CN113784923B - Spinel powder - Google Patents
Spinel powder Download PDFInfo
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- CN113784923B CN113784923B CN202080034405.0A CN202080034405A CN113784923B CN 113784923 B CN113784923 B CN 113784923B CN 202080034405 A CN202080034405 A CN 202080034405A CN 113784923 B CN113784923 B CN 113784923B
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- spinel
- aluminum
- magnesium
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 101
- 239000011029 spinel Substances 0.000 title claims abstract description 101
- 239000000843 powder Substances 0.000 title claims abstract description 90
- 239000011777 magnesium Substances 0.000 claims abstract description 64
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 61
- 238000010304 firing Methods 0.000 claims abstract description 59
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 45
- 238000010298 pulverizing process Methods 0.000 claims abstract description 38
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 36
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims description 55
- 238000000034 method Methods 0.000 claims description 30
- 238000009826 distribution Methods 0.000 claims description 25
- 230000001186 cumulative effect Effects 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 11
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 7
- 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 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 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 2
- 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 2
- 229940009827 aluminum acetate Drugs 0.000 claims description 2
- 229940118662 aluminum carbonate Drugs 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 37
- 239000000395 magnesium oxide Substances 0.000 description 27
- 239000000203 mixture Substances 0.000 description 22
- UUNNUENETDBNPB-HKBOAZHASA-N (2s)-2-[[(2s,3r)-3-amino-2-hydroxy-4-(4-phenylmethoxyphenyl)butanoyl]amino]-4-methylpentanoic acid Chemical compound C1=CC(C[C@@H](N)[C@H](O)C(=O)N[C@@H](CC(C)C)C(O)=O)=CC=C1OCC1=CC=CC=C1 UUNNUENETDBNPB-HKBOAZHASA-N 0.000 description 18
- 239000012535 impurity Substances 0.000 description 18
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 17
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 13
- 239000000347 magnesium hydroxide Substances 0.000 description 13
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 229910020068 MgAl Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000013329 compounding Methods 0.000 description 5
- -1 magnesium aluminate Chemical class 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 235000013619 trace mineral Nutrition 0.000 description 3
- 239000011573 trace mineral Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000010296 bead milling Methods 0.000 description 1
- 238000001354 calcination Methods 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
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—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
- C04B35/6261—Milling
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The spinel powder has a purity of 99.95wt% or more. The spinel powder has a content of Mg and Al expressed in terms of oxide of MgO:9 to 78wt% and Al 2 O 3 :22wt% to 91 wt%. The preparation method of the spinel powder comprises the following steps: a mixing step of mixing a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more to obtain a mixed powder; a pulverizing step of pulverizing the mixed powder to obtain a precursor; and a firing step of firing the precursor at a temperature of 1500 ℃ or lower.
Description
Technical Field
The present application relates to a spinel powder. In particular, the application relates to a magnesium aluminate spinel powder.
Background
The chemical composition is shown as MgAl 2 O 4 Magnesium aluminate spinel (MgO-Al) 2 O 3 Spinel, hereinafter referred to as "spinel") is used in various fields as a ceramic sintered body excellent in thermal stability and chemical stability. Examples of applications of the ceramic sintered body using the spinel include an optical material, a heat-resistant container, an insulating material, a catalyst carrier, an adsorbent, a support, and a coating material.
In general, a ceramic sintered body using spinel is obtained by sintering spinel powder. It is known that trace elements contained in spinel powder affect characteristics as a ceramic sintered body for various applications.
JP-A2018-501178 (patent document 1) discloses a composition comprising MgO, at least 0.1wt% of a dopant and Al 2 O 3 A sintered ceramic component having a total impurity content of less than 0.7 wt%. WO2015/140459 (patent document 2) proposes a magnesia-alumina oxide MgAl constructed from spinel 2 O 4 And/or MgO-MgAl 2 O 4 Fused particles composed of a matrix (matrix) of eutectic mixture. More than 95.0% by weight of the fused particles represents Al 2 O 3 And MgO chemical composition, caO and ZrO 2 The cumulative content of (2) is less than 4000 mass ppm.
