JP2018052747A - 酸化マグネシウム含有スピネル粉末及びその製造方法 - Google Patents
酸化マグネシウム含有スピネル粉末及びその製造方法 Download PDFInfo
- Publication number
- JP2018052747A JP2018052747A JP2016186656A JP2016186656A JP2018052747A JP 2018052747 A JP2018052747 A JP 2018052747A JP 2016186656 A JP2016186656 A JP 2016186656A JP 2016186656 A JP2016186656 A JP 2016186656A JP 2018052747 A JP2018052747 A JP 2018052747A
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- Prior art keywords
- magnesium
- magnesium oxide
- particles
- oxide
- aluminum
- 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
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 129
- 239000000843 powder Substances 0.000 title claims abstract description 108
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 102
- 239000011029 spinel Substances 0.000 title claims abstract description 102
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 239000002245 particle Substances 0.000 claims abstract description 85
- 239000000919 ceramic Substances 0.000 claims abstract description 48
- 239000011777 magnesium Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 229910052782 aluminium Inorganic materials 0.000 claims description 35
- 229910052749 magnesium Inorganic materials 0.000 claims description 35
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 27
- 239000000347 magnesium hydroxide Substances 0.000 claims description 27
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 27
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 23
- 238000010304 firing Methods 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 21
- 230000001186 cumulative effect Effects 0.000 claims description 21
- 238000010298 pulverizing process Methods 0.000 claims description 21
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 15
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 6
- 239000001095 magnesium carbonate Substances 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- 238000013001 point bending Methods 0.000 claims description 6
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 5
- 239000011654 magnesium acetate Substances 0.000 claims description 5
- 235000011285 magnesium acetate Nutrition 0.000 claims description 5
- 229940069446 magnesium acetate Drugs 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 229940118662 aluminum carbonate Drugs 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- AFHJQYHRLPMKHU-XXWVOBANSA-N Aloin Natural products O=C1c2c(O)cc(CO)cc2[C@H]([C@H]2[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O2)c2c1c(O)ccc2 AFHJQYHRLPMKHU-XXWVOBANSA-N 0.000 abstract 1
- CPUHNROBVJNNPW-UHFFFAOYSA-N aloin A Natural products OC1C(O)C(O)C(CO)OC1OC1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 CPUHNROBVJNNPW-UHFFFAOYSA-N 0.000 abstract 1
- AFHJQYHRLPMKHU-WEZNYRQKSA-N aloin B Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@H]1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-WEZNYRQKSA-N 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- AFHJQYHRLPMKHU-UHFFFAOYSA-N isobarbaloin Natural products OC1C(O)C(O)C(CO)OC1C1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-UHFFFAOYSA-N 0.000 abstract 1
