JP6664650B2 - Manufacturing method of molded object - Google Patents
Manufacturing method of molded object Download PDFInfo
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- JP6664650B2 JP6664650B2 JP2016007443A JP2016007443A JP6664650B2 JP 6664650 B2 JP6664650 B2 JP 6664650B2 JP 2016007443 A JP2016007443 A JP 2016007443A JP 2016007443 A JP2016007443 A JP 2016007443A JP 6664650 B2 JP6664650 B2 JP 6664650B2
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- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000000843 powder Substances 0.000 claims description 170
- 239000011230 binding agent Substances 0.000 claims description 56
- 238000000465 moulding Methods 0.000 claims description 55
- 229920001169 thermoplastic Polymers 0.000 claims description 47
- 239000004416 thermosoftening plastic Substances 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 38
- 239000002994 raw material Substances 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 239000000919 ceramic Substances 0.000 claims description 15
- 239000012298 atmosphere Substances 0.000 claims description 9
- 230000004927 fusion Effects 0.000 claims description 9
- 230000009477 glass transition Effects 0.000 claims description 9
- 230000001678 irradiating effect Effects 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 45
- 238000009826 distribution Methods 0.000 description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 18
- 239000002904 solvent Substances 0.000 description 14
- 239000011362 coarse particle Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 12
- 239000000839 emulsion Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 235000021355 Stearic acid Nutrition 0.000 description 9
- 125000004432 carbon atom Chemical group C* 0.000 description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 239000008117 stearic acid Substances 0.000 description 9
- 235000014113 dietary fatty acids Nutrition 0.000 description 8
- 239000000194 fatty acid Substances 0.000 description 8
- 229930195729 fatty acid Natural products 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 150000004665 fatty acids Chemical class 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- -1 sialon Chemical compound 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 229920001187 thermosetting polymer Polymers 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000019271 petrolatum Nutrition 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000007580 dry-mixing Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011361 granulated particle Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000004200 microcrystalline wax Substances 0.000 description 2
- 235000019808 microcrystalline wax Nutrition 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000012169 petroleum derived wax Substances 0.000 description 2
- 235000019381 petroleum wax Nutrition 0.000 description 2
- 150000004671 saturated fatty acids Chemical group 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 239000004264 Petrolatum Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 229910026551 ZrC Inorganic materials 0.000 description 1
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- SJKRCWUQJZIWQB-UHFFFAOYSA-N azane;chromium Chemical compound N.[Cr] SJKRCWUQJZIWQB-UHFFFAOYSA-N 0.000 description 1
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000002181 crystalline organic material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 235000019809 paraffin wax Nutrition 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 229940066842 petrolatum Drugs 0.000 description 1
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- 239000011802 pulverized particle Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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- 230000004580 weight loss Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Description
本発明は、粉末床溶融結合法を用いた造形物の製造方法に関する。 The present invention relates to a method for manufacturing a shaped article using a powder bed fusion bonding method.
近年、複雑な形状を有するセラミックス部材、モデル品、或いは少量多品種のセラミックス部材の製造方法として、粉末床溶融結合法が注目されている。粉末床溶融結合法とは、原料として粉末を用いた積層造形法であり、造形用粉末を厚さ数十〜数百μｍの粉末層を形成させる粉末層形成工程と、こうして形成された粉末層に対して三次元造形物の断面形状にレーザーや電子ビーム等を照射することで選択的に加熱し、溶融固化または焼結させる断面形状形成行程と、を繰り返して積層することにより、三次元造形物を作製する方法である。 2. Description of the Related Art In recent years, a powder bed fusion bonding method has attracted attention as a method for manufacturing ceramic members having complicated shapes, model products, or ceramic members of various types in small quantities. The powder bed fusion bonding method is a layered molding method using powder as a raw material, and a powder layer forming step of forming a powder layer having a thickness of several tens to several hundreds μm of the molding powder, and a powder layer thus formed. By selectively irradiating the cross-sectional shape of the three-dimensional object with a laser, an electron beam, or the like, and melting and solidifying or sintering the cross-sectional shape forming process. This is a method of manufacturing a product.
しかし、セラミックスや金属は、樹脂に比べて融点が高いことから、これら材料自身を溶融固化または焼結により造形物を作製することは困難である。また、セラミックスや一部の金属については、塑性変形し難く、熱応力が大きいため、溶融固化または焼結することができても、造形物に割れやクラック等が生じ易くなり、良好な造形物を得ることは困難である。このため、これらのセラミックスや金属の粉末積層造形においては、まずはバインダーを含んだ原料粉末を積層し、バインダーをレーザー等で固化することにより成形体を作製した後、焼結を行うことが行われている。 However, since ceramics and metals have a higher melting point than resins, it is difficult to produce a shaped article by melting and solidifying or sintering these materials themselves. In addition, ceramics and some metals are difficult to plastically deform and have high thermal stress, so even if they can be melted and solidified or sintered, cracks and cracks are likely to occur in the molded product, and a good molded product It is difficult to get. Therefore, in the powder additive manufacturing of these ceramics and metals, first, a raw material powder containing a binder is laminated, and the binder is solidified by a laser or the like to form a compact, and then sintering is performed. ing.
例えば、特許文献１には、熱可塑性樹脂を含む、平均粒子径が1〜１００μｍの球状の粉末焼結積層造形法に使用される微小球体であって、微小球体の表面の一部又は全部が凝集防止粒子で被覆されていることで、滑り性もしくは流動性に優れ、かつ高い充填率が達成可能な粉末焼結積層造形に適した微小球体について記載されている。 For example, Patent Literature 1 discloses a microsphere used in a powder-sintering lamination molding method including a thermoplastic resin and having an average particle diameter of 1 to 100 μm, and part or all of the surface of the microsphere is included. It describes a microsphere suitable for powder sintering additive manufacturing, which is coated with anti-agglomeration particles, has excellent slipperiness or fluidity, and can achieve a high filling rate.