WO2014/119177 (patent document 3) discloses a gas nozzle provided with a body composed of a spinel sintered body. The spinel sintered body has a main component comprising 90 to 99.9wt% of magnesium aluminate and a sintering aid comprising 0.1 to 10wt% of Ca, mg or Zr. WO2013/038916 (patent document 4) proposes conversion of Zn and K contents into ZnO and K, respectively 2 The total amount of the magnesium aluminate sintered body after O is 30ppm to 500ppm. Patent document 4 describes conversion of Si, ca, and P contents into SiO, respectively 2 CaO and P 2 O 5 The total amount is controlled to 500ppm to 2500 ppm.
As disclosed in patent documents 1 to 4, when a desired property is imparted or enhanced by a trace element, it is important to contain no other unnecessary element as an impurity. In addition, impurities affect the thermal expansion rate of the ceramic sintered body. When the impurity content is large and the purity is low, the thermal expansion coefficient of the ceramic sintered body varies. In addition, in the use of optical materials, there is a problem that absorption or dispersion of light due to impurities occurs to deteriorate transparency. Therefore, spinels of higher purity are required for various applications.
Japanese patent application laid-open No. 62-72556 (patent document 5) discloses a method of obtaining high-purity MgAl having a purity of 99.9% or more by pre-firing a coprecipitate obtained by an alkoxide coprecipitation method 2 O 4 Raw material technology. JP-A2018-507156 (patent document 6) proposes a method of compounding magnesium with a compound of magnesiumAnd (3) adding a pH-adjusted alumina dispersant to the aqueous dispersant, drying the slurry (slurry), and calcining the dried slurry to prepare the magnesia-alumina spinel. Japanese patent application laid-open No. 2018-52747 (patent document 7) discloses a method for producing a spinel powder containing magnesium oxide, which comprises a step of mixing magnesium source particles and aluminum source particles having a predetermined particle diameter and then pre-firing the mixture at 900 to 1400 ℃.
Prior art literature:
patent literature:
patent document 1: japanese patent application laid-open No. 2018-501178
Patent document 2: WO2015/140459
Patent document 3: WO2014/119177
Patent document 4: WO2013/038916
Patent document 5: japanese patent laid-open No. 62-72556
Patent document 6: japanese patent application laid-open No. 2018-507156
Patent document 7: japanese patent application laid-open No. 2018-52747.
Disclosure of Invention
Problems to be solved by the application:
the methods disclosed in patent documents 5 and 6 have problems of complicated operation and difficult control of particle size. In addition, the method of patent document 5 uses an alkoxide having a high valence, and therefore has a problem in terms of cost.
In the case of the solid phase method as in patent document 7, it is considered that the obtained spinel is highly purified by using high-purity magnesium source particles and aluminum source particles as raw materials. However, it is known that trace elements as impurities promote MgAl caused by firing in the solid phase method 2 O 4 Is generated. For example, when a raw material having a purity of 99.95wt% or more is used, the acceleration effect cannot be obtained, and therefore, it is difficult to sufficiently perform spinelle at a firing temperature of about 900 to 1400 ℃. Spinel formation may be promoted by firing for a long period of time at a temperature of 1600 ℃ or higher, but there is a high possibility that impurities are mixed during firing, and activity such as sinterability is reduced due to firing at a high temperatureProblems. In addition, spinel after high-temperature firing is strongly sintered, so that strong crushing and pulverization are required to obtain a predetermined particle size, and the possibility of mixing in impurities is high. Further, it is very disadvantageous in terms of industrial aspects such as productivity, facilities, energy costs, etc., and there is a problem in practical use.
According to the findings of the present inventors, the industrial spinel powder has a substantial purity of about 99.9%. In various applications, in order to achieve higher functionality and higher added value of a ceramic sintered body using spinel, it is necessary to further highly purify spinel powder as a raw material thereof.
The purpose of the present application is to provide a spinel powder which has high purity and no deterioration in activity due to high-temperature firing, and a process for producing the same.
Means for solving the problems:
the present inventors have intensively studied and found that the firing can be performed at a relatively low temperature even in a high purity by controlling the particle size in the solid phase reaction of a magnesium source and an aluminum source, thereby completing the present application.
Namely, the spinel powder of the present application has a purity of 99.95wt% or more. The spinel powder has a content of Mg and Al expressed in terms of oxide of MgO:9 to 78wt% and Al 2 O 3 :22wt% to 91 wt%.
Preferably, the spinel powder has a purity of 99.99wt% or more.
Preferably, the spinel powder has a Ca content of less than 30ppm and a Si content of less than 30ppm. Preferably, the spinel powder has a total content of elements other than Mg, al and O of less than 500ppm.
