WO2021161661A1 - グラスライニング製品の製造方法 - Google Patents
グラスライニング製品の製造方法 Download PDFInfo
- Publication number
- WO2021161661A1 WO2021161661A1 PCT/JP2020/047753 JP2020047753W WO2021161661A1 WO 2021161661 A1 WO2021161661 A1 WO 2021161661A1 JP 2020047753 W JP2020047753 W JP 2020047753W WO 2021161661 A1 WO2021161661 A1 WO 2021161661A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- glaze
- frit
- mass
- glass lining
- particle size
- Prior art date
Links
- 239000011521 glass Substances 0.000 title claims abstract description 94
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 95
- 239000002184 metal Substances 0.000 claims abstract description 95
- 239000002245 particle Substances 0.000 claims abstract description 94
- 238000010304 firing Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims description 66
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 19
- 230000003746 surface roughness Effects 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 10
- 239000004575 stone Substances 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- -1 platinum group metals Chemical class 0.000 claims description 5
- 229910000510 noble metal Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 abstract description 46
- 229910052708 sodium Inorganic materials 0.000 abstract description 14
- 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 abstract description 11
- 238000010828 elution Methods 0.000 abstract description 11
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 3
- 229910052681 coesite Inorganic materials 0.000 abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract 3
- 229910052682 stishovite Inorganic materials 0.000 abstract 3
- 229910052905 tridymite Inorganic materials 0.000 abstract 3
- 238000009304 pastoral farming Methods 0.000 abstract 2
- 239000002585 base Substances 0.000 description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000002270 dispersing agent Substances 0.000 description 16
- 238000009826 distribution Methods 0.000 description 16
- 239000000203 mixture Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- 239000002562 thickening agent Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 description 10
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 10
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 10
- 239000010419 fine particle Substances 0.000 description 10
- 239000007921 spray Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 8
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 7
- 239000000654 additive Substances 0.000 description 7
- 238000007561 laser diffraction method Methods 0.000 description 7
- 238000005488 sandblasting Methods 0.000 description 7
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000001186 cumulative effect Effects 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 4
- 229910001626 barium chloride Inorganic materials 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 235000010288 sodium nitrite Nutrition 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 229910052570 clay Inorganic materials 0.000 description 3
- 239000006103 coloring component Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 2
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000156 glass melt Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 2
- 238000009863 impact test Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- 230000004520 agglutination Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D5/00—Coating with enamels or vitreous layers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/22—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions containing two or more distinct frits having different compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/18—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing free metals
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/08—Glass having a rough surface
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/02—Fibres; Filaments; Yarns; Felts; Woven material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/08—Metals
Definitions
- the present invention relates to a method for manufacturing a glass lining product.
- Glass-lining products are used in fields such as the chemical industry, pharmaceutical industry, food industry, and electronics industry, where high corrosion resistance and high product purity are required.
- the glass lining product is made of a metal base material such as a low carbon steel plate and a stainless steel plate as a base material, and a glass lining composition having a predetermined composition containing SiO 2 as a main component is fused to the surface of the base material to make it corrosion resistant and inert. It is manufactured by forming a glass lining layer that also has heat resistance.
- the temperature inside the product is often controlled by heating or cooling the iron material from the outside of the product using a jacket or the like installed on the outside of the product. Since the thermal conductivity is worse than that of the metal base material, there is a problem that it is difficult to finely control the temperature. Further, due to the poor thermal conductivity of the glass lining layer, the manufacturing lead time may be lengthened, and the product quality and yield may be deteriorated.
- the particle size composition of the frit constituting the glass lining slurry composition within a specific range (Patent Document 1: Patent No. 5860713). Gazette). Specifically, the particle size of the frit is in the range of 0.1 to 250 ⁇ m, and the proportion of the frit fine particles in the range of 0.1 to 1 ⁇ m is in the range of 1 to 50% by mass. Further, a glass lining composition has been proposed in which the normal distribution of the particle size of the frit is displayed at 50% and is composed of the frit within the range of 1.5 to 20 ⁇ m.
- Na 2 O is conventionally blended in order to match the coefficient of thermal expansion with the metal base material, lower the temperature at the time of melting the glass, and ensure the solubility of a plurality of components. That is, Na 2 O acts to modify the glass network structure of the glass lining, cut the SiO 2 network structure, (i) increase the coefficient of linear thermal expansion, and (ii) increase the solubility. Therefore, it is an essential ingredient for glass lining.
- the sodium component is easily eluted from the glass lining layer containing Na 2 O, and this sodium component is mixed in the chemical solution in the chemical solution manufacturing process. Therefore, the chemical solution used in the manufacturing process of semiconductors and TFT type panels. Conventional glass lining products cannot be used in the manufacture of.
- Patent Document 2 Japanese Patent No. 5191384.
- the conventional glass lining layer is an insulating material having a volume resistivity of 1 ⁇ 10 10 to 1 ⁇ 10 12 ⁇ ⁇ m, it is possible to stir and operate an organic content liquid such as benzene or normal hexane having low conductivity. The amount of electric charge generated by the liquid greatly exceeded the amount of electric charge leaked, and the electrostatic charge became large, which could cause dielectric breakdown of the glass lining layer even if the ground was grounded to the glass lining product.
- Patent Document 3 Japanese Patent No. 3783742
- Patent Document 4 Patent No. 4: 3432399 (Ab.).
- a glass lining product capable of suppressing the elution amount of a sodium component has a problem that heat transfer is poor due to the presence of air bubbles in the glass and a thick film thickness, and the productivity is lowered in applications involving heat exchange. Further, even if the elution amount of the sodium component can be suppressed, the electrostatic charge cannot be suppressed.
- a glass lining product capable of suppressing electrostatic charge has a problem that heat transfer is poor due to the presence of air bubbles in the glass and a thick film thickness, and the productivity is lowered in applications involving heat exchange. Also, it cannot be used in fields where the sodium component is disliked. Therefore, it is desirable to obtain a hybrid type glass lining product having a plurality of characteristics.
- the present invention has been made in view of the above circumstances, and in one embodiment, it is an object of the present invention to provide a method for producing a glass lining product which is excellent in heat transfer and can suppress the elution amount of a sodium component. In a preferred embodiment, it is an object of the present invention to provide a method for producing a glass lining product capable of further suppressing electrostatic charge.
- the first glaze contains 0.01 to 5 parts by mass of metal fibers having a diameter of 0.1 to 2 ⁇ m and a length of 50 to 1000 ⁇ m with respect to 100 parts by mass of the frit in the first glaze.
- the second glaze contains 0.01 to 5 parts by mass of metal fibers having a diameter of 0.2 to 2 ⁇ m and a length of 50 to 1000 ⁇ m with respect to 100 parts by mass of the frit in the second glaze.
- the third glaze contains 0.01 to 5 parts by mass of metal fibers having a diameter of 0.2 to 2 ⁇ m and a length of 50 to 1000 ⁇ m with respect to 100 parts by mass of the frit in the third glaze.