- 238000000465 moulding Methods 0.000 description 21
- 239000011812 mixed powder Substances 0.000 description 19
- 238000005469 granulation Methods 0.000 description 16
- 230000003179 granulation Effects 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 238000005452 bending Methods 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 239000011010 synthetic spinel Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 238000010079 rubber tapping Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004901 spalling Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- OCYUQKSNQVZPED-UHFFFAOYSA-L aluminum;magnesium;dihydroxide Chemical compound [OH-].[OH-].[Mg+2].[Al+3] OCYUQKSNQVZPED-UHFFFAOYSA-L 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/162—Magnesium aluminates
-
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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
- C04B35/44—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 aluminates
- C04B35/443—Magnesium aluminate spinel
-
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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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- C04B35/00—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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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- C04B2235/32—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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- C04B2235/32—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
- C04B2235/3218—Aluminium (oxy)hydroxides, e.g. boehmite, gibbsite, alumina sol
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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Abstract
Description
次に、本発明の酸化マグネシウム含有スピネル粉末を製造する方法の一例について説明する。本発明の酸化マグネシウム含有スピネル粉末は、マグネシウム源からなる粉末とアルミニウム源からなる粉末を混合して得た混合粉末を高温で仮焼合成して合成スピネル原料を作製し、これを所定の粒子径及び粒度分布となるように粉砕することで製造することができる。
本発明の酸化マグネシウム含有スピネル粉末の造粒体を形成した後、これを所望の形状に成形し、焼成することで所望の形状のセラミックス焼結体を製造することができる。本発明により製造されるセラミックス焼結体は、あらかじめ酸化マグネシウム含有スピネル粉末におけるMgとAlの組成比を調整しておくことで、耐食性、耐スポーリング性、熱膨張率を容易に制御することが可能である。
(1)曲げ強度試験方法
曲げ強度試験は、JIS−R−1601:2008(ファインセラミックスの室温曲げ強さ試験方法)における3点曲げ試験方法に準じて行った。試験片(セラミックス焼結体)の形状は、断面が長方形の角柱とする。寸法は全長50mm、幅4.0±0.1mm、厚さ3.0±0.1mmとなるよう、セラミック焼結体を切断研磨して加工した。測定装置は、テンシロン万能材料試験機(RTA−500 株式会社オリエンテック製)を使用し、試験片をスパン幅=40mmの支持具に置き、上部からクロスヘッドを速度0.5mm/minの変位で押し当てて、試験ジグ内の試験片に荷重を加え、試験片が破壊するまでの最大荷重を測定した。最大荷重から以下の計算式にて、曲げ強度を算出した。
σb3=3PL/2wt2
ここで、σb3:3点曲げ強さ(MPa)、P:試験片が破壊したときの最大荷重(N)、L:外部支点間距離(mm)、w:試験片の幅(mm)、t:試験片の厚さ(mm)である。
ワイブル係数は、JIS−R−1625−2010(ファインセラミックスの強さデータのワイブル統計解析法)に準じて算出した。ワイブル係数の数値が大きいものほど、強度分布の幅が狭く、安定性が高いといえる。曲げ強度試験方法で算出した3点曲げ強度σ(n=15〜30)を値の低いものから順に並べ、データの累積破壊確率Fiを平均ランク法によって求めた。
Fi=i/(n+1)
ここで、nはサンプル数、iは小さい順に並び替えた順位(順位数)である。
嵩密度は、粉体特性測定装置パウダテスタ(PT−N ホソカワミクロン株式会社製)を用いて測定した。
各粉末の体積基準の累積10%粒子径、体積基準の累積50%粒子径、及び体積基準の累積90%粒子径(D10、D50、及びD90)は、レーザ回折散乱式粒度分布測定装置(MT3300 日機装株式会社製)を用いて測定した。溶媒にはメタノールを使用し、超音波ホモジナイザー(US−300T 株式会社日本精機製作所製)にて120Wで3分間分散処理を施した後、各粒子径を測定した。得られた各粒子径の値から、(D90−D50)/(D50−D10)を算出した。