Preferably, the spinel powder is a powder obtained by solid phase reaction of a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more at a reaction temperature of 1500 ℃ or less.
Furthermore, the application relates to a method for the preparation of the spinel powder. The preparation method comprises the following steps:
(1) A mixing step of mixing a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more to obtain a mixed powder;
(2) A pulverizing step of pulverizing the mixed powder to obtain a precursor; and
(3) And a firing step in which the precursor is fired at a temperature of 1500 ℃ or lower.
Preferably, the magnesium source and the aluminum source are each a powder composed of a plurality of particles. The ratio D50 (1)/D50 (2) of the particle diameter D50 (1) of 50% of the cumulative distribution of the volume basis of the magnesium source to the particle diameter D50 (2) of 50% of the cumulative distribution of the volume basis of the aluminum source is 0.2 to 5.0.
Preferably, the pulverizing step is performed by wet pulverization.
The application has the following effects:
the spinel powder of the present application has a purity of 99.95wt% or more. The spinel powder is obtained by mixing a magnesium source and an aluminum source and then firing the mixture at a temperature of 1500 ℃ or lower. The spinel powder has no activity reduction caused by high-temperature firing, and has a sufficiently small content of impurity elements, so that the spinel powder is suitable for various applications requiring high purity.
As described in the background art, about 99.9wt% of spinel powder has been used in the past. However, in the technical field of the present application, the purity of 99.9wt% (3N) and the purity of 99.95wt% (3N 5) are not only numerical differences but also very different in technical level. The application is achieved by overcoming the technical difficulty.
Detailed Description
The present application will be described in detail below based on preferred embodiments, but the present application is not limited to the following embodiments, and various modifications are possible within the scope of the claims. In the present specification, "X to Y" in the expression range means "X or more and Y or less". Unless otherwise noted, "%" refers to "wt%", and "ppm" refers to "mass ppm".
In the present specification, "spinel" means a material having MgAl 2 O 4 The magnesium aluminate spinel with chemical composition is MgO-Al 2 O 3 Is a two-component compound of (a). The spinel powder of the present application is not a single unit such as magnesia and aluminaThe mixture of the magnesium oxide matrix and the aluminum oxide matrix separated as a pure mixture is formed wholly or partially into an oxide obtained by compounding magnesium and aluminum, and has a composition with higher uniformity.
The purity of the spinel powder of the present application is 99.95wt% or more, preferably 99.99wt% or more. Here, the purity means a value obtained by subtracting the impurity content contained in the spinel powder from 100%.
The content of elements other than Mg, al and O, i.e., impurities in the spinel powder having a purity of 99.95wt% or more is sufficiently smaller than that in the conventional spinel powder. According to the spinel powder, the variation in the thermal expansion coefficient of the obtained ceramic sintered body is reduced. Further, by using the spinel powder, a ceramic sintered body having high transparency can be obtained. The spinel powder is suitable for various applications requiring a high purity of 99.95wt% or more.
The spinel powder of the present application has a content of Mg and Al expressed in terms of oxide of MgO:9wt% to 78wt% and less, al 2 O 3 :22wt% to 91 wt%. The ceramic sintered body obtained by using the spinel powder in this range can be given various characteristics required for various applications. From this viewpoint, the content of Mg and Al is preferably MgO:12 to 70wt% of Al 2 O 3 :30wt% to 88wt% inclusive, more preferably, mgO:14wt% to 61wt%, al 2 O 3 :39wt% to 86 wt%. Preferably, the stoichiometric ratio of Mg and Al of the spinel powder is between 9: 1-2: 8. For example, when the spinel powder is used as a ceramic material, if the proportion of Mg increases, the thermal expansion coefficient tends to increase, and the spalling resistance tends to decrease. If the Mg content is reduced, the corrosion resistance may be lowered. Further, since the hardness of the spinel powder increases as the proportion of Al increases, the possibility of mixing in impurities during pulverization increases. In addition, a method for measuring the content of Mg and Al will be described in examples later.
The spinel powder may contain elements other than Mg, al, and O within a range that does not hinder the effects of the present application. Examples of the elements other than Mg, al, and O contained in the spinel powder include Ca, si, fe, mn, ni, cu, zn, na. There are cases where P, S, B, ti, zr, ba and the like are included.