また、特許文献２には、合成樹脂粉末３０〜９０重量％と無機充填剤１０〜７０重量％からなる材料を粉末層に展開し、レーザー光を照射して照射部位を溶融、固化させる。材料の粉末層展開とレーザー光照射による溶融固化を繰り返し行うことで三次元的モデルを作製することが記載されている。 Further, in Patent Document 2, a material composed of 30 to 90% by weight of a synthetic resin powder and 10 to 70% by weight of an inorganic filler is spread on a powder layer, and irradiated with laser light to melt and solidify an irradiated portion. It is described that a three-dimensional model is produced by repeatedly performing powder layer development of a material and melting and solidification by laser light irradiation.
さらに、特許文献３には、砂粒子表面が熱硬化性樹脂成分にて被覆されたレジンコーテッドサンドを粉末層に形成し、レーザー光を照射して所要の２次元パターンの硬化層を形成する工程とを繰り返すことにより３次元造形物を得る方法が記載されている。この方法によれば、粉末層に形成されたレジンコーテッドサンドを予熱しておかなくても、レーザー光を照射すれば硬化剤が樹脂を架橋して熱硬化性樹脂となるため、そのまま所定の２次元パターン硬化させることができる。 Further, Patent Document 3 discloses a process of forming a resin-coated sand having a surface of sand particles coated with a thermosetting resin component in a powder layer, and irradiating a laser beam to form a cured layer having a required two-dimensional pattern. And a method of obtaining a three-dimensional structure by repeating the above. According to this method, even if the resin-coated sand formed on the powder layer is not preheated, the curing agent crosslinks the resin and becomes a thermosetting resin when irradiated with a laser beam. The dimensional pattern can be cured.
しかし、上記の従来のセラミックスや金属の粉末を原料とする粉末床溶融結合法では、粉末層に対してレーザー等で加熱した場合、急激な温度変化により造形物に反りやクラックが生じるという問題があった。この問題を解決するため、レーザー等を照射する前に粉末層を融点付近まで予熱しておくことが行われていた。しかしながら、粉末層を予熱するためには、装置内部全体を加熱する必要があるため、多くの時間とエネルギーを必要とするため、生産速度の低下やコスト増を招くという不具合を生じることになる。
また、上記特許文献３に記載の、硬化剤及び樹脂を含有する造形用粉末を用いた造形物の製造方法では、レーザー光の照射時に、熱硬化反応に伴うガスが発生し、造形物内部に欠陥が生じるという問題があった。
本発明は、上記従来の実情に鑑みてなされたものであって、粉末床溶融結合法において、粉末層を予熱することなく造形物を作成することが可能であって、レーザー光照射時にガスの発生による造形物内部に欠陥が生じない造形物の製造方法を提供することを課題とする。
However, in the conventional powder bed fusion bonding method using a ceramic or metal powder as a raw material, when a powder layer is heated by a laser or the like, a problem occurs in that a rapid change in temperature causes warpage or cracks in a formed object. there were. In order to solve this problem, it has been practiced to preheat the powder layer to near the melting point before irradiating with a laser or the like. However, in order to preheat the powder layer, it is necessary to heat the entire inside of the apparatus, which requires a lot of time and energy, resulting in a problem that the production speed is reduced and the cost is increased.
Further, in the method for manufacturing a molded article using a molding powder containing a curing agent and a resin described in Patent Document 3, a gas accompanying a thermosetting reaction is generated at the time of irradiation with laser light, and the gas is generated inside the molded article. There is a problem that defects occur.
The present invention has been made in view of the above-described conventional circumstances, and in a powder bed fusion bonding method, it is possible to form a shaped article without preheating a powder layer, and to generate a gas during laser beam irradiation. An object of the present invention is to provide a method for manufacturing a modeled object in which a defect is not generated inside the modeled object due to occurrence.
本発明の造形物の製造方法は、粉末床溶融結合法を用いた造形物の製造方法であって、融点又はガラス転移点が２０℃以上１３０℃以下である熱可塑性バインダーと、セラミックス及び／又は金属の原料粉末と、を混合して造形用粉末とする造形用粉末調製工程と、前記造形用粉末を造形ステージ上に予熱を行うことなく粉末層を形成する粉末層形成工程と、前記粉末層にレーザー光を照射して所定のパターン形状に固化させる照射工程と、を繰り返すことによって造形物を得ることを特徴とする。 The method for producing a shaped article of the present invention is a method for producing a shaped article using a powder bed fusion bonding method, wherein a thermoplastic binder having a melting point or a glass transition point of 20 ° C or more and 130 ° C or less, ceramics and / or A molding powder preparation step of mixing a metal raw material powder with a molding powder to form a molding powder; a powder layer forming step of forming a powder layer without preheating the molding powder on a molding stage; and And an irradiation step of irradiating the substrate with a laser beam to solidify it into a predetermined pattern shape.
本発明の造形物の製造方法では、まず造形用粉末調製工程として、熱可塑性バインダーと、セラミックス及び／又は金属の原料粉末とを混合して造形用粉末とする。そして、粉末層形成工程として、造形用粉末を造形ステージ上に予熱を行うことなく粉末層を形成する。さらに、照射工程として、粉末層にレーザー光を照射して所定のパターン形状に固化させる。ここで、粉末層を構成している造形用粉末に混合されている熱可塑性バインダーとしては、融点又はガラス転移点が２０℃以上１３０℃以下の範囲という低い温度のものを用いるため、粉末層にレーザー光を照射してバインダーを溶融するのに、それほど急激な温度変化は生じず、造形物に反りやクラックが生じるおそれが少ない。このため、粉末層をレーザー等を照射する前に予熱しておく必要がなく、多くの時間とエネルギーを必要とすることもないことから、ひいては、生産速度の向上と製造コストの低廉化を実現できる。
なお、ここで熱可塑性バインダーとは、加熱によって硬化する熱硬化性バインダーを含まない意であり、架橋反応を行うための硬化剤も含まれていないものをいう。このため、硬化剤を含有する熱硬化性バインダーと異なり、レーザー光照射時にガスが発生することはなく、ガス発生による造形物内部に欠陥が生じない。
In the method for producing a molded article according to the present invention, first, as a molding powder preparation step, a thermoplastic binder and a ceramic and / or metal raw material powder are mixed to form a molding powder. Then, as a powder layer forming step, a powder layer is formed without preheating the forming powder on the forming stage. Further, as an irradiation step, the powder layer is irradiated with laser light to be solidified into a predetermined pattern shape. Here, as the thermoplastic binder mixed with the molding powder constituting the powder layer, a material having a low melting point or a glass transition point of 20 ° C. or more and 130 ° C. or less is used. When the binder is melted by irradiating the laser beam, the temperature does not change so sharply, and the molded article is less likely to warp or crack. Therefore, it is not necessary to preheat the powder layer before irradiating it with a laser, etc., and it does not require much time and energy, thereby improving the production speed and reducing the production cost. it can.