酸化マグネシウム含有スピネル粉末の組成分析は、多元素同時蛍光X線分析装置(Simultix12 株式機会社リガク製)にて、ガラスビード法にて行った。各元素含有量を酸化物換算で算出し、酸化マグネシウムと酸化アルミニウムの組成比を算出した。また、主要な不純物となるCa、Si、P、S、B、Fe、Ti、Zn、Cu、Baを酸化物換算し、100%から減算して、酸化マグネシウム含有スピネル粉末の純度を算出した。
水酸化マグネシウム及び水酸化アルミニウムの純度は、(5)と同様に、多元素同時蛍光X線分析装置(Simultix12 株式機会社リガク製)にて、主要な不純物となるCa、Si、P、S、Fe、B、Naを酸化物換算し、100%から減算して算出した。
Mgイオン濃度が2.0mol/Lになるように調整した塩化マグネシウム水溶液と、水酸化ナトリウム溶液に純水を加えて濃度2.7mol/Lに調整した溶液を、それぞれ定量ポンプで反応槽に送液して、塩化マグネシウムに対する水酸化ナトリウムの反応率が90mol%となるよう、連続化合反応を実施した。反応スラリーは反応槽より滞留時間30分でオーバーフローさせ、水酸化マグネシウムスラリーを回収した。これを濾過、水洗、乾燥し、水酸化マグネシウム乾燥粉末を得た。得られた水酸化マグネシウム乾燥粉末の純度が99.9%、D50が33.06μmであった。
MgとAlの組成比が酸化物換算でMgO:Al2O3が50:50になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=1.94μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が60:40になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=1.86μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が80:20になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=1.69μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が90:10になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=1.74μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1200℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=2.20μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1100℃、1時間仮焼し、ボールミルで8時間粉砕することで、D50=0.44μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで6時間粉砕することで、D50=1.63μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1100℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=0.71μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1500℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=16.03μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、シャトルキルンで1600℃、1時間仮焼し、ボールミルで3時間粉砕することで、D50=15.39μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
実施例9の方法で作製した酸化マグネシウム含有スピネル粉末と、比較例2の方法で作製した酸化マグネシウム含有スピネル粉末を、75:25になるように乾式で十分に混合してD50=0.82μmの酸化マグネシウム含有粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
D50=1.20μmの酸化マグネシウム粉末及びD50=0.50μmの酸化アルミニウム粉末を、MgとAlの組成比が酸化物換算でMgO:Al2O3が70:30になるように配合し、乾式で均一になるよう十分に混合してD50=0.69μmの混合粉末を得た。得られた混合粉末の仮焼及び粉砕を行わず、すなわち酸化マグネシウム含有スピネル粉末を得ることなく、前記混合粉末を用いて、実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
MgとAlの組成比が酸化物換算でMgO:Al2O3が30:70になるように配合して水酸化マグネシウムと水酸化アルミニウムの混合粉末を得た後、電気炉で1000℃、1時間仮焼し、ボールミルで4時間粉砕することで、D50=1.84μmの酸化マグネシウム含有スピネル粉末を得た。得られた酸化マグネシウム含有スピネル粉末を用いて、以後実施例1と同様の方法で造粒、成形及び焼成を行い、所定形状のセラミックス焼結体を得た。
Claims (4)
- レーザ回折散乱式粒度分布測定による体積基準の累積50%粒子径(D50)が0.30〜10.00μmであり、体積基準の累積90%粒子径(D90)とD50の差およびD50と体積基準の累積10%粒子径(D10)の差の比:(D90−D50)/(D50−D10)が1.0〜5.0であり、かつMgとAlの組成比が酸化物に換算してMgOが50〜90重量%、Al2O3が50〜10重量%である、酸化マグネシウム含有スピネル粉末。
- ゆるめ嵩密度が0.20〜1.50g/cm3、かため嵩密度が0.30〜2.50g/cm3である、請求項1記載の酸化マグネシウム含有スピネル粉末。
- 前記酸化マグネシウム含有スピネル粉末の成形体を焼成してなるセラミック焼結体は、3点曲げ強度が150MPa以上、ワイブル係数が13.0以上である、請求項1又は2記載の酸化マグネシウム含有スピネル粉末。
- 請求項1〜3のいずれか1項に記載の酸化マグネシウム含有スピネル粉末を製造する方法であって、
体積基準の累積50%粒子径(D50)が0.50〜100.00μmの、水酸化マグネシウム粒子、酸化マグネシウム粒子、炭酸マグネシウム粒子、塩基性炭酸マグネシウム粒子、硝酸マグネシウム粒子、酢酸マグネシウム粒子、及び硫酸マグネシウム粒子から選択される1種類以上のマグネシウム源粒子と、D50が0.30〜15.00μmの、水酸化アルミニウム粒子、酸化アルミニウム粒子、炭酸アルミニウム粒子、硝酸アルミニウム粒子、酢酸マグネシウム粒子、及び硫酸アルミニウム粒子から選択される1種類以上のアルミニウム源粒子とを混合した後、900〜1400℃で0.1〜10.0時間仮焼し、次いで粉砕する工程を含む製造方法。
