering temperature of 1200 ° C to 1500 ° C.
  • the sintering temperature may be 1400 ° C to 1500 ° C.
  • magnesia (MgO) ceramic is titanium dioxide with an oxide to magnesia (MgO) (TiO 2), pentoxide, niobium (Nb 2 O 5), zirconium oxide (ZrO 2) and / or alumina (Al 2 O 3 ) is added in an appropriate amount, the alcohol is mixed with a solvent in a ball mill, and then the mixture is pulverized and dried.
  • the dried mixed powder is molded into a circular metal mold having a diameter of 15 mm at a pressure of 100 MPa and then sintered at an electric furnace at a temperature of 1200 ° C to 1500 ° C for 2 hours.
  • the high thermal conductivity magnesia (MgO) ceramics produced by the above method can exhibit a relative density value of 93% to 99.9% based on the theoretical density (3.6 g / cm 3 ) of magnesia (MgO).
  • the high thermal conductivity magnesia (MgO) ceramics produced by the manufacturing method according to the present invention exhibits a high relative density value as compared to the conventional magnesia (MgO) ceramics.
  • the high thermal conductivity magnesia (MgO) ceramics produced by the above method can exhibit a thermal diffusivity of 10.4 mm 2 / s to 21.9 mm 2 / s.
  • the high thermal conductivity magnesia (MgO) ceramics produced by the production method according to the present invention exhibits a high relative density value, and accordingly, the high thermal conductivity magnesia MgO) ceramics exhibit high thermal diffusivity values compared to conventional magnesia (MgO) ceramics.
  • the high thermal conductivity magnesia (MgO) ceramics according to the present invention can be obtained from the above equations (1) to (5) by using magnesium oxide (MgO), titanium dioxide (TiO 2 ), niobium oxide (Nb 2 O 5 ), zirconium oxide 2 ) and alumina (Al 2 O 3 ) were derived, and a high thermal conductivity magnesia (MgO) ceramics was produced based on the derived composition ratio.
  • the high thermal conductivity magnesia (MgO) ceramics according to the present invention has a high relative density value of 93% to 99.9% of the theoretical density (3.6 g / cm 3 ) of magnesia (MgO) and has a relative density of 10.4 mm 2 / s to 21.9 mm 2 / s, which indicates that superior relative density and thermal diffusivity characteristics are obtained as compared with the conventional ceramics.
  • FIG. 6 is a graph showing the relationship between the specimen prepared from the composition of magnesia (MgO) + 2.0 wt.% Titanium dioxide (TiO 2 ) and the specimen prepared from the composition of magnesia (MgO) + 2.0 wt.% Zirconium oxide (ZrO 2 ) And the surface of the sintered body is observed with an electron microscope.
  • MgO magnesia
  • TiO 2 titanium dioxide
  • ZrO 2 Zirconium oxide
  • a sintering temperature of 1400 ° C. shows a very dense microstructure, and in particular, a zirconium oxide (ZrO 2 ) added sample has a small grain size of 7 ⁇ m or less.
  • MoO 2 magnesia
  • the dried mixed powder is molded into a circular metal mold having a diameter of 15 mm at a pressure of 100 MPa and then sintered at 1300 ° C for 2 hours using an electric furnace.
  • Example 2 TiO 2 , niobium oxide (Nb 2 O 5 ), zirconium oxide (ZrO 2 ) and / or alumina (Al 2 O 3 ) as oxides in the magnesia (MgO) And then sintered at 1300 ° C or 1400 ° C, the same procedure as in Example 1 was carried out to produce a high thermal conductivity magnesia ceramics.
  • Magnesia ceramics were produced in the same manner as in Example 1, except that no oxide was added to the magnesia (MgO) in Example 1.
  • Magnesia ceramics were produced in the same manner as in Example 1, except that no oxide was added to the magnesia (MgO) of Example 1, and the magnesia (MgO) was sintered at a temperature of 1400 ° C.
  • Magnesia ceramics were produced in the same manner as in Example 1, except that no oxide was added to the magnesia (MgO) of Example 1, and the magnesia (MgO) was sintered at a temperature of 1700 ⁇ ⁇ .
  • Example 11 Addition amount (wt.%) Sintering temperature (°C) Density (g / cm 3) Relative density (%) Thermal Diffusivity (mm 2 / s) Oxide (additive) TiO 2 Nb 2 O 5 ZrO 2 Al 2 O 3
  • Example 1 0.5 - - - 1300 3.48 96.7 16.4
  • Example 2 1.5 - - - 1300 3.52 97.8 16.6
  • Example 3 10.0 - - - 1300 3.53 98.1 10.4
  • Example 4 - - 0.5 - 1300 3.02 83.9 12.6
  • Example 6 - 1.0 - - 1300 3.37 93.6 15.5
  • Example 7 - 3.0 - - 1300 3.42 95.0 15.5
  • Example 8 0.3 0.3 - - 1300 3.44 95.6 16.9
  • Example 9 0.3 0.3 0.05 - 1300 3.54 98.3 20.5
  • magnesia (MgO) composition is sufficiently performed in the temperature range of 1300 ° C. to 1400 ° C., and the relative density and the thermal diffusivity of the magnesia (MgO) have.
  • magnesia (MgO) ceramics according to the present invention exhibit excellent relative density values of 93% to 99.9% , And excellent thermal diffusivity values of 10.4 mm 2 / s to 21.9 mm 2 / s are shown.
  • magnesia (MgO) ceramics according to the present invention exhibits a further excellent relative density and thermal diffusivity.