Here, the thermoplastic binder means that it does not include a thermosetting binder which is cured by heating and does not include a curing agent for performing a crosslinking reaction. For this reason, unlike a thermosetting binder containing a curing agent, no gas is generated at the time of laser beam irradiation, and no defect occurs inside the molded article due to gas generation.
セラミックス及び／又は金属としては、金属酸化物、金属非酸化物、及び金属の少なくとも１種類を用いることができる。 As the ceramic and / or metal, at least one of a metal oxide, a metal non-oxide, and a metal can be used.
また、固化工程は大気雰囲気又は不活性ガス雰囲気で行うことができる。固化工程を不活性ガス雰囲気で行えば、酸素と反応し易いセラミックスや金属を用いる場合に、化学変化が生じないため好適である。不活性ガスとしてはアルゴン、ヘリウム、窒素等を用いることができる。 The solidification step can be performed in an air atmosphere or an inert gas atmosphere. It is preferable to carry out the solidification step in an inert gas atmosphere because no chemical change occurs when ceramics or metals that react easily with oxygen are used. As the inert gas, argon, helium, nitrogen or the like can be used.
本発明の造形物の製造方法によれば、粉末層を予熱することなく造形物を作成することができ、レーザー光照射時にガスの発生による造形物内部に欠陥が生じない造形物を製造することができる。 According to the method for manufacturing a shaped object of the present invention, a shaped object can be created without preheating the powder layer, and a shaped object that does not cause defects inside the shaped object due to generation of gas at the time of laser light irradiation can be manufactured. Can be.
以下、本発明を具体化した実施形態について説明する。
（造形用粉末調整工程）
本発明の造形物の製造方法に用いられる造形用粉末の原料となるセラミックスとしては、特に限定はなく、例えば、金属酸化物、金属窒化物、金属炭化物、複合酸化物等が挙げられる。これらは、単独でもよいし、二種以上を併用してもよい。また、本発明の造形用粉末の原料となる金属としてはシリコン、アルミニウム、鉄、ステンレス、チタン、タングステン等が挙げられる。
Hereinafter, embodiments embodying the present invention will be described.
(Modeling powder adjustment process)
The ceramic used as the raw material of the molding powder used in the method for producing a molded article of the present invention is not particularly limited, and examples thereof include metal oxides, metal nitrides, metal carbides, and composite oxides. These may be used alone or in combination of two or more. Examples of the metal which is a raw material of the molding powder of the present invention include silicon, aluminum, iron, stainless steel, titanium, and tungsten.
金属酸化物としては特に限定されないが、例えば、酸化アルミニウム、酸化マグネシウム、酸化ケイ素、酸化カルシウム、酸化チタン、酸化バナジウム、酸化クロム、酸化マンガン、酸化鉄、酸化コバルト、酸化銅、酸化亜鉛、酸化イットリウム、酸化ジルコニウム、酸化ニオブ、酸化モリブデン、酸化タンタル、酸化タングステン、アパタイトなどが挙げられる。
また、金属窒化物としては特に限定されないが、例えば、窒化アルミニウム、窒化ケイ素、窒化ホウ素、窒化チタン、窒化バナジウム、窒化クロム、窒化ジルコニウム、窒化ニオブ、窒化タンタルなどが挙げられ、
さらに、金属炭化物としては特に限定されないが、例えば、炭化ケイ素、炭化チタン、炭化バナジウム、炭化ジルコニウム、炭化ニオブ、炭化モリブデン、炭化タンタル、炭化タングステンなどが挙げられる。
また、複合酸化物としては特に限定されないが、例えば、コージェライト、ムライト、サイアロン、チタン酸バリウム、チタン酸ストロンチウムなどが挙げられる。
The metal oxide is not particularly limited, for example, aluminum oxide, magnesium oxide, silicon oxide, calcium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, iron oxide, cobalt oxide, copper oxide, zinc oxide, yttrium oxide , Zirconium oxide, niobium oxide, molybdenum oxide, tantalum oxide, tungsten oxide, apatite, and the like.
Further, the metal nitride is not particularly limited, for example, aluminum nitride, silicon nitride, boron nitride, titanium nitride, vanadium nitride, chromium nitride, zirconium nitride, niobium nitride, tantalum nitride, and the like,
Further, the metal carbide is not particularly limited, and examples thereof include silicon carbide, titanium carbide, vanadium carbide, zirconium carbide, niobium carbide, molybdenum carbide, tantalum carbide, and tungsten carbide.
The composite oxide is not particularly limited, and examples thereof include cordierite, mullite, sialon, barium titanate, and strontium titanate.
また、造形用粉末に添加されるバインダーとしては、加熱によって溶融あるいは軟化するものであって、融点あるいはガラス転移点が２０℃以上１３０℃以下であるものであれば、融点を有する結晶性の有機化合物やガラス転移点を有する非結晶性の有機化合物等を用いることができる。融点あるいはガラス転移点が２０℃以上１３０℃以下であるものであれば、粉末層形成工程において形成された粉末層に対し、レーザーや電子ビーム等を照射することによって、容易に溶解、固化して造形物を形成することができるため、予熱を行う必要がない。 In addition, as a binder added to the molding powder, a binder that melts or softens when heated and has a melting point or a glass transition point of 20 ° C. or more and 130 ° C. or less is a crystalline organic material having a melting point. A compound, a non-crystalline organic compound having a glass transition point, or the like can be used. If the melting point or the glass transition point is 20 ° C. or more and 130 ° C. or less, the powder layer formed in the powder layer forming step is easily melted and solidified by irradiating a laser or an electron beam or the like. Since a model can be formed, it is not necessary to perform preheating.