- [5] The method for producing a glass lining product according to any one of [1] to [4], wherein the surface of the metal base material has a surface roughness Ra of 2 to 10 ⁇ m measured by JIS B 0633: 2001.
- the average particle size of the frit in the third glaze is larger than the average particle size of the frit in the first glaze and the average particle size of the frit in the second glaze. How to make glass lining products.
- the method for manufacturing a glass lining product according to an embodiment of the present invention is as follows. On the surface of the metal substrate, A frit having an average particle size of 1.5 to 20 ⁇ m containing SiO 2 as a main component and Na 2 O; and one or more kinds of inorganic refractory powders selected from the group consisting of silica stone, alumina and aluminum nitride. body; A step of forming a ground coat layer having a thickness of 0.1 to 0.5 mm composed of one layer or a plurality of layers by glazing and firing the first glaze containing the above.
- One or more layers are formed by glazing and firing a second glaze containing a frit having an average particle size of 1.5 to 20 ⁇ m, which contains SiO 2 as a main component and Na 2 O, on the ground coat layer.
- a step of forming an intermediate layer having a thickness of 0.4 to 1.1 mm and On the intermediate layer contains no Na 2 O, by the average particle diameter as a main component SiO 2 is glazed third glaze containing frit 1.5 ⁇ 50 [mu] m, baked, one or more layers
- FIG. 1 schematically shows an example of a layer structure of the glass lining product 10 obtained by the manufacturing method.
- the glass lining product 10 has a surface structure in which a ground coat layer 12, an intermediate layer 13, and a cover coat layer 14 are laminated in this order on the surface of the metal base material 11.
- the total thickness of the ground coat layer, the intermediate layer and the cover coat layer is 0.6 to 1.8 mm.
- the total thickness is 1.8 mm or less, preferably 1.4 mm or less, the effect of improving thermal conductivity can be obtained.
- the total thickness is 0.6 mm or more, preferably 0.8 mm or more, safe corrosion resistance as a product can be obtained.
- Glass lining products include, but are not limited to, reactors, stirring blades, tanks (eg, stirring tanks), heat exchangers, dryers, evaporators, filters, etc.
- the ground coat layer is formed by glazing a first glaze on the surface of a metal base material and firing it.
- the metal base material include, but are not limited to, iron alloys such as low carbon steel and stainless steel.
- the shape of the metal base material is also not particularly limited, and examples thereof include a wall shape, a plate shape, a wing shape, and a rod shape.
- the surface roughness Ra (JIS B 0601: 1994) measured by JIS B 0633: 2001 is preferably 2 to 10 ⁇ m, and more preferably 2 to 9 ⁇ m on the surface of the metal base material.
- the surface roughness Ra of the metal substrate is preferably 3 ⁇ m or more, more preferably 5 ⁇ m or more.
- the upper limit of the surface roughness Ra of the metal base material is 9 ⁇ m or less, an advantage of suppressing the generation of coarse bubbles in the ground coat layer can be obtained.
- the surface roughness Ra of the metal substrate is preferably 8 ⁇ m or less, more preferably 7 ⁇ m or less.
- the surface of the metal base material preferably has a surface roughness Rz (10-point average roughness) (JIS B 0601: 1994) measured by JIS B 0633: 2001 of 15 to 39 ⁇ m.
- Rz 10-point average roughness
- the surface roughness Rz of the metal substrate is preferably 20 ⁇ m or more, and more preferably 25 ⁇ m or more.
- the upper limit of the surface roughness Rz of the metal base material is 39 ⁇ m or less, an advantage of suppressing the generation of coarse bubbles in the ground coat layer can be obtained.
- the surface roughness Rz of the metal substrate is preferably 37 ⁇ m or less, more preferably 35 ⁇ m or less.
- the surface roughness of the metal base material can be controlled by performing a roughening treatment.
- the surface of a metal base material can be roughened by sandblasting.
- the sandblasting process comprises spraying an abrasive having an average particle size of 0.5 mm or more and 1.6 mm or less.
- the surface of the metal base material can be easily controlled within the above-mentioned range, and the ground coat layer and the metal can be easily controlled. Adhesion of the base material is likely to be improved.
- the abrasive although not limited, alumina powder, iron grid powder, iron shot powder and the like can be preferably used for the reason of preventing excessive reaction with glass.
- the average particle size of the abrasive is plotted as an integrated percentage (mass%) with respect to the nominal opening of each sieve obtained by a sieving test using a test sieve specified in JIS Z8801-1: 2019. Then, in the figure in which each point is connected by a straight line, the average particle size is defined by the value of the opening at which the integrated percentage is 50% by mass.
- Conditions such as glazing operation and firing temperature for forming the ground coat layer are not particularly limited, and conventional and known operations in glass lining can be used.
- the glaze operation is preferably sprayed because the thickness can be easily controlled.
- the firing temperature is preferably 800 to 900 ° C. for the reason of suppressing deformation of the metal base material.
- the thickness of the ground coat layer formed by glazing the first glaze on the surface of the metal base material and firing it is preferably 0.1 to 0.5 mm. When the thickness of the ground coat layer is 0.5 mm or less, the thermal conductivity can be enhanced.
- the thickness of the ground coat layer is more preferably 0.4 mm or less. Further, when the thickness of the ground coat layer is 0.1 mm or more, a stable glass lining layer can be obtained.
- the thickness of the ground coat layer is more preferably 0.2 mm or more.
- the ground coat layer can be composed of one layer or a plurality of layers.
- the first glaze is one selected from the group consisting of a frit containing SiO 2 as a main component and Na 2 O and having an average particle size of 1.5 to 20 ⁇ m, and silica stone, alumina, and aluminum nitride. Alternatively, it contains two or more kinds of inorganic refractory powders.
- the upper limit of the average particle size of the frit in the first glaze is 20 ⁇ m or less, it is possible to glaz with a very thin thickness, the obtained glass lining layer can be remarkably thinned, and the frit particles can be made significantly thinner. Since the gap between them becomes smaller, the diameter of the internal bubbles in the glass lining layer can be reduced.
- the average particle size of the frit is preferably 15 ⁇ m or less, more preferably 10 ⁇ m or less. Further, when the lower limit of the average particle size of the frit is 1.5 ⁇ m or more, it is possible to obtain an advantage that agglutination of particles is less likely to occur and the uniformity of the film thickness when the film is thinned can be improved.
- the average particle size of the frit is preferably 3 ⁇ m or more, more preferably 5 ⁇ m or more.
- the average particle size of the frit refers to the median diameter (D50) when the cumulative particle size distribution on a volume basis is measured by a laser diffraction method. In the examples, the measurement was performed by a laser diffraction particle size distribution device (model: LMS-30) manufactured by Seishin Enterprise Co., Ltd.