Preferably, the spinel powder has a Ca content of less than 30ppm and a Si content of less than 30ppm. By reducing Si and Ca to an extremely small amount, the change in characteristics due to impurities becomes extremely small, so that the characteristics of the spinel powder can be controlled more precisely. Thereby, high functionalization and high added value are realized. From this viewpoint, the content of Ca is more preferably 25ppm or less, and still more preferably 20ppm or less. From the same viewpoint, the Si content is more preferably 25ppm or less, and still more preferably 20ppm or less.
Preferably, the spinel powder has a total content of elements other than Mg, al and O of less than 500ppm. By making the total content of elements other than Mg, al, and O in this range, a high purity of 99.95wt% or more is achieved. From this viewpoint, the total content of elements other than Mg, al, and O is preferably 100ppm or less, more preferably 70ppm or less. The total content is obtained as the sum of the contents of other elements than Mg, al, and O. The type of the "other element" is not particularly limited, and elements other than Mg, al, and O detected by the measurement method described in the following examples are used as the "other element" to calculate the total content. As a specific example of the "other element", ca, si, fe, mn, ni, cu, zn, na, P, S, B, ti, zr, ba and the like are given, for example.
Preferably, the spinel powder is a product obtained by mixing a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more as raw materials, and then performing a solid phase reaction at a temperature of 1500 ℃ or less. The solid phase reaction at 1500 ℃ or less suppresses the strong sintering of the obtained spinel powder. The spinel powder avoids impurity mixing caused by strong crushing and crushing after sintering. In addition, since the spinel powder is not subjected to a high temperature treatment, the activity such as sinterability can be maintained.
The method for producing the spinel powder of the present application will be described in detail below.
The preparation method comprises a mixing process, a crushing process and a sintering process. The mixing step is a step of mixing a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more to obtain a mixed powder. The pulverizing step is a step of pulverizing the mixed powder to obtain a precursor. The firing step is a step of firing the precursor at a temperature of 1500 ℃ or lower. The preparation method may also include a particle size adjustment step after the firing step. The preparation method may further include other processes as long as the object of the present application is achieved.
In this production method, the purity of the magnesium source used as a raw material is 99.95wt% or more. By using a magnesium source of this purity, a high degree of purification of the resulting spinel powder is achieved. From this viewpoint, the purity of the magnesium source is preferably 99.99wt% or more.
The kind of the magnesium source is not particularly limited as long as the effect of the present application is not impaired. As specific examples of the magnesium source, there are magnesium hydroxide, magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium nitrate, magnesium acetate, magnesium sulfate, and the like. Magnesium hydroxide and magnesium oxide are preferred, and magnesium hydroxide is more preferred. Magnesium hydroxide becomes magnesium oxide with a high specific surface area during the firing process. By the presence of the magnesium oxide with high specific surface area around the aluminum source, mgAl is promoted 2 O 4 The reaction proceeds to a relatively low firing temperature region to realize sufficient spinelle formation.
The method for producing the magnesium source having a purity of 99.95wt% or more is not particularly limited. For example, as an example of a method for producing magnesium hydroxide having a purity of 99.95wt% or more, for example, a method in which an alkaline aqueous solution such as ammonia, calcium hydroxide, sodium hydroxide or the like is added to an aqueous solution containing magnesium chloride, and the mixture is reacted and then dried to obtain magnesium hydroxide powder is used. The magnesium oxide powder obtained by firing the magnesium hydroxide powder thus obtained and pulverizing the magnesium hydroxide powder to a desired particle size can be used as a magnesium source. Further, there is a method of obtaining magnesium oxide powder by a gas phase method of burning and oxidizing metallic magnesium, for example.
The magnesium source is preferably a powder composed of a plurality of fine particles. The particle size D50 (1) of the magnesium source, which is a volume-based cumulative distribution of 50%, is preferably 0.1 μm or more and 1.0 μm or less. The particle size of the magnesium source is within this range, so that the spinel powder obtained does not have a residual matrix of magnesium oxide, but rather a spinel phase obtained by compounding magnesium oxide and aluminum oxide is sufficiently formed. From this viewpoint, the particle diameter D50 (1) of the magnesium source whose volume-based cumulative distribution is 50% is preferably 0.2 μm or more and 0.9 μm or less, more preferably 0.2 μm or more and 0.8 μm or less. In addition, a measurement method of the particle diameter D50 (1) in which the volume-based cumulative distribution of the magnesium source is 50% will be described in the following examples.