熱可塑性バインダーは、結晶質であるか、非晶質であるかを問わず、石油ワックス、脂肪酸、脂肪酸エステル、及び脂肪酸アミドからなる群より選ばれた少なくとも１種類を用いることができる。
石油ワックスとしては、日本工業規格 (JIS K2235) によって規定されている、パラフィンワックス、マイクロクリスタリンワックス、ペトロラタムのいずれも用いることができる。好適には炭素鎖が直鎖構造を持った飽和脂肪族炭化水素で、かつ炭素原子数が１８以上３５以下のものが好ましく、炭素原子数が２０以上３０以下のものはさらに好ましい。
また、脂肪酸としては、炭素鎖の形状、炭素原子数、炭素鎖の結合状態（飽和もしくは不飽和）によって特に限定されるものではないが、好適には炭素鎖が直鎖構造を持った飽和脂肪酸で、かつ炭素原子数が１０以上２５以下のものが好ましく、１５以上２０以下のものがさらに好ましい。
さらに、脂肪酸エステルとしては、脂肪酸とアルコールの炭素鎖の形状、炭素原子数、炭素鎖の結合状態（飽和もしくは不飽和）によって特に限定されるものではないが、好適には炭素鎖が直鎖構造をもった飽和脂肪酸エステルで、かつ炭素原子数が、１０以上２５以下のものが好ましく、１５以上２０以下のものはさらに好ましい、
また、脂肪酸アミドとしては、脂肪酸の炭素鎖の形状、炭素原子数、炭素鎖の結合状態（飽和もしくは不飽和）によって特に限定されるものではないが、好適には炭素鎖が直鎖構造を持った飽和脂肪酸アミドであり、かつ炭素原子数が、１０以上２５以下のものが好ましく、１５以上２０以下のものがさらに好ましい、
さらに、ポリビニルアセタールとしては、ポリビニルブチラールが挙げられる。ポりビニルブチラールとしては、分子量が１．０×１０４以上２０.０×１０４であり、１．５×１０４以上１０.０×１０４のものが好ましい。
Regardless of whether the thermoplastic binder is crystalline or amorphous, at least one selected from the group consisting of petroleum wax, fatty acids, fatty acid esters, and fatty acid amides can be used.
As the petroleum wax, any of paraffin wax, microcrystalline wax, and petrolatum specified by Japanese Industrial Standards (JIS K2235) can be used. Preferably, the carbon chain is a saturated aliphatic hydrocarbon having a straight-chain structure and has 18 to 35 carbon atoms, and more preferably 20 to 30 carbon atoms.
The fatty acid is not particularly limited by the shape of the carbon chain, the number of carbon atoms, and the bonding state of the carbon chain (saturated or unsaturated), but is preferably a saturated fatty acid having a straight-chain carbon chain. And those having 10 to 25 carbon atoms are preferable, and those having 15 to 20 carbon atoms are more preferable.
Further, the fatty acid ester is not particularly limited by the shape of the carbon chain of the fatty acid and the alcohol, the number of carbon atoms, and the bonding state (saturated or unsaturated) of the carbon chain, but preferably the carbon chain has a linear structure. Is preferably a saturated fatty acid ester having a carbon atom number of 10 or more and 25 or less, more preferably 15 or more and 20 or less.
The fatty acid amide is not particularly limited by the shape of the carbon chain of the fatty acid, the number of carbon atoms, or the bonding state of the carbon chain (saturated or unsaturated), but preferably the carbon chain has a linear structure. Is preferably a saturated fatty acid amide having 10 to 25 carbon atoms, and more preferably 15 to 20 carbon atoms.
Further, as polyvinyl acetal, polyvinyl butyral may be mentioned. Polyvinyl butyral has a molecular weight of 1.0 × 10 4 or more and 20.0 × 10 4 , preferably 1.5 × 10 4 or more and 10.0 × 10 4 .
また、熱可塑性バインダーの融点又はガラス転移点は、２０℃未満ではハンドリング時に熱可塑性バインダーの融解が容易に始まるために用いることができず、１３０℃を超えると造形時に予熱を必要とするため、２０℃以上１３０℃以下の範囲にあることが必要である。好ましくは３０℃以上１２０℃以下であり、さらに好ましいのは４０℃以上１１０℃以下である。また、熱可塑性バインダーは２種類以上を混合して用いてもよく、結晶質の熱可塑性バインダーと非晶質の熱可塑性バインダーとを混合して用いてもよい。 Further, the melting point or glass transition point of the thermoplastic binder, if less than 20 ℃, can not be used to easily start melting of the thermoplastic binder at the time of handling, if it exceeds 130 ℃, requires preheating at the time of molding, It is necessary to be in the range of 20 ° C. or more and 130 ° C. or less. Preferably it is 30 to 120 degreeC, More preferably, it is 40 to 110 degreeC. Further, two or more kinds of thermoplastic binders may be used as a mixture, or a crystalline thermoplastic binder and an amorphous thermoplastic binder may be used as a mixture.
さらに、造形用粉末のＨａｕｓｎｅｒ比は１．１０以上１．４０以下であることが好ましく、１．１０以上１．３０以下であることがさらに好ましく、１．１１以上１．２０以下であることが最も好ましい。Ｈａｕｓｎｅｒ比が１．１０未満であると造形用粉末の流動性が優れることから、粉末層形成時の層の乱れが生じやすくなる。また、Ｈａｕｓｎｅｒ比が１．４０を超えると造形用粉末の流動性が悪くなり、やはり粉末層形成時の層の乱れが生じやすくなる。
Ｈａｕｓｎｅｒ比とは、造形用粉末の静かさ密度とタップ密度の値を、下記の式（１）を用いて計算した値をいう。ここで、かさ密度とは、造形用粉末を静かに容器に入れたときの粉末の密度であり、ＪＩＳ−Ｒ１６２８に準じて測定した値をいう。
また、タップ密度とは、造形用粉末を容器に入れた後，容器にタップによる衝撃を加え，体積変化がなくなったときの粉末の密度を指し、ＪＩＳ−Ｋ５１０１に準じて、タップ回数は２００回とした場合の値をいう。
The Hausner ratio refers to a value obtained by calculating the values of the quiet density and the tap density of the molding powder using the following equation (1). Here, the bulk density is the density of the powder when the molding powder is gently placed in a container, and refers to a value measured according to JIS-R1628.