- the frit in the first glaze preferably contains frit fine particles having a particle size in the range of 0.1 to 1 ⁇ m in an amount of 1 to 50% by mass, more preferably 1.5 to 30% by mass.
- the proportion of the frit fine particles having a particle size in the range of 0.1 to 1 ⁇ m is 1% by mass or more, it is possible to obtain an advantage that uniform thinning can be easily performed. Further, when the ratio of the frit fine particles is 50% by mass or less, it is possible to prevent the ground coat layer from being turned over or cracking.
- the content ratio of the frit fine particles in which the particle size in the frit is in the range of 0.1 to 1 ⁇ m is determined based on the volume-based particle size distribution measured by the laser diffraction method. In the examples, the measurement was performed by a laser diffraction particle size distribution device (model: LMS-30) manufactured by Seishin Enterprise Co., Ltd.
- the particle size of the frit in the first glaze is preferably in the range of 0.1 to 250 ⁇ m, more preferably in the range of 0.1 to 149 ⁇ m.
- the particle size of the frit is 0.1 ⁇ m or more, it is possible to prevent the particles from agglomerating. Further, when the particle size of the frit is 250 ⁇ m or less, the film thickness uniformity when the spray gun is applied can be improved.
- the range of the particle size of the frit can be obtained from the volume-based cumulative particle size distribution measured by the laser diffraction method.
- the glass melt having a predetermined composition is rapidly cooled and roughly pulverized, then dry pulverized by a ball mill using alumina balls, and further classified and pulverized as appropriate. Can be obtained at.
- the frit in the first glaze contains SiO 2 as a main component and Na 2 O.
- the first glaze forms a ground coat layer that adheres to the metal substrate. Therefore, it is important to improve the adhesion by bringing the coefficient of thermal expansion closer to the metal substrate by containing Na 2 O.
- the fact that the frit contains SiO 2 as a main component means that the mass concentration of SiO 2 in the frit is the highest.
- the concentration of SiO 2 in the frit is preferably 41 to 72% by mass, more preferably 50 to 65% by mass.
- the concentration of Na 2 O in the frit is preferably 8 to 22% by mass, more preferably 10 to 15% by mass.
- the frit in the first glaze has the following composition.
- the content of the component (A) in the frit is 41% by mass or more, it is possible to prevent the strength of the frit itself from decreasing. Further, when the content of the component (A) in the frit is 72% by mass or less, it is possible to prevent the melt viscosity of the frit from becoming too high and the melting point of the first glaze from rising excessively.
- the meltability of the frit can be improved. Further, when the content of the component (B) in the frit is 22% by mass or less, it is possible to prevent the linear thermal expansion coefficient of the frit from being excessively increased and the physical property balance from being lost.
- the content of the component (C) in the frit is 1% by mass or more, the alkali resistance performance of the frit can be improved.
- the content of the component (C) in the frit is 7% by mass or less, it is possible to prevent the melt viscosity of the frit from becoming too high and the melting point of the first glaze from rising excessively.
- the content of the component (D) in the frit is 1% by mass or more, the effect of preventing devitrification can be obtained. Further, when the content of the component (D) in the frit is 18% by mass or less, the foaming phenomenon during firing can be suppressed.
- the content of the component (E) in the frit is 6% by mass or less, the effect of improving the adhesion to the metal substrate can be obtained while suppressing the foaming phenomenon during firing.
- the first glaze further contains one or more inorganic refractory powders selected from the group consisting of silica stone, alumina and aluminum nitride.
- the content of the inorganic refractory powder can be 20 to 120 parts by mass, preferably 40 to 100 parts by mass with respect to 100 parts by mass of the frit.
- the content of the inorganic refractory powder is 20 parts by mass or more with respect to 100 parts by mass of the frit, the content effect is significantly exhibited. Further, when the content of the inorganic refractory powder is 120 parts by mass or less with respect to 100 parts by mass of the frit, firing defects are less likely to occur.
- the particle size of the inorganic refractory powder is preferably 149 ⁇ m or less, and more preferably in the range of 0.1 to 74 ⁇ m.
- the particle size of the inorganic refractory powder is 149 ⁇ m or less, the ground coat layer can be easily thinned uniformly.
- the particle size of the inorganic refractory powder is 0.1 ⁇ m or more, it is easy to uniformly disperse in the first glaze.
- the range of the inorganic refractory powder can be determined from the volume-based cumulative particle size distribution measured by the laser diffraction method.
- the average particle size of the inorganic refractory powder can be 5 to 50 ⁇ m, preferably 10 to 40 ⁇ m, and more preferably 15 to 25 ⁇ m.
- the average particle size of the inorganic fire-resistant powder refers to the median diameter (D50) when the cumulative particle size distribution on a volume basis is measured by a laser diffraction method. In the examples, the measurement was performed by a laser diffraction particle size distribution device (model: LMS-30) manufactured by Seishin Enterprise Co., Ltd.
- the first glaze can further contain metal fibers.
- the metal fiber is not limited, but preferably contains one or more selected from the group consisting of stainless-based metal fibers, noble metal-based metal fibers, and alloy fibers of platinum and platinum group metals.
- the noble metal-based metal fiber include Ag fiber (volume resistivity: 1.6 ⁇ 10 -8 ⁇ m), Au fiber (volume resistivity: 2.4 ⁇ 10 -8 ⁇ m), and Pt fiber (volume resistivity: 10). .6 ⁇ 10 -8 ⁇ m) etc. can be used.
- the alloy fiber of platinum and the platinum group metal for example, an alloy of Pt and one or more selected from the group consisting of Pd, Ir, Rh, Os and Ru can be used.
- the amount of the metal fiber added to the frit is preferably 0.01 to 5 parts by mass with respect to 100 parts by mass of the frit.
- the amount of the metal fiber added is more preferably 0.05 parts by mass or more, and even more preferably 0.1 parts by mass or more with respect to 100 parts by mass of the frit.
- the amount of the metal fiber added is 5 parts by mass or less with respect to 100 parts by mass of the frit, the spray workability is improved.
- the amount of the metal fiber added is more preferably 2 parts by mass or less with respect to 100 parts by mass of the frit, and even more preferably 1 part by mass or less.
- the diameter of the metal fiber is preferably 0.1 to 2 ⁇ m, more preferably 0.2 to 2 ⁇ m, and further preferably 0.3 to 1 ⁇ m.
- the diameter of the metal fiber is 0.1 ⁇ m or more, the metal fiber can be processed at low cost. Further, when the diameter of the metal fiber is 2 ⁇ m or less, the spray workability is improved.
- the diameter of a metal fiber refers to the diameter of a circle equal to the area of a cross section orthogonal to the extending direction of the metal fiber.
- the length of the metal fiber is preferably 50 to 1000 ⁇ m, more preferably 100 to 800 ⁇ m.