In the preparation method, the purity of the aluminum source used as the raw material is 99.95wt% or more. By using this pure aluminum source, a high degree of purification of the resulting spinel powder is achieved. From this viewpoint, the purity of the aluminum source is preferably 99.99wt% or more.
The kind of the aluminum source is not particularly limited as long as the effect of the present application is not impaired. Specific examples of the aluminum source include aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum nitrate, aluminum acetate, aluminum sulfate, and the like. A preferred aluminum source is aluminum oxide.
The method for producing the aluminum source having a purity of 99.95wt% or more is not particularly limited. For example, as an example of a method for producing aluminum hydroxide having a purity of 99.95wt% or more, there is a method in which bauxite is reacted with an aqueous sodium hydroxide solution under pressure and heat, the resulting aqueous solution is filtered to extract a sodium aluminate solution, and the sodium aluminate solution is cooled to obtain aluminum hydroxide. The aluminum oxide obtained by firing the aluminum hydroxide thus obtained and pulverizing the aluminum hydroxide to a desired particle size can be used as an aluminum source.
The aluminum source is preferably a powder composed of a plurality of fine particles. The particle size of the aluminum source is preferably such that the particle size D50 (2) having a cumulative distribution of 50% by volume is 0.1 μm or more and 1.0 μm or less. The particle size of the magnesium source is within this range, so that the spinel powder obtained does not have alumina matrix residue, but a spinel phase obtained by compounding magnesium oxide and alumina is sufficiently formed. From this viewpoint, the particle diameter D50 (2) of the aluminum source whose volume-based cumulative distribution is 50% is preferably 0.2 μm or more and 0.9 μm or less, more preferably 0.2 μm or more and 0.8 μm or less. In addition, a measurement method of the particle diameter D50 (2) in which the volume-based cumulative distribution of the aluminum source is 50% will be described in the following examples.
Preferably, the ratio D50 (1)/D50 (2) of the particle diameter D50 (1) of the magnesium source to the particle diameter D50 (2) of the aluminum source is 0.2 to 5.0. By mixing the magnesium source and the aluminum source in the ratio D50 (1)/D50 (2) within this range in the mixing process, a mixed powder having a relatively uniform particle size distribution can be obtained. The particle size distribution of the precursor (mixture before firing) obtained by pulverizing the mixed powder is also uniform. Regarding the precursor having a uniform particle size distribution, the reaction of the magnesium source and the aluminum source proceeds at a relatively low firing temperature, promoting the formation of the spinel phase. From this viewpoint, the ratio D50 (1)/D50 (2) is more preferably 0.4 to 4.0, particularly preferably 0.3 to 3.0.
The mixing ratio of the magnesium source and the aluminum source to be mixed in the mixing step may be adjusted so that the Mg and Al contents (also referred to as composition ratio) of the obtained spinel powder fall within the aforementioned range. In this production method, the method of mixing the magnesium source and the aluminum source is not particularly limited, and a known mixing device can be appropriately selected and used. As specific examples, there are a vessel rotary type mixer such as a V-type mixer, a ribbon mixer, a henschel mixer, a coulter mixer (ploughshare mixer), a high-speed mixer, a dry ball mill, and the like. Preferably, the mixture is mixed as homogeneously as possible.
The mixed powder obtained in the mixing step is pulverized to a predetermined particle size in a pulverizing step before firing. By this pulverizing step, the formation of a spinel phase in a relatively low firing temperature region is further promoted.
In this production method, the method of pulverizing the mixed powder is not particularly limited, and may be wet pulverization or dry pulverization. Wet milling is preferred from the standpoint of easier availability of a more uniform particle size distribution. In the case of wet pulverization, the mixed powder is pulverized in a state of being dispersed in a solvent. Examples of the solvent used include water and ethanol. Water and ethanol may be used in combination.
Examples of the pulverizing device used in the pulverizing step include jaw crushers, cone crushers, impact crushers, roller crushers, choppers, mashers, ring mills, jet crushers, hammer mills, pin crushers, ball mills, vibration mills, bead mills, cyclone grinders, and the like. The pulverizing conditions are not particularly limited. The pulverizing time, the rotation speed, etc. may be appropriately adjusted according to the particle size of the mixed powder, the kind of the pulverizing apparatus used, etc., thereby achieving a desired particle size distribution.