In addition, the tap density refers to the density of the powder when the volume change is eliminated after the shaping powder is put into a container and the container is subjected to an impact by tapping, and the number of taps is 200 times according to JIS-K5101. Means the value when
また、造形用粉末は、単一もしくは複数の粒度分布ピークが１０μｍ以上５００μｍ以下の範囲にあることが好ましく、さらに好ましいのは２０μｍ以上３００μｍ以下であり、最も好ましいのは３０μｍ以上１００μｍ以下である。造形用粉末の粒度分布ピークが１０μｍ以上であれば流動性に優れ、粉末層形成における精度が向上する。また、造形用粉末の粒度分布ピークが５００μｍ以下であれば、作製した造形物の強度に優れたものとなる。なお、造形用粉末の粒度分布は、測定方法が特に限定されるものではないが、例えば、乾式のレーザー回折・散乱式粒度分布計や写真撮影と画像解析による分布測定により測定することができる。 The modeling powder preferably has a single or plural particle size distribution peaks in a range of 10 μm to 500 μm, more preferably 20 μm to 300 μm, and most preferably 30 μm to 100 μm. When the particle size distribution peak of the molding powder is 10 μm or more, the fluidity is excellent, and the accuracy in forming the powder layer is improved. If the particle size distribution peak of the molding powder is 500 μm or less, the produced molded article has excellent strength. The particle size distribution of the molding powder is not particularly limited in the measuring method, but can be measured by, for example, a dry laser diffraction / scattering type particle size distribution meter or a distribution measurement by photographing and image analysis.
また、熱可塑性バインダーの体積をセラミックス及び／又は金属の原料粉末の表面積で除した値は、０.０３μｍ以上３．００μｍ以下が好ましく、さらに好ましいのは０．０４μｍ以上１．００μｍ以下である。熱可塑性バインダーの体積を原料粉末の表面積で除した値が０．０３μｍ未満では、加熱による造形用粉末の固化体の強度が小さくなる。また、３．００μｍを超える場合、熱可塑性バインダーの含有量が多すぎて加熱時の熱可塑性バインダー溶融により造形物の寸法精度が低下するおそれがある。なお、原料粉末の表面積は、測定方法が特に限定されるものではないが、例えば、ガス吸着法を用いた表面積分析装置により比表面積を測定したのち、式（２）を用いて計算することができる。
造形用粉末は、セラミックス及び／又は金属の原料粉末と熱可塑性バインダーとを混合することによって製造することができる。混合方法としては、乾式法（原料粉末と熱可塑性バインダーを乾式で混合する方法）及び湿式法（原料粉末と熱可塑性バインダーを湿式溶媒中に分散し、あるいは、溶解した熱可塑性バインダーを原料粉末と混ぜた後に、溶媒を取り除き、熱可塑性バインダーを原料粉末の粒子表面に固定化させる方法で混合する方法）のいずれの方法も用いることができる。乾式混合の方法ではボールミルやＶ型混合機を用いた混合方法などが挙げられ、湿式混合ではバインダーを分散させた溶液と原料粉末と混ぜ合わせた後に、加熱噴霧・乾燥させるスプレードライ法や、溶媒に溶かしたバインダーを加熱減圧下で溶媒を取り除き混合させる方法などが挙げられる。なお、湿式法で混合した場合においいて、溶媒中に分散した熱可塑性バインダーを用いた場合、原料粉末と混合後に溶媒を熱可塑性バインダーの融点よりも低い温度で取り除くことで熱可塑性バインダーが分散粒子状態で原料粉末の粒子表面に吸着され、分散した熱可塑性バインダーの融点よりも高い温度で溶媒を取り除く、もしくは溶媒に溶解した熱可塑性バインダーを用いた場合、熱可塑性バインダーが原料粉末の粒子表面に膜状に吸着される。 The molding powder can be produced by mixing a ceramic and / or metal raw material powder and a thermoplastic binder. The mixing method includes a dry method (a method of mixing the raw material powder and the thermoplastic binder in a dry manner) and a wet method (a method in which the raw material powder and the thermoplastic binder are dispersed in a wet solvent, or in which the dissolved thermoplastic binder is mixed with the raw material powder). After the mixing, the solvent is removed, and the thermoplastic binder is fixed to the particle surface of the raw material powder by mixing. Examples of the dry mixing method include a mixing method using a ball mill or a V-type mixer. In the case of wet mixing, a solution in which a binder is dispersed is mixed with a raw material powder, and then a spray drying method in which heating is sprayed and dried, or a solvent is used. And a method in which the solvent dissolved in the binder is removed under heating and reduced pressure to remove the solvent. In the case of mixing by a wet method, when a thermoplastic binder dispersed in a solvent is used, the solvent is removed at a temperature lower than the melting point of the thermoplastic binder after mixing with the raw material powder, so that the thermoplastic binder is dispersed particles. In a state, the solvent is removed at a temperature higher than the melting point of the dispersed thermoplastic binder, or the thermoplastic binder is applied to the particle surface of the raw material powder when the thermoplastic binder dissolved in the solvent is used. Adsorbed in film form.
（粉末層形成工程）
本発明の造形物の製造方法における粉末層形成工程としては、ブレード等を移動させて粉末を粉末層に展開する方法や、回転するローラーを移動させて粉末を粉末層に展開する方法、逆回転のローラーを移動させて粉末を粉末層に展開する方法などが挙げられる。
(Powder layer forming step)
As the powder layer forming step in the manufacturing method of the molded article of the present invention, a method of moving the blade or the like to spread the powder on the powder layer, a method of moving the rotating roller to spread the powder on the powder layer, a reverse rotation And developing the powder into a powder layer by moving the roller.