- the length of the metal fiber is 50 ⁇ m or more, the effect of adding the metal fiber is significantly more likely to be exhibited. Further, when the length is 1000 ⁇ m or less, the spray workability is improved.
- the average aspect ratio of the length / diameter of the metal fiber is preferably 50 or more.
- the electric resistance of the glass lining layer can be reduced without blending a large amount of metal fibers.
- the first glaze contains metal fibers
- a thickener By adding a thickener, it is possible to prevent the metal fibers from settling and unevenly distributed downward in the first glaze. Thereby, the effect of improving the conductivity and the effect of improving the thermal conductivity of the glass lining layer can be obtained.
- the thickener is preferably added in an amount of 32 to 65 parts by mass, more preferably 38 to 60 parts by mass, and even more preferably 45 to 55 parts by mass with respect to 100 parts by mass of the frit. When the amount of the thickener added is 45 parts by mass or more with respect to 100 parts by mass of the frit, the effect of preventing the metal fibers from settling can be enhanced. Further, when the amount of the thickener added is 65 parts by mass or less with respect to 100 parts by mass of the frit, the effect of improving the spray workability can be obtained.
- a cellulose derivative can be preferably used, although it is not limited.
- the cellulose derivative include CMC (carboxymethyl cellulose), HEC (hydroxyethyl cellulose), HPMC (hydroxypropyl methyl cellulose), hydroxypropyl cellulose (HPC), methyl cellulose (MC) and the like.
- CMC carboxymethyl cellulose
- HEC hydroxyethyl cellulose
- HPMC hydroxypropyl methyl cellulose
- HPC hydroxypropyl cellulose
- MC methyl cellulose
- One type of thickener may be used alone, or two or more types may be used in combination.
- the first glaze contains metal fibers
- a dispersant By adding the dispersant, the uniform dispersibility of the metal fiber can be improved, and thereby the effect of improving the conductivity and the effect of improving the thermal conductivity can be obtained.
- a glaze suitable for spraying can be obtained without using alcohol as a solvent.
- the dispersant is preferably added in an amount of 0.01 to 0.2 parts by mass, more preferably 0.02 to 0.1 parts by mass, and 0.03 to 0.08 parts by mass with respect to 100 parts by mass of the frit. It is even more preferable to add it.
- the amount of the dispersant added is 0.01 parts by mass or more with respect to 100 parts by mass of the frit, the dispersibility of the metal fiber can be enhanced. Further, when the amount of the dispersant added is 0.2 parts by mass or less with respect to 100 parts by mass of the frit, the effect of suppressing odor can be obtained.
- the dispersant is not limited, but is a polymer such as a polycarboxylic acid dispersant, a sodium phthalene sulfonic acid formalin condensation type, polyethylene glycol, a polyether type, and a polyalkylene polyamine type for the reason of suppressing the generation of air bubbles during firing.
- a type dispersant can be preferably used.
- the polycarboxylic acid-based dispersant for example, an ammonium polycarboxylic acid salt can be preferably used.
- One type of dispersant may be used alone, or two or more types may be used in combination.
- additives commonly used for glass lining for example, clay, barium chloride, sodium nitrite, etc.
- a predetermined amount of solvent can be added to the first glaze.
- the clay can be added in an amount of 3 to 8 parts by mass, preferably 5 to 7 parts by mass with respect to 100 parts by mass of the frit, although not limited.
- Barium chloride can be added in an amount of 0.05 to 0.3% by mass, preferably 0.1 to 0.2% by mass, based on 100 parts by mass of the frit, without limitation.
- Sodium nitrite can be added in an amount of 0.1 to 0.6 parts by mass, preferably 0.2 to 0.5 parts by mass, based on 100 parts by mass of the frit, without limitation.
- the solvent used include, but are not limited to, water-soluble solvents such as water and alcohol, and water is preferable because it has no odor and improves the working environment.
- the alcohol include ethanol.
- the solvent one type may be used alone, or two or more types may be mixed and used.
- the solvent can be added, but not limited to, from 0 to 40 parts by mass, preferably 5 to 30 parts by mass with respect to 100 parts by mass of the frit.
- the alcohol concentration in the first glaze is preferably 1% by mass or less, more preferably 0.1% by mass or less, and even more preferably 0% by mass.
- the intermediate layer is formed by glazing a second glaze on the ground coat layer and firing it.
- Conditions such as glazing operation and firing temperature for forming the intermediate layer are not particularly limited, and conventional and known operations in glass lining can be used.
- the glazed operation is preferably sprayed for the reason of thickness control.
- the firing temperature is preferably lower than that of the ground coat, it is preferably 700 to 800 ° C.
- the thickness of the intermediate layer formed by glazing a second glaze on the ground coat layer and firing is preferably 0.4 to 1.1 mm. When the thickness of the intermediate layer is 1.1 mm or less, the thermal conductivity can be enhanced.
- the thickness of the intermediate layer is more preferably 1.0 mm or less, and even more preferably 0.8 mm or less.
- the thickness of the intermediate layer is 0.4 mm or more, an advantage of suppressing air bubbles from the ground coat layer can be obtained.
- the thickness of the intermediate layer is more preferably 0.5 mm or more, and more preferably 0.6 mm or more.
- the intermediate layer can be composed of one layer or a plurality of layers.
- the second glaze contains a frit containing SiO 2 as a main component and Na 2 O, and having an average particle size of 1.5 to 20 ⁇ m. Since the preferred embodiment of the powder characteristics such as the average particle size of the frit, the ratio of the frit fine particles, and the particle size is the same as that of the frit in the first glaze, the description thereof will be omitted.
- the frit in the second glaze contains SiO 2 as a main component and Na 2 O. Since the second glaze also contains Na 2 O like the first glaze, it has an advantage of improving the adhesion to the ground coat layer.
- the fact that the frit contains SiO 2 as a main component means that the mass concentration of SiO 2 in the frit is the highest.
- the concentration of SiO 2 in the frit is preferably 41 to 72% by mass, more preferably 45 to 70% by mass.
- the concentration of Na 2 O in the frit is preferably 8 to 22% by mass, more preferably 10 to 20% by mass.
- the frit in the second glaze has the following composition for the same reasons as the frit in the first glaze.
- R'O R'represents Ca, Ba, Zn or Mg): 1 to 7% by mass However, CaO: 1-7% by mass BaO: 0 to 6% by mass ZnO: 0 to 6% by mass MgO: 0-5% by mass
- one or more inorganic refractory powders selected from the group consisting of silica stone, alumina and aluminum nitride are used because the firing temperature can be lower than that of the first glaze and the corrosion resistance is not lowered. It is preferable to have as few as possible.
- the content of the inorganic refractory powder is preferably 10 parts by mass or less, more preferably 5 parts by mass or less, and even more preferably 1 part by mass or less with respect to 100 parts by mass of the frit.