In this production method, the pulverized mixed powder is supplied to the firing step as a precursor (mixture before firing). The particle size of the precursor to be used in the firing step is not particularly limited as long as the object of the present application is achieved. From the viewpoint of promoting the recombination of magnesium oxide and aluminum oxide at a relatively low firing temperature, the particle size (D50) of the precursor, which is a volume-based cumulative distribution, is preferably 0.1 μm to 1.0 μm, more preferably 0.2 μm to 0.9 μm, and still more preferably 0.2 μm to 0.8 μm. The particle size of the precursor can be measured by the same method as that for the magnesium source and the aluminum source.
In the case where the pulverization in the pulverization step is wet pulverization, a pulverized product slurry including the pulverized mixed powder and the solvent is obtained. The dried powder obtained by drying the pulverized slurry to remove the solvent is used as a precursor for the firing step. The drying method of the pulverized slurry is not particularly limited, and a known dryer such as a vacuum dryer, a spray dryer, or a freeze dryer may be appropriately selected and used. The drying method is not particularly limited, and may be adjusted in accordance with the drying apparatus used, the characteristics of the crushed slurry, and the like.
In this production method, the temperature at which the precursor is fired in the firing step is 1500 ℃ or lower. The precursor is fired at a temperature of 1500 ℃ or lower, whereby a spinel material obtained by compounding magnesium oxide and aluminum oxide can be obtained. In addition, when the firing temperature is 1500 ℃ or lower, since strong sintering does not occur after firing, the possibility of mixing in foreign matter accompanying the pulverizing operation is reduced. The firing temperature is preferably 1500 ℃ or lower, more preferably 1470 ℃ or lower, and even more preferably 1450 ℃ or lower, from the viewpoint of achieving the desired high purity and not deteriorating the activity due to the high-temperature firing. The firing temperature is preferably 1400 ℃ or higher from the viewpoint of the reaction efficiency of forming the spinel phase.
The firing time can be appropriately adjusted according to the firing temperature. For example, the firing time is preferably 1 to 12 hours at a temperature of 1450 to 1500 ℃, and preferably 3 to 18 hours at a temperature of 1400 to 1450 ℃. By setting the firing time within this range, the spinel phase is sufficiently formed, and strong sintering is avoided.
Firing of the precursor is usually performed using a firing vessel. The type of the firing vessel is not particularly limited, and a general alumina sagger, magnesia sagger, or the like can be used. Preferably, in the firing step, the top surface of the firing vessel into which the precursor is put is covered with a lid. Thus, during the firing process, the contamination of impurities from the outside can be avoided. The material of the firing vessel and the lid is preferably high-purity magnesium oxide having a purity of 99.99wt% or more. By making the material of the firing vessel and the lid of high purity magnesia, transfer and mixing of impurities from the firing vessel and the lid are avoided, and higher purification of the obtained spinel powder is achieved.
The apparatus used for firing is not particularly limited as long as it can perform firing at 1500 ℃. Known firing furnaces such as a box furnace, a crucible furnace, a tube furnace, a tunnel furnace, a vacuum furnace, a furnace bottom lift furnace, a resistance heating furnace, an induction heating furnace, and a through-electric furnace can be used.
The spinel powder may be obtained by crushing or pulverizing the spinel raw material obtained in the firing step, and adjusting the particle diameter and the particle size distribution. As the crushing or pulverizing, for example, jaw crushers, gyratory crushers, cone crushers, impact crushers, roll crushers, choppers, stamp crushers, ring crushers, roll grinders, jet crushers, hammer grinders, roller grinders, vibration grinders, planetary grinders, ball grinders, cyclone grinders, and the like can be used.
The conditions for crushing or pulverizing are not particularly limited, and may be appropriately adjusted depending on the type of apparatus used, the composition of the precursor, the particle size, the firing conditions, and the like. For example, the purity of the spinel powder is maintained by adjusting the rotational speed, the treatment time, and the like during crushing and pulverizing to avoid mixing of impurities. Thereby, a high purity spinel powder having a desired particle size and particle size distribution is obtained. For example, when the pulverization is performed using a dry ball mill, the preferable pulverization time is 24 hours, and the preferable rotation speed is 80rpm.