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JP2016186656A JP6845645B2 (ja) | 2016-09-26 | 2016-09-26 | 酸化マグネシウム含有スピネル粉末及びその製造方法 |
CN201780058292.6A CN109715560B (zh) | 2016-09-26 | 2017-09-26 | 含氧化镁的尖晶石粉末及其制造方法 |
KR1020197002502A KR102360147B1 (ko) | 2016-09-26 | 2017-09-26 | 산화마그네슘 함유 스피넬 분말 및 그 제조방법 |
US16/335,489 US10766783B2 (en) | 2016-09-26 | 2017-09-26 | Magnesium oxide-containing spinel powder and method for producing same |
TW106132887A TWI732944B (zh) | 2016-09-26 | 2017-09-26 | 含氧化鎂之尖晶石粉末及其製造方法 |
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Cited By (3)
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CN109550492A (zh) * | 2018-12-12 | 2019-04-02 | 余嘉琪 | 一种高导热高比表面积镁铝尖晶石的制备方法 |
WO2020145342A1 (ja) * | 2019-01-11 | 2020-07-16 | Dic株式会社 | スピネル粒子及びその製造方法、樹脂組成物、成形物、組成物、グリーンシート、焼成物、並びに、ガラスセラミックス基板 |
WO2020195721A1 (ja) * | 2019-03-28 | 2020-10-01 | タテホ化学工業株式会社 | スピネル粉末 |
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CN111747731B (zh) * | 2019-03-26 | 2022-02-08 | 中国科学院上海硅酸盐研究所 | 一种氧化镁基超高压介质陶瓷及其制备方法 |
WO2021117742A1 (ja) * | 2019-12-10 | 2021-06-17 | 黒崎播磨株式会社 | 耐火物 |
EP4074433A4 (en) * | 2019-12-10 | 2023-04-12 | Krosakiharima Corporation | REFRACTORY MATERIAL |
DE102019220085A1 (de) * | 2019-12-18 | 2021-06-24 | Refratechnik Holding Gmbh | Versatz zur Herstellung eines grobkeramischen feuerfesten basischen Erzeugnisses, derartiges Erzeugnis sowie Verfahren zu seiner Herstellung, Zustellung eines Industrieofens und Industrieofen |
CN114906866B (zh) * | 2022-05-16 | 2023-09-22 | 山东恒源兵器科技股份有限公司 | 一种复合镁铝尖晶石粉及其制备方法和应用 |
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JPS5767074A (en) | 1980-10-15 | 1982-04-23 | Shin Nihon Kagaku Kogyo Kk | Manufacture of high density spherical body containing spinel as major ingredient |
JPH09142916A (ja) | 1995-11-17 | 1997-06-03 | Kawasaki Refract Co Ltd | スピネル含有耐火物 |
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JP5435397B2 (ja) * | 2009-04-02 | 2014-03-05 | 住友電気工業株式会社 | スピネル製光透過用窓材及びその製造方法 |
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WO2013069742A1 (ja) * | 2011-11-11 | 2013-05-16 | 堺化学工業株式会社 | ハイドロタルサイトとその製造方法 |
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JP6363014B2 (ja) * | 2014-12-25 | 2018-07-25 | 第一稀元素化学工業株式会社 | スピネル粉末及びその製造方法 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109550492A (zh) * | 2018-12-12 | 2019-04-02 | 余嘉琪 | 一种高导热高比表面积镁铝尖晶石的制备方法 |
WO2020145342A1 (ja) * | 2019-01-11 | 2020-07-16 | Dic株式会社 | スピネル粒子及びその製造方法、樹脂組成物、成形物、組成物、グリーンシート、焼成物、並びに、ガラスセラミックス基板 |
WO2020195721A1 (ja) * | 2019-03-28 | 2020-10-01 | タテホ化学工業株式会社 | スピネル粉末 |
KR20210144777A (ko) | 2019-03-28 | 2021-11-30 | 다테호 가가쿠 고교 가부시키가이샤 | 스피넬 분말 |
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KR20190052668A (ko) | 2019-05-16 |
WO2018056456A1 (ja) | 2018-03-29 |
US10766783B2 (en) | 2020-09-08 |
TWI732944B (zh) | 2021-07-11 |
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