- the second glaze can further contain metal fibers. Since the second glaze contains metal fibers, the electrical resistance of the intermediate layer is reduced, it is possible to suppress electrostatic charge of the glass lining product, and it is also possible to improve the thermal conductivity. Since the preferred embodiment of the metal fiber such as the type, addition amount, diameter, length, and average aspect ratio of the metal fiber is the same as that of the metal fiber in the first glaze, detailed description thereof will be omitted.
- the second glaze contains metal fibers
- additives commonly used for glass lining for example, clay, barium chloride, sodium nitrite, etc.
- a predetermined amount of solvent can be added to the second glaze. Since the preferred embodiments of the additive and the solvent are the same as those of the additive in the first glaze, detailed description thereof will be omitted.
- cover coat layer is formed by glazing a third glaze on the intermediate layer and firing it.
- Conditions such as glazing operation and firing temperature for forming the cover coat layer are not particularly limited, and conventional and known operations in glass lining can be used.
- the glazed operation is preferably sprayed for the reason of thickness control.
- the firing temperature is preferably lower than that of the ground coat, it is preferably 700 to 800 ° C.
- the thickness of the cover coat layer formed by glazing a third glaze on the intermediate layer and firing is preferably 0.1 to 1.3 mm. When the thickness of the cover coat layer is 1.3 mm or less, the thermal conductivity can be enhanced.
- the thickness of the cover coat layer is more preferably 1.0 mm or less, and even more preferably 0.8 mm or less.
- the thickness of the cover coat layer is 0.1 mm or more, there is an advantage that Na elution can be effectively suppressed.
- the thickness of the cover coat layer is more preferably 0.2 mm or more, and even more preferably 0.3 mm or more.
- the cover coat layer can be composed of one layer or a plurality of layers.
- the third glaze does not contain Na 2 O and contains a frit containing SiO 2 as a main component and having an average particle size of 1.5 to 50 ⁇ m.
- the average particle size of the frit in the third glaze can be 1.5 to 20 ⁇ m, similar to the average particle size of the frit in the first glaze and the frit in the second glaze, which is preferable.
- the range is similar to the average particle size of the frit in the first glaze and the frit in the second glaze.
- the average particle size of the frit in the third glaze can be 10 to 50 ⁇ m. In this case, it may be larger than the average particle size of the frit in the first glaze and the average particle size of the frit in the second glaze. Since the average particle size of the frit in the third glaze is larger than the average particle size of the frit in the first glaze and the average particle size of the frit in the second glaze, there is an advantage that the thickness can be easily secured. When the upper limit of the average particle size of the frit is 10 ⁇ m or more, there is an advantage that the construction can be made thicker.
- the average particle size of the frit is preferably 20 ⁇ m or more, more preferably 30 ⁇ m or more.
- the upper limit of the average particle size of the frit is preferably 50 ⁇ m or less, and more preferably 40 ⁇ m or less because the spray workability is deteriorated.
- the upper limit of the average particle size of the frit can be made larger than that in the first glaze and the second glaze, because it effectively suppresses Na elution.
- the frit in the third glaze preferably contains frit fine particles having a particle size in the range of 0.1 to 1 ⁇ m in an amount of 1 to 50% by mass, more preferably 1.5 to 30% by mass.
- the proportion of the frit fine particles having a particle size in the range of 0.1 to 1 ⁇ m is 1% by mass or more, it is possible to obtain an advantage that uniform thinning can be easily performed. Further, when the ratio of the frit fine particles is 50% by mass or less, it is possible to prevent the cover coat layer from being turned over or cracks.
- the content ratio of the frit fine particles in which the particle size in the frit is in the range of 0.1 to 1 ⁇ m is determined based on the volume-based particle size distribution measured by the laser diffraction method. In the examples, the measurement was performed by a laser diffraction particle size distribution device (model: LMS-30) manufactured by Seishin Enterprise Co., Ltd.
- the particle size of the frit in the third glaze is preferably in the range of 0.1 to 250 ⁇ m, and more preferably in the range of 0.1 to 149 ⁇ m.
- the particle size of the frit is 0.1 ⁇ m or more, it is possible to prevent the particles from agglomerating. Further, when the particle size of the frit is 250 ⁇ m or less, the film thickness uniformity when the spray gun is applied can be improved.
- the range of the particle size of the frit can be obtained from the volume-based cumulative particle size distribution measured by the laser diffraction method.
- the glass melt having a predetermined composition is rapidly cooled and roughly pulverized, then dry pulverized by a ball mill using alumina balls, and further classified and pulverized as appropriate. Can be obtained at.
- the frit in the third glaze does not contain Na 2 O and contains SiO 2 as a main component. Thereby, the elution amount of the sodium component can be suppressed.
- the fact that the frit contains SiO 2 as a main component means that the mass concentration of SiO 2 in the frit is the highest.
- the concentration of SiO 2 in the frit is preferably 40 to 75% by mass, more preferably 45 to 70% by mass. When the concentration of SiO 2 in the frit is 40% by mass or more, acid resistance and water resistance are improved. When the concentration of SiO 2 in the frit is 75% by mass or less, the viscosity does not become too high and the coefficient of linear thermal expansion does not become too small.
- the frit in the third glaze is selected from the group consisting of 40-75% by weight SiO 2 and 0-10% by weight ZrO 2 and R 2 O (where R is Li, K, and Cs). 1 type or 2 or more types) is 8 to 22% by mass, R'O (where R'indicates 1 type or 2 or more types selected from the group consisting of Mg, Ca, Sr, and Ba). Is contained in an amount of 1 to 7% by mass, and Na 2 O is not added.
- the content of ZrO 2 in the frit is 10% by mass or less, it becomes difficult to crystallize and it is possible to prevent the viscosity from becoming too high. Further, when the content of ZrO 2 in the frit is 0% by mass or more, water resistance and alkali resistance are improved.
- the preferred content of ZrO 2 in the frit is in the range of 2-8% by weight.
- R 2 O in the frit When the content of R 2 O in the frit is 22% by mass or less, the water resistance is less likely to decrease. Further, when the content of R 2 O in the frit is 8% by mass or more, it is possible to prevent the viscosity from becoming too high.
- the preferred content of R 2 O in the frit is in the range of 10-20% by weight.
- the acid resistance is improved.
- the content of R'O in the frit is 1% by mass or more, the water resistance is improved.
- the preferred content of R'O in the frit is in the range of 2-5% by weight.
- the frit may contain one or more selected from the group consisting of TiO 2 , Al 2 O 3 , La 2 O 3 , B 2 O 3 and Zn O. These components prevent phase separation and crystallization during glass lining firing, are strongly fixed in the glass network structure, fill and tighten the network, improve water resistance, and suppress the generation of air bubbles. do.
- the content of TiO 2 in the frit is 0 to 16% by mass, preferably 0 to 10% by mass, and the content of Al 2 O 3 is 0 to 6% by mass, preferably 0 to 4% by mass.