Examples:
the effects of the present application are illustrated by the following examples, but the present application should not be construed as being limited based on the description of the examples. In the examples and comparative examples described below, the properties of each substance were measured in the following manner.
[ particle size ]
The particle diameter (D10) of the spinel powder was measured to have a volume-based cumulative distribution of 10%, the particle diameter (D50) of the spinel powder was measured to have a volume-based cumulative distribution of 50%, and the particle diameter (D90) of the spinel powder was measured to have a volume-based cumulative distribution of 90%, using a laser diffraction/scattering particle size distribution measuring instrument (commercially available from daily necessities, inc.). The assay samples were prepared by the following method: after each spinel powder was added to methanol, dispersion treatment was performed at 120W for 3 minutes by an ultrasonic homogenizer (manufactured by Japanese refiner, inc. under the trade name "US-300T").
[ composition ratio of spinel powder ]
The composition analysis of the spinel powder was performed by a microglass bead milling method using a multi-element simultaneous X-ray fluorescence analyzer (manufactured by Rigaku Co., ltd., trade name "Simultix 12"). The contents of Al and Mg were calculated in terms of oxides to obtain MgO and Al 2 O 3 Is a component ratio of (3).
Purity of spinel powder and content of various elements
A solution diluted with ultrapure water after the spinel powder was completely dissolved was prepared as a measurement sample. The content of each element in the measurement sample was measured by an ICP emission spectrometry device (Hitachi High-Tech Science Corporation, manufactured by Hitachi, inc.), under the trade name "PS3520 VDD". The detected elements other than Mg and Al were Ca, si, fe, mn, ni, cu, zn, na, P, S, B, ti, zr and Ba. The sum of the contents of these elements was calculated as the total content (ppm). In addition, since the content is less than 1ppm (< 1), the total content is not counted up below the detection limit. The total content was converted into% and subtracted from 100%, whereby the purity (wt%) of the spinel powder was calculated.
[ purity of magnesium oxide and aluminum oxide ]
Magnesium oxide and aluminum oxide were measured using a multi-element simultaneous X-ray fluorescence analyzer (manufactured by Rigaku Co., ltd., trade name "Simultix 12"). The purity of magnesium oxide and aluminum oxide was determined by converting the total content (ppm) of the elements other than Mg, al and O detected into% and subtracting from 100%. The main element other than Mg and Al detected was Ca, si, fe, mn, ni, cu, zn.
[ example 1 ]
The magnesium chloride aqueous solution with the concentration of Mg ions adjusted to 2.0mol/L and the sodium hydroxide aqueous solution with the concentration adjusted to 2.7mol/L are respectively transferred to a reaction tank by a metering pump, and continuous chemical combination reaction is carried out. The reaction rate of sodium hydroxide to magnesium chloride was controlled to be 90mol%. The resulting reaction slurry was overflowed from the reaction tank with a residence time of 30 minutes and recovered. The reaction slurry (magnesium hydroxide slurry) was filtered, washed and dried to obtain a magnesium hydroxide dry powder. The purity of the obtained magnesium hydroxide dry powder was 99.99% or more, and the particle diameter (D50) at which the cumulative distribution on a volume basis was 50% was 0.58. Mu.m.
MgO in terms of oxide is the composition ratio of Mg to Al: al (Al) 2 O 3 Is 1:1, mixing an aluminum hydroxide powder having a purity of 99.99% or more and a cumulative volume-based distribution of 50% and a particle diameter (D50) of 0.20 μm with the magnesium hydroxide dry powder obtained by the above method, and then thoroughly and uniformly mixing by a dry method, thereby obtaining a mixed powder of magnesium hydroxide and aluminum hydroxide.
Mixing the obtained mixed powder with a solvent (industrial ethanol) according to a mass ratio of 1:1 (filling ratio 35%) was charged into a pot mill, and wet grinding was performed by a ball mill (rotation speed 80rpm/24 hours). Thereafter, the slurry of the content was collected and sufficiently dried by an explosion-proof dryer to obtain a mixture (precursor) before firing.
The mixture before firing was filled into a square alumina sagger, heated and fired at 1400 ℃ for 3 hours, and cooled, whereby a spinel raw material was obtained. The spinel raw material and a solvent (industrial ethanol) are mixed according to the mass ratio of 1:1 was charged into a pot mill (charging rate: 35%) and wet-milled by a ball mill (rotation speed: 80rpm/24 hours). Thereafter, the spinel powder of example 1 was obtained by recovering a slurry of the content and passing through a 500-mesh sieve and then drying it with an explosion-proof dryer. The composition ratio, particle diameter and purity of the spinel powder of example 1 are shown in table 1 below. The contents of the various elements in the spinel powder and the total contents are shown in table 2 below.