（照射工程）
照射工程において、粉末層に照射するためのレーザーとしては、例えばＣＯ２レーザー、ファイバーレーザー、ＹＡＧレーザー、エキシマレーザー、Ｈｅ−Ｃｄレーザー、半導体励起固体レーザーなどを挙げることができる。この中で、ＣＯ２レーザーは、簡易に制御でき、特に好適に用いることができる。これらのレーザーは、１種を単独で用いることができ、あるいは、２種以上を組み合わせて用いることができる。
また、レーザー光照射時の雰囲気としては、例えばヘリウム、窒素、アルゴンなどのガス中、あるいは大気中においても実施できる。雰囲気を不活性ガスとすることで、造形用粉末の酸化や腐食を防止するとともに、レーザー光照射による造形物の過熱による変形を防止することができる。
(Irradiation process)
In the irradiation step, examples of a laser for irradiating the powder layer include a CO 2 laser, a fiber laser, a YAG laser, an excimer laser, a He—Cd laser, and a semiconductor-excited solid laser. Among them, the CO 2 laser can be easily controlled and can be particularly preferably used. One of these lasers can be used alone, or two or more can be used in combination.
The laser beam irradiation may be performed in a gas such as helium, nitrogen, or argon, or in the atmosphere. By using an inert gas as the atmosphere, it is possible to prevent the molding powder from being oxidized and corroded, and to prevent deformation of the molded article due to overheating due to laser beam irradiation.
[実施例１]
アルミナ粗粒粉(粒度分布ピーク４１μｍ)１００重量部に対してステアリン酸１５重量部を温エタノール（５０℃）に溶解させ、アルミナ粗粒粉と混合した。加熱減圧下でエタノールを取り除き、粉砕した。１００μｍのふるいを通して粗大な粒子を取り除き、実施例１の造形用粉末を得た。
[Example 1]
15 parts by weight of stearic acid was dissolved in 100 parts by weight of alumina coarse powder (particle size distribution peak 41 μm) in warm ethanol (50 ° C.) and mixed with alumina coarse powder. The ethanol was removed under heating and reduced pressure, and pulverized. Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Example 1.
[実施例２]
アルミナ粗粒粉(粒度分布ピーク４１μｍ)１００重量部に対してステアリン酸エマルジョン（固形成分３０重量％、溶媒：水）中の固形成分が２０重量部になるよう、アルミナ粗粒粉とステアリン酸エマルジョンを混合した。混合水溶液を室温で乾燥させ粉砕した。１００μｍのふるいを通して粗大な粒子を取り除き、実施例２の造形用粉末を得た。
[Example 2]
Alumina coarse powder and stearic acid emulsion such that the solid component in the stearic acid emulsion (solid component 30% by weight, solvent: water) is 20 parts by weight with respect to 100 parts by weight of the alumina coarse powder (particle size distribution peak 41 μm). Was mixed. The mixed aqueous solution was dried at room temperature and pulverized. Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Example 2.
[実施例３〜実施例１１]
アルミナ粗粒粉(粒度分布ピーク３１μｍ)１００重量部に対してステアリン酸粗粒粉（粒度分布ピーク１２５μｍ）１５重量部をＶ型混合機（ＶＭ−２：筒井理化学器機株式会社製）にて混合した。２５０μｍのふるいを通して粗大な粒子を取り除き、実施例３の造形用粉末を得た。
また、実施例４では熱可塑性バインダーとしてポリビニルブチラール粗粒粉（粒度分布ピーク５５μｍ）を用い、実施例５ではベヘニル酸エステル粗粒粉（粒度分布ピーク７６μｍ）を用い、その他の条件は実施例３と同様にして造形用粉末を得た。
さらに、実施例６シリコン粗粒粉(粒度分布ピーク２３μｍ)、実施例７ではシリカ粗粒粉(粒度分布ピーク４６μｍ)、実施例８ではムライト粗粒粉(粒度分布ピーク１５μｍ)、実施例９ではジルコニア粗粒粉(粒度分布ピーク２８μｍ)、実施例１０では炭化ケイ素粗粒粉(粒度分布ピーク２６μｍ)、実施例１１では炭化ケイ素粗粒粉(粒度分布ピーク４３μｍ)、を用い、その他の条件は実施例３と同様にして造形用粉末を得た。
[Examples 3 to 11]
15 parts by weight of stearic acid coarse particle powder (particle size distribution peak 125 μm) is mixed with 100 parts by weight of alumina coarse particle powder (particle size distribution peak 31 μm) using a V-type mixer (VM-2: manufactured by Tsutsui Rikakiki Co., Ltd.) did. Coarse particles were removed through a 250 μm sieve to obtain a molding powder of Example 3.
Further, in Example 4, polyvinyl butyral coarse powder (particle size distribution peak 55 μm) was used as the thermoplastic binder, in Example 5, behenyl ester coarse powder (particle size distribution peak 76 μm) was used, and other conditions were the same as those in Example 3. In the same manner as in the above, a molding powder was obtained.
Further, in Example 6, silicon coarse powder (particle size distribution peak 23 μm), in Example 7, silica coarse powder (particle size distribution peak 46 μm), in Example 8, mullite coarse powder (particle size distribution peak 15 μm), and in Example 9, Using zirconia coarse powder (particle size distribution peak 28 μm), silicon carbide coarse powder (particle size distribution peak 26 μm) in Example 10, and silicon carbide coarse powder (particle size distribution peak 43 μm) in Example 11, A molding powder was obtained in the same manner as in Example 3.
［実施例１２〜実施例１５］
アルミナ微粒粉(粒度分布ピーク０．５μｍ)１００重量部に対して分散剤（Ａ６１１４、東亜合成株式会社製）1重量部、水２５重量部を加え、各種熱可塑性バインダーの水系エマルジョン（実施例１２ではマイクロクリスタリンワックスのエマルジョン、実施例１３ではステアリン酸のエマルジョン、実施例１４ではパラフィンワックスのエマルジョン、実施１５ではステアリン酸アミドのエマルジョン）をアルミナ微粒粉１００重量部に対して熱可塑性バインダー固形成分が２０重量部になるように混合した。混合水溶液をスプレードライ装置（スプレードライヤＡＤＬ３１１Ｓ：ヤマト科学株式会社製）にて造粒粒子径が約３０μｍになるように調製して造粒した。１００μｍのふるいを通して粗大な粒子を取り除き、実施例１２〜実施例１５の造形用粉末を得た。
[Examples 12 to 15]
1 part by weight of a dispersant (A6114, manufactured by Toagosei Co., Ltd.) and 25 parts by weight of water were added to 100 parts by weight of alumina fine powder (particle size distribution peak: 0.5 μm), and an aqueous emulsion of various thermoplastic binders (Example 12) In Example 13, an emulsion of microcrystalline wax, an emulsion of stearic acid in Example 13, an emulsion of paraffin wax in Example 14, and an emulsion of stearic acid amide in Example 15) were used. The mixture was mixed to 20 parts by weight. The mixed aqueous solution was prepared and granulated with a spray dryer (spray dryer ADL311S: manufactured by Yamato Scientific Co., Ltd.) so that the granulated particle diameter became about 30 μm. Coarse particles were removed through a 100 μm sieve to obtain molding powders of Examples 12 to 15.