- La 2 O 3 content is 0 to 4% by mass, preferably 0 to 2% by mass
- B 2 O 3 content is 0 to 18% by mass, preferably 0 to 14% by mass
- ZnO content is in the range of 0 to 6% by mass, preferably 0 to 4% by mass, and when two or more kinds are used in combination, the total amount is 1 to 10% by mass, preferably 1 to 8% by mass. It is within the range. If the respective contents and the total contents of these components exceed the upper limit, the melting point of the frit becomes high and the solubility tends to deteriorate. Further, if it is below the lower limit, the addition effect is unlikely to appear.
- one or more coloring components selected from the group consisting of CoO, Sb 2 O 3 , Cr 2 O 3 , Fe 2 O 3 , SnO 2 and CeO 2 are added to 100% by mass of the frit.
- it can be blended in an amount of up to 3% by mass in terms of Fe 2 O 3 conversion amount.
- CoO which is a blue component, is preferable from the viewpoint of visibility. This has the advantage that the surface condition such as the corroded state of the glass lining layer can be easily recognized.
- the blending amount of the coloring component exceeds 3% by mass in terms of Fe 2 O 3 , the acid resistance is lowered, and the foaming phenomenon is likely to occur during firing.
- Japanese Patent No. 5156277 is incorporated herein by reference.
- the above SiO 2 , Al 2 O 3 and Ca O components can be used in the form of fluoride.
- the fluoride for example, K 2 SiF 6 , K 3 AlF 6 , CaF 2 and the like can be used.
- the amount of one or more kinds of inorganic refractory powders selected from the group consisting of silica stone, alumina and aluminum nitride is as small as possible in the third glaze.
- the content of the inorganic refractory powder is preferably 10 parts by mass or less, more preferably 5 parts by mass or less, and even more preferably 1 part by mass or less with respect to 100 parts by mass of the frit.
- the third glaze can further contain metal fibers.
- the electrical resistance of the cover coat layer is reduced, electrostatic charge of the glass lining product can be suppressed, and thermal conductivity can be improved. Since the preferred embodiment of the metal fiber such as the type, addition amount, diameter, length, and average aspect ratio of the metal fiber is the same as that of the metal fiber in the first glaze, detailed description thereof will be omitted.
- the third glaze contains metal fibers, it is preferable to add a thickener and a dispersant. Since the preferred embodiments of the thickener and the dispersant are the same as those of the thickener and the dispersant in the first glaze, detailed description thereof will be omitted.
- a conventional additive for example, clay, barium chloride, sodium nitrite, etc.
- a predetermined amount of solvent can be added to the glass lining composition as the third glaze. Since the preferred embodiments of the additive and the solvent are the same as those of the additive in the first glaze, detailed description thereof will be omitted.
- the frit prepared above was selected according to the test number as shown in Table 3, and a 1.5% by mass aqueous solution of CMC was mixed with 100 parts by mass of the frit at the mass ratio (in terms of solid content) shown in Table 3. It was put into a machine and stirred for 5 minutes. Then, ethanol was added to the mixer at the mass ratio shown in Table 3 and further stirred for 20 minutes to obtain a slurry-like second glaze.
- the frit prepared above was selected according to the test number as shown in Table 4, and a 1.5% by mass aqueous solution of CMC was mixed with 100 parts by mass of the frit at the mass ratio (in terms of solid content) shown in Table 4. It was put into a machine and stirred for 5 minutes. Then, ethanol was added to the mixer at the mass ratio shown in Table 4 and further stirred for 20 minutes to obtain a slurry-like third glaze.
- Examples 3 to 6, Comparative Example 4 The frit prepared above was selected according to the test number as shown in Table 2, and silica stone, platinum fiber and a 1.5% by mass aqueous solution of CMC were mixed in a mass ratio shown in Table 2 with respect to 100 parts by mass of the frit. And stirred for 10 minutes. Then, ethanol, water, and an ammonium polycarboxylic acid salt were added to the mixer at the mass ratios shown in Table 2 and further stirred for 20 minutes to obtain a slurry-like first glaze.
- the frit prepared above was selected according to the test number as shown in Table 3, and platinum fiber and a 1.5% by mass aqueous solution of CMC were added to the mixer at the mass ratio shown in Table 3 with respect to 100 parts by mass of the frit. And stirred for 10 minutes. Then, ethanol, water, and an ammonium polycarboxylic acid salt were added to the mixer at the mass ratios shown in Table 3 and further stirred for 20 minutes to obtain a slurry-like second glaze.
- the frit prepared above was selected according to the test number as shown in Table 4, and platinum fiber and a 1.5% by mass aqueous solution of CMC were added to the mixer at the mass ratio shown in Table 4 with respect to 100 parts by mass of the frit. And stirred for 10 minutes. Then, ethanol, water, and an ammonium polycarboxylic acid salt were added to the mixer at the mass ratios shown in Table 4 and further stirred for 20 minutes to obtain a slurry-like third glaze.
- Thermal conductivity test> A bowl-shaped test piece made of low carbon steel with a maximum diameter of 100 mm was prepared.
- the first glazes of Examples and Comparative Examples were spray-coated on the inner surface of the test piece and fired at 860 ° C. for 15 minutes once to obtain a ground coat layer having the thickness shown in Table 5. rice field.
- the second glazes of Examples and Comparative Examples were spray-coated on the ground coat layer and fired at 800 ° C. for 15 minutes three times to obtain an intermediate layer having the thickness shown in Table 5. (Excluding Comparative Examples 1, 2 and 4).
- the third glazes of Examples and Comparative Examples were spray-coated on the intermediate layer and fired at 800 ° C. for 15 minutes three times to cover the thickness shown in Table 5. A coat layer was obtained.
- Na elution test> A round bar made of low carbon steel having a diameter of 12 mm and a length of 80 mm was prepared. A glass lining layer composed of a ground coat layer, an intermediate layer, and a cover coat layer was formed on the surface of the round bar in the same process as the thermal conductivity test. The Na elution test was carried out by immersing the round bar with the glass lining layer thus obtained in 200 mL of ultrapure water (specific resistance: 18 M ⁇ ) at 50 ° C. in a PTFE container for 100 hours. After the test, the Na concentration in ultrapure water was determined by ICP analysis (inductively coupled plasma mass spectrometry) to determine the amount of Na eluted. The results are shown in Table 5 as the ratio when the Na elution amount in Comparative Example 1 is 100%.
- a glass lining layer composed of a ground coat layer, an intermediate layer, and a cover coat layer is applied to one of the main surfaces of a low carbon steel sheet having a square shape with a side of 100 mm and a thickness of 5 mm in the same process as the thermal conductivity test. Formed. With respect to the steel sheet with a glass lining layer thus obtained, an electrode (probe) was applied to the surface of the glass lining layer and the steel sheet using a battery-powered insulation resistance tester, and the electric resistance value was measured. The results are shown in Table 5.