[ comparative example 1 ]
The procedure of example 1 was repeated except that an aluminum hydroxide powder having a purity of 99.99% or more and a volume-based cumulative distribution of 50% and a particle diameter (D50) of 8.3 μm was used, thereby obtaining a spinel powder of comparative example 1. The composition ratio, particle diameter and purity of the spinel powder of comparative example 1 are shown in table 1 below. The contents of the various elements in the spinel powder and the total contents are shown in table 2 below.
[ Table 1 ]
(Table 1)
。
[ Table 2 ]
(Table 2)
。
As shown in Table 1 and Table 2, in example 1, spinel powders having a purity of 99.95% by weight or more and an extremely low impurity content were obtained. The content of Ca and Si in the spinel powder is less than 30mm. In contrast, in comparative example 1, the purity was less than 99.95wt%, and the content of Ca and Si was 30ppm or more. From the evaluation results, the superiority of the present application was apparent.
Industrial applicability:
the spinel powder described above is suitable for various fields where a high purity ceramic sintered body is required.
Claims (2)
1. A method for preparing spinel powder, which is characterized by comprising the following procedures:
a mixing step of mixing a magnesium source having a purity of 99.95wt% or more and an aluminum source having a purity of 99.95wt% or more to obtain a mixed powder;
a pulverizing step of pulverizing the mixed powder to obtain a precursor; and
a firing step of firing the precursor at a temperature of 1500 ℃ or lower;
the aluminum source is at least one of aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum nitrate, aluminum acetate and aluminum sulfate;
the magnesium source and the aluminum source are powders composed of a plurality of particles, and the ratio D50 (1)/D50 (2) of the particle diameter D50 (1) of 50% of the cumulative distribution of the volume basis of the magnesium source to the particle diameter D50 (2) of 50% of the cumulative distribution of the volume basis of the aluminum source is not less than 0.2 and not more than 5.0.
2. The method according to claim 1, wherein,
the pulverizing step is performed by wet pulverizing.
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| WO2018066636A1 (en) * | 2016-10-05 | 2018-04-12 | 信越化学工業株式会社 | Transparent spinel sintered body, optical member and method for producing transparent spinel sintered body |
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| DE19515490A1 (en) * | 1995-04-27 | 1996-10-31 | Abb Patent Gmbh | Ceramic material and process for its manufacture |
| JP2011063467A (en) * | 2009-09-16 | 2011-03-31 | Sumitomo Electric Ind Ltd | Production process for oxide ceramic, translucent spinel ceramic structure, and optical device for color crystal liquid projector |
| WO2013038916A1 (en) | 2011-09-14 | 2013-03-21 | 京セラ株式会社 | Magnesium aluminate-based sintered body and member for use in semiconductor manufacturing devices |
| WO2014119177A1 (en) | 2013-01-30 | 2014-08-07 | 京セラ株式会社 | Gas nozzle and plasma device employing same |
| FR3018804B1 (en) | 2014-03-18 | 2016-03-25 | Saint Gobain Ct Recherches | FADE GRAINS OF MAGNESIUM ALUMINATE RICH IN MAGNESIUM. |
| EP3218324A4 (en) | 2014-11-10 | 2018-04-11 | Saint-Gobain Ceramics&Plastics, Inc. | Sintered ceramic component and a process of forming the same |
| EP3250510B1 (en) | 2015-01-28 | 2021-11-17 | Sasol (USA) Corporation | Method of producing magnesium aluminate spinels |
| JP6845645B2 (en) | 2016-09-26 | 2021-03-24 | タテホ化学工業株式会社 | Magnesium oxide-containing spinel powder and its manufacturing method |
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| CN103204528A (en) * | 2013-04-26 | 2013-07-17 | 沈阳三聚凯特催化剂有限公司 | Preparation method for magnesia-alumina spinel |
| WO2018066636A1 (en) * | 2016-10-05 | 2018-04-12 | 信越化学工業株式会社 | Transparent spinel sintered body, optical member and method for producing transparent spinel sintered body |
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