［実施例１６］
アルミナ微粒粉(粒度分布ピーク０．５μｍ)１００重量部に対してステアリン酸エマルジョン（固形成分３０重量％、溶媒：水）の固形成分が２０重量部になるように混合した。混合水溶液を室温で乾燥させ、１００μｍのふるいを通して粗大な粒子を取り除き、実施例１６の造形用粉末を得た。
[Example 16]
The solid component of the stearic acid emulsion (solid component 30% by weight, solvent: water) was mixed to 20 parts by weight with respect to 100 parts by weight of the alumina fine powder (particle size distribution peak 0.5 μm). The mixed aqueous solution was dried at room temperature, and coarse particles were removed through a 100 μm sieve to obtain a molding powder of Example 16.
［実施例１７］
アルミナ粗粒粉(粒度分布ピーク１２μｍ)７０重量部とアルミナ微粒粉(粒度分布ピーク０．５μｍ) ３０重量部を混合し、混合したアルミナ原料粉末１００重量部に対して分散剤（Ａ６１１４、東亜合成株式会社製）1重量部、水２５重量部を加え、ステアリン酸エマルジョン(固形成分３０重量％、溶媒：水)の固形成分が２０重量部になるように混合した。混合水溶液をスプレードライ装置（スプレードライヤＡＤＬ３１１Ｓ：ヤマト科学株式会社製）にて造粒粒子径が約３０μｍになるように調製して造粒した。１００μｍのふるいを通して粗大な粒子を取り除き、実施例１７の造形用粉末を得た。
[Example 17]
70 parts by weight of alumina coarse powder (particle size distribution peak 12 μm) and 30 parts by weight of alumina fine powder (particle size distribution peak 0.5 μm) were mixed, and a dispersant (A6114, Toa Gosei) was mixed with 100 parts by weight of the mixed alumina raw material powder. 1 part by weight (produced by Co., Ltd.) and 25 parts by weight of water were added and mixed so that the solid component of the stearic acid emulsion (solid component: 30% by weight, solvent: water) was 20 parts by weight. The mixed aqueous solution was prepared and granulated with a spray dryer (spray dryer ADL311S: manufactured by Yamato Scientific Co., Ltd.) so that the granulated particle diameter became about 30 μm. Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Example 17.
［実施例１８］
アルミナ粗粒粉(粒度分布ピーク３１μｍ) ８０重量部とアルミナ微粒粉(粒度分布ピーク０．５μｍ) ２０重量部を混合し、混合したアルミナ原料粉末１００重量部に対してステアリン酸エマルジョン(固形成分３０重量％、溶媒：水)の固形成分が２０重量部になるように混合した。混合水溶液を室温で乾燥させ粉砕後、１００μｍのふるいを通して粗大な粒子を取り除き、実施例１８の造形用粉末を得た。
[Example 18]
80 parts by weight of alumina coarse powder (particle size distribution peak 31 μm) and 20 parts by weight of alumina fine powder (particle size distribution peak 0.5 μm) were mixed, and 100 parts by weight of the mixed alumina raw material powder was mixed with stearic acid emulsion (solid component 30). (% By weight, solvent: water) was mixed so as to be 20 parts by weight. The mixed aqueous solution was dried at room temperature and pulverized, and coarse particles were removed through a 100-μm sieve to obtain a molding powder of Example 18.
［実施例１９］
アルミナ微粒粉(粒度分布ピーク０．５μｍ)１００重量部に対して分散剤（Ａ６１１４、東亜合成株式会社製）1重量部、水３０重量部を加え、ステアリン酸エマルジョン（固形成分３０重量％、溶媒：水）をアルミナ微粒粉１００重量部に対して熱可塑性バインダー固形成分が３０重量部になるように混合した。混合水溶液をスプレードライ装置（スプレードライヤＡＤＬ３１１Ｓ：ヤマト科学株式会社製）にて造粒した。１００μｍのふるいを通して粗大な粒子を取り除き、造粒粉を作製した。作製した造粒粉１００重量部に対して、アルミナ粗粒粉(粒度分布ピーク３１μｍ)を２０重量部に配合して、Ｖ型混合機（ＶＭ−２：筒井理化学器機株式会社製）にて混合した。１００μｍのふるいを通して粗大な粒子を取り除き、実施例１９の造形用粉末を得た。
[Example 19]
1 part by weight of a dispersant (A6114, manufactured by Toagosei Co., Ltd.) and 30 parts by weight of water are added to 100 parts by weight of alumina fine powder (particle size distribution peak: 0.5 μm), and stearic acid emulsion (solid component: 30% by weight, solvent: : Water) was mixed such that the thermoplastic binder solid component was 30 parts by weight with respect to 100 parts by weight of alumina fine powder. The mixed aqueous solution was granulated with a spray dryer (spray dryer ADL311S: manufactured by Yamato Scientific Co., Ltd.). Coarse particles were removed through a 100 μm sieve to produce a granulated powder. Alumina coarse powder (particle size distribution peak: 31 μm) is blended in 20 parts by weight with respect to 100 parts by weight of the prepared granulated powder, and mixed by a V-type mixer (VM-2: manufactured by Tsutsui Rikakiki Co., Ltd.). did. Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Example 19.