- the glass lining layer of Example 1 composed of the ground coat layer, the intermediate layer, and the cover coat layer was formed.
- the mechanical impact property of the glass lining layer and the steel sheet and the state of blow defects accompanied by air bubbles were measured by a mechanical impact test of DIN-51155 standard. The results are shown in Table 6.
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Abstract
Description
ナトリウム成分の溶出量を抑制可能なグラスライニング製品は、ガラス中の気泡の存在や膜厚が厚くなることにより伝熱が悪く、熱交換を伴う用途においては生産性が低くなるという問題が生じる。また、ナトリウム成分の溶出量を抑制できたとしても静電気帯電を抑制することはできない。
静電気帯電を抑制可能なグラスライニング製品は、ガラス中の気泡の存在や膜厚が厚くなることにより伝熱が悪く、熱交換を伴う用途においては生産性が低くなるという問題が生じる。また、ナトリウム成分を嫌う分野では使用できない。
従って、複数の特性を併せ持つハイブリッド型のグラスライニング製品が得られることが望ましい。
金属基材の表面上に、
SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリット;並びに
珪石、アルミナ及び窒化アルミニウムからなる群から選択される1種又は2種以上の無機質耐火性粉体;
を含む第一釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~0.5mmのグランドコート層を形成する工程と、
グランドコート層の上に、SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリットを含有する第二釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.4~1.1mmの中間層を形成する工程と、
中間層の上に、Na2Oを含有せず、SiO2を主成分とし平均粒径が1.5~50μmのフリットを含有する第三釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~1.3mmのカバーコート層を形成する工程と、
を含むグラスライニング製品の製造方法。
[2]
第一釉薬、第二釉薬及び第三釉薬が共に金属繊維を含有する[1]に記載のグラスライニング製品の製造方法。
[3]
金属繊維がステンレス系金属繊維、貴金属系金属繊維、及び白金と白金族金属との合金繊維からなる群から選択される1種又は2種以上を含む[2]に記載のグラスライニング製品の製造方法。
[4]
第一釉薬は、第一釉薬中のフリット100質量部に対して直径0.1~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有し、
第二釉薬は、第二釉薬中のフリット100質量部に対して直径0.2~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有し、
第三釉薬は、第三釉薬中のフリット100質量部に対して直径0.2~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有する、
[2]又は[3]に記載のグラスライニング製品の製造方法。
[5]
金属基材の前記表面は、JIS B 0633:2001で測定される表面粗さRaが2~10μmである[1]~[4]の何れか一項に記載のグラスライニング製品の製造方法。
[6]
第一釉薬及び第二釉薬中のフリット中のNa2Oの含有量はそれぞれ8~22質量%である[1]~[5]の何れか一項に記載のグラスライニング製品の製造方法。
[7]
第三釉薬中のフリットの平均粒径は、第一釉薬中のフリットの平均粒径及び第二釉薬中のフリットの平均粒径よりも大きい[1]~[6]の何れか一項に記載のグラスライニング製品の製造方法。
[8]
第三釉薬中のフリットの平均粒径が10~50μmである[7]に記載のグラスライニング製品の製造方法。
[9]
第三釉薬中のフリットの平均粒径が1.5~20μmである[1]~[6]の何れか一項に記載のグラスライニング製品の製造方法。
[10]
グランドコート層、中間層及びカバーコート層の合計厚みが0.6~1.8mmである[1]~[9]の何れか一項に記載のグラスライニング製品の製造方法。
金属基材の表面上に、
SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリット;並びに
珪石、アルミナ及び窒化アルミニウムからなる群から選択される1種又は2種以上の無機質耐火性粉体;
を含む第一釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~0.5mmのグランドコート層を形成する工程と、
グランドコート層の上に、SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリットを含有する第二釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.4~1.1mmの中間層を形成する工程と、
中間層の上に、Na2Oを含有せず、SiO2を主成分とし平均粒径が1.5~50μmのフリットを含有する第三釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~1.3mmのカバーコート層を形成する工程と、
を含む。
グランドコート層は、金属基材の表面上に第一釉薬を施釉し、焼成することにより形成される。金属基材としては、限定的ではないが、低炭素鋼、ステンレス鋼等の鉄合金が例示される。金属基材の形状にも特に制限はないが、壁状、板状、翼状及び棒状等が挙げられる。
(A)SiO2+TiO2+ZrO2:41~72質量%
ただし、
SiO2:41~72質量%
TiO2:0~16質量%
ZrO2:0~10質量%
(B)R2O(RはNa、K又はLiを表す):8~22質量%
ただし、
Na2O:8~22質量%
K2O:0~16質量%
Li2O:0~10質量%
(C)R’O(R’はCa、Ba、Zn又はMgを表す):1~7質量%
ただし、
CaO:1~7質量%
BaO:0~6質量%
ZnO:0~6質量%
MgO:0~5質量%
(D)B2O3+Al2O3:1~18質量%
ただし、
B2O3:1~18質量%
Al2O3:0~6質量%
(E)CoO+NiO+MnO2+CeO2:0~6質量%
ただし、
CoO:0~6質量%
NiO:0~5質量%
MnO2:0~5質量%
CeO2:0~5質量%
中間層は、グランドコート層の上に第二釉薬を施釉し、焼成することにより形成される。
(A)SiO2+TiO2+ZrO2:41~72質量%
ただし、
SiO2:41~72質量%
TiO2:0~16質量%
ZrO2:0~10質量%
(B)R2O(RはNa、K又はLiを表す):8~22質量%
ただし、
Na2O:8~22質量%
K2O:0~16質量%
Li2O:0~10質量%
(C)R’O(R’はCa、Ba、Zn又はMgを表す):1~7質量%
ただし、
CaO:1~7質量%
BaO:0~6質量%
ZnO:0~6質量%
MgO:0~5質量%
(D)B2O3+Al2O3:1~18質量%
ただし、
B2O3:1~18質量%
Al2O3:0~6質量%
(E)CoO+NiO+MnO2+CeO2:0~6質量%
ただし、
CoO:0~6質量%
NiO:0~5質量%
MnO2:0~5質量%
CeO2:0~5質量%
カバーコート層は、中間層の上に第三釉薬を施釉し、焼成することにより形成される。
表1に記載する組成の原料配合物を1260℃で4時間加熱することにより溶融し、次いで、急冷することにより粗粉砕物を得た。得られた粗粉砕物を慣用のアルミナボールを用いたボールミルにて乾式粉砕し、得られた粉砕物を種々の条件で分級することにより、表1に記載の粒度分布をもつ各種のフリットを得た。粒度分布は、(株)セイシン企業製のレーザー回折粒度分布装置(型式:LMS-30)により測定される体積基準の累積粒度分布に基づいて求めた。