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Abstract

La présente invention concerne une composition de magnésie (MgO) à conductivité thermique élevée, un procédé de préparation de céramique de magnésie (MgO), et de la céramique de magnésie (MgO) et, particulièrement, une composition de magnésie (MgO) à conductivité thermique élevée caractérisée par la formule mathématique (1) MgO + x % en pds de TiO2, formule mathématique (2) MgO + y % en pds de Nb2O5, formule mathématique (3) MgO + z % en pds de ZrO2, et formule mathématique (4) MgO + w % en pds d'Al2O3 (dans les formules mathématiques (1) à (4) ci-dessus, x, y, z, et w sont 0 < x, y, z, w ≤ 10,0), un procédé de préparation de céramique de magnésie (MgO), et de la céramique de magnésie (MgO) faisant preuve d'une conductivité thermique élevée.
PCT/KR2018/013526 2017-11-09 2018-11-08 Composition de magnésie à conductivité thermique élevée et céramique de magnésie WO2019093781A1 (fr)

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KR1020170148527A KR20190052797A (ko) 2017-11-09 2017-11-09 고열전도성 마그네시아 조성물 및 마그네시아 세라믹스
KR10-2017-0148527 2017-11-09

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WO2019093781A1 true WO2019093781A1 (fr) 2019-05-16

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KR102205178B1 (ko) * 2018-12-13 2021-01-21 한국재료연구원 마그네시아 및 그 제조 방법, 및 고열전도성 마그네시아 조성물, 이를 이용한 마그네시아 세라믹스

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JPH05330903A (ja) * 1990-01-19 1993-12-14 Ube Ind Ltd マグネシア系焼結体
JP2007284314A (ja) * 2006-04-19 2007-11-01 Nitsukatoo:Kk 耐食性マグネシア質焼結体、それよりなる熱処理用部材および前記焼結体の製造方法
US20100233497A1 (en) * 2007-04-18 2010-09-16 Alfred Thimm Ceramic material with a composition which is matched to a coefficient of thermal expansion specified by a metallic material
JP2012126591A (ja) * 2010-12-14 2012-07-05 Ohtsuka Ceramics Inc 高熱伝導性マグネシアセラミックス焼結体
KR20170100490A (ko) * 2014-11-10 2017-09-04 생-고뱅 세라믹스 앤드 플라스틱스, 인코포레이티드 소결 세라믹 부품 및 이의 형성 방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05330903A (ja) * 1990-01-19 1993-12-14 Ube Ind Ltd マグネシア系焼結体
JP2007284314A (ja) * 2006-04-19 2007-11-01 Nitsukatoo:Kk 耐食性マグネシア質焼結体、それよりなる熱処理用部材および前記焼結体の製造方法
US20100233497A1 (en) * 2007-04-18 2010-09-16 Alfred Thimm Ceramic material with a composition which is matched to a coefficient of thermal expansion specified by a metallic material
JP2012126591A (ja) * 2010-12-14 2012-07-05 Ohtsuka Ceramics Inc 高熱伝導性マグネシアセラミックス焼結体
KR20170100490A (ko) * 2014-11-10 2017-09-04 생-고뱅 세라믹스 앤드 플라스틱스, 인코포레이티드 소결 세라믹 부품 및 이의 형성 방법

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