［比較例１］
アルミナ粗粒粉(粒度分布ピーク３１μｍ) １００重量部に対してナイロン樹脂粗粒粉(粒度分布ピーク５０μｍ)１０重量部をＶ型混合機（ＶＭ−２：筒井理化学器機株式会社製）にて混合した。１００μｍのふるいを通して粗大な粒子を取り除き、比較例１の造形用粉末を得た。
[Comparative Example 1]
100 parts by weight of alumina coarse powder (particle size distribution peak: 31 μm) and 10 parts by weight of nylon resin coarse powder (particle size distribution peak: 50 μm) are mixed by a V-type mixer (VM-2: manufactured by Tsutsui Rikakiki Co., Ltd.). did. Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Comparative Example 1.
[比較例２]
アルミナ粗粒粉(粒度分布ピーク３１μｍ) １００重量部に対してポリプロピレン樹脂粉末１０重量部をＶ型混合機（ＶＭ−２：筒井理化学器機株式会社製）にて混合した。１００μｍのふるいを通して粗大な粒子を取り除き、比較例２の造形用粉末を得た。
[Comparative Example 2]
100 parts by weight of alumina coarse powder (particle size distribution peak 31 μm) was mixed with 10 parts by weight of a polypropylene resin powder using a V-type mixer (VM-2: manufactured by Tsutsui Rikakiki Co., Ltd.). Coarse particles were removed through a 100 μm sieve to obtain a molding powder of Comparative Example 2.
以上のようにして得られた実施例１〜１９及び比較例１、２の造形用粉末を、粉末床溶融結合装置（Ｒａｆａｅｌ３００：株式会社アスペクト製）を用いて予熱を行わず、レーザー出力１０Ｗで造形物を作製した。 The molding powders of Examples 1 to 19 and Comparative Examples 1 and 2 obtained as described above were not preheated using a powder bed fusion bonding apparatus (Rafael 300: manufactured by Aspect Co., Ltd.), and the laser power was 10 W. A model was produced.
＜評 価＞
以上のようにして調製した実施例１〜１９及び比較例１、２の造形用粉末、及びそれによって製造された造形物について、以下の測定を行った。結果を表１及び表２に示す。
［熱可塑性バインダー含有量の測定］
熱分析装置（ＴＧ８１２０：リガク株式会社製）を用いて、大気下で１０００℃まで加熱し熱可塑性バインダーを燃焼させ、重量減少から熱可塑性バインダー含有量（ｇ）、残留重量から原料粉末含有量（ｇ）を計算した。
［熱可塑性バインダー融点の測定］
熱分析装置（ＴＧ８１２０：リガク株式会社製）を用いて、ＤＴＡ曲線をから判断した。
［熱可塑性バインダーガラス転移点の測定］
熱分析装置（ＳＤＴ Ｑ６００：ティ・エイ・インストルメンツ・ジャパン株式会社製）を用いて、ＤＳＣ曲線から判断した。
［Ｈａｕｓｎｅｒ比の測定］
粉末の静かさ密度とタップ密度を測定し、前述した式（１）を用いて計算した。
[粒度分布の測定］
乾式のレーザー回折・散乱式粒度分析計（ＭＴ３０００、マイクロトラックベル社製）により測定した。
[原料粉末の表面積]
比表面積を表面積分析装置（ＡＵＴＯＳＯＲＢ-３：ユアサアイオニクス株式会社製）を用いて測定し、前述した式（２）を用いて計算した。
[熱可塑性バインダーの体積]
造形用粉末中の熱可塑性バインダーの重量と熱可塑性バインダーの密度から、前述した式（３）を用いて体積を計算した。
［造形物の作製］
粉末床溶融結合装置（Ｒａｆａｅｌ３００、光源：ＣＯ２のレーザー、株式会社アスペクト製）を用い、大気下、予熱無しで造形物（３ｍｍ×５ｍｍ×７０ｍｍ）を作製した。
<Evaluation>
The following measurements were carried out on the molding powders of Examples 1 to 19 and Comparative Examples 1 and 2 prepared as described above, and the molded articles produced thereby. The results are shown in Tables 1 and 2.
[Measurement of thermoplastic binder content]
Using a thermal analyzer (TG8120: manufactured by Rigaku Corporation), the material is heated to 1000 ° C. in the atmosphere to burn the thermoplastic binder, and the content of the thermoplastic binder (g) is calculated from the weight loss, and the content of the raw material powder is calculated from the residual weight ( g) was calculated.
[Measurement of melting point of thermoplastic binder]
The DTA curve was determined from the DTA curve using a thermal analyzer (TG8120: manufactured by Rigaku Corporation).
[Measurement of glass transition point of thermoplastic binder]
Judgment was made from the DSC curve using a thermal analyzer (SDT Q600: manufactured by TA Instruments Japan Co., Ltd.).
[Measurement of Hausner ratio]
The quietness density and tap density of the powder were measured and calculated using the above-described equation (1).
[Measurement of particle size distribution]
It was measured by a dry laser diffraction / scattering particle size analyzer (MT3000, manufactured by Microtrack Bell).
[Surface of raw powder]
The specific surface area was measured using a surface area analyzer (AUTOSORB-3: manufactured by Yuasa Ionics Co., Ltd.), and calculated using the above-described equation (2).
[Volume of thermoplastic binder]
From the weight of the thermoplastic binder in the molding powder and the density of the thermoplastic binder, the volume was calculated using the above-described formula (3).
[Preparation of molded object]
A molded product (3 mm × 5 mm × 70 mm) was produced without preheating in the atmosphere using a powder bed fusion device (Rafael 300, light source: laser of CO 2 , manufactured by Aspect Co., Ltd.).
表１に示すように、融点（非晶質ではガラス転移点）が低い熱可塑性バインダーを用いた実施例１〜１１では、粉末層形成の工程を１回又は複数回行えば、予熱すること無しに、粉末床溶融結合法により造形物の作製が可能であった。また、レーザー光照射時にガスが発生することもなかった。
一方、高融点の熱可塑性バインダーを用いた比較例１及び比較例２では、粉末層の予熱を行わず造形を行うと、造形物に反りやクラックが生じ、正常な造形物を作成することができなかった。
As shown in Table 1, in Examples 1 to 11 using a thermoplastic binder having a low