(実施例1~2、比較例1~3)
上記で作製したフリットを試験番号に応じて表2に示すように選択し、フリットの100質量部に対して、珪石(平均粒径20μm、粒径範囲0.1μm~100μm)及びCMC1.5質量%水溶液を表2に記載の質量割合(固形分換算)で混合機に投入し、5分間撹拌した。その後、エタノールを表2に記載の質量割合で混合機に投入し、更に20分間撹拌して、スラリー状の第一釉薬を得た。
上記で作製したフリットを試験番号に応じて表2に示すように選択し、フリット100質量部に対して、珪石、白金繊維及びCMC1.5質量%水溶液を表2に記載の質量割合で混合機に投入し、10分間撹拌した。その後、エタノール、水、及びポリカルボン酸アンモニウム塩を表2に記載の質量割合で混合機に投入し、更に20分間撹拌して、スラリー状の第一釉薬を得た。
低炭素鋼製の最大直径100mmのお椀状のテストピースを用意した。当該テストピースの内面に実施例及び比較例の各第一釉薬をスプレー塗布により施釉して860℃で15分間焼成する工程を1回行うことにより、表5に記載の厚みのグランドコート層を得た。次いで、実施例及び比較例の各第二釉薬をグランドコート層の上にスプレー塗布により施釉して800℃で15分間焼成する工程を3回実施することにより、表5に記載の厚みの中間層を得た(比較例1、2及び4を除く。)。次いで、実施例及び比較例の各第三釉薬を中間層の上にスプレー塗布により施釉して800℃で15分間焼成する工程を1~3回実施することにより、表5に記載の厚みのカバーコート層を得た。このようにして得られたグラスライニング層付きテストピースに水を200cc入れ、600Wのヒーターで加熱したときに、水温が20℃から80℃まで上昇するのに要する時間を測定した。結果は、比較例1における時間を100%としたときの比率として表5に示す。
直径12mm×長さ80mmの低炭素鋼製の丸棒を用意した。当該丸棒の表面に熱伝導性試験と同様の工程で、グランドコート層、中間層、及びカバーコート層で構成されるグラスライニング層を形成した。このようにして得られたグラスライニング層付き丸棒を、PTFE製の容器に入れた50℃の超純水(比抵抗:18MΩ)200mL中に100時間浸漬することでNa溶出試験を行った。試験後、超純水中のNa濃度をICP分析(誘導結合プラズマ質量分析)することで、Na溶出量を求めた。結果は、比較例1におけるNa溶出量を100%としたときの比率として表5に示す。
1辺が100mmの正方形状で厚みが5mmの低炭素鋼板の一方の主表面に熱伝導性試験と同様の工程で、グランドコート層、中間層、及びカバーコート層で構成されるグラスライニング層を形成した。このようにして得られたグラスライニング層付き鋼板について、電池式絶縁抵抗計を用いて、グラスライニング層表面と鋼板に電極(プローブ)を当て、電気抵抗値を測定した。結果を表5に示す。
1辺が100mmの正方形状で厚みが5mmの低炭素鋼板の一方の主表面に対して、サンドブラスト処理を行った。この際、サンドブラスト処理するときの研磨材(ブラウンアルミナ)の平均粒径を変化させることで種々の表面粗さをもつ低炭素鋼板を得た。サンドブラスト処理後の各低炭素鋼板の表面粗さRa及びRz(JIS B 0601:1994)を接触式のポータブル粗さ計(MITECHINSTRUMENT製/MDT310)でJIS B 0633:2001に準拠して測定した。結果を表6に示す。
11 金属基材
12 グランドコート層
13 中間層
14 カバーコート層
Claims (10)
- 金属基材の表面上に、
SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリット;並びに
珪石、アルミナ及び窒化アルミニウムからなる群から選択される1種又は2種以上の無機質耐火性粉体;
を含む第一釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~0.5mmのグランドコート層を形成する工程と、
グランドコート層の上に、SiO2を主成分としNa2Oを含有する、平均粒径が1.5~20μmのフリットを含有する第二釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.4~1.1mmの中間層を形成する工程と、
中間層の上に、Na2Oを含有せず、SiO2を主成分とし平均粒径が1.5~50μmのフリットを含有する第三釉薬を施釉し、焼成することにより、一層又は複数層で構成される厚み0.1~1.3mmのカバーコート層を形成する工程と、
を含むグラスライニング製品の製造方法。 - 第一釉薬、第二釉薬及び第三釉薬が共に金属繊維を含有する請求項1に記載のグラスライニング製品の製造方法。
- 金属繊維がステンレス系金属繊維、貴金属系金属繊維、及び白金と白金族金属との合金繊維からなる群から選択される1種又は2種以上を含む請求項2に記載のグラスライニング製品の製造方法。
- 第一釉薬は、第一釉薬中のフリット100質量部に対して直径0.1~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有し、
第二釉薬は、第二釉薬中のフリット100質量部に対して直径0.2~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有し、
第三釉薬は、第三釉薬中のフリット100質量部に対して直径0.2~2μm、長さ50~1000μmの金属繊維を0.01~5質量部含有する、
請求項2又は3に記載のグラスライニング製品の製造方法。 - 金属基材の前記表面は、JIS B 0633:2001で測定される表面粗さRaが2~10μmである請求項1~4の何れか一項に記載のグラスライニング製品の製造方法。
- 第一釉薬及び第二釉薬中のフリット中のNa2Oの含有量はそれぞれ8~22質量%である請求項1~5の何れか一項に記載のグラスライニング製品の製造方法。
- 第三釉薬中のフリットの平均粒径は、第一釉薬中のフリットの平均粒径及び第二釉薬中のフリットの平均粒径よりも大きい請求項1~6の何れか一項に記載のグラスライニング製品の製造方法。
- 第三釉薬中のフリットの平均粒径が10~50μmである請求項7に記載のグラスライニング製品の製造方法。
- 第三釉薬中のフリットの平均粒径が1.5~20μmである請求項1~6の何れか一項に記載のグラスライニング製品の製造方法。
- グランドコート層、中間層及びカバーコート層の合計厚みが0.6~1.8mmである請求項1~9の何れか一項に記載のグラスライニング製品の製造方法。
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- 2020-12-21 EP EP20918380.5A patent/EP4105356A4/en active Pending
- 2020-12-21 JP JP2022500249A patent/JP7225469B2/ja active Active
- 2020-12-21 KR KR1020227026240A patent/KR20220123066A/ko not_active Application Discontinuation
- 2020-12-21 CN CN202080094071.6A patent/CN115038813A/zh active Pending
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- 2022-07-12 US US17/862,575 patent/US20220340479A1/en active Pending
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EP4105356A1 (en) | 2022-12-21 |
US20220340479A1 (en) | 2022-10-27 |
JP7225469B2 (ja) | 2023-02-20 |
EP4105356A4 (en) | 2024-02-07 |
CN115038813A (zh) | 2022-09-09 |
KR20220123066A (ko) | 2022-09-05 |
JPWO2021161661A1 (ja) | 2021-08-19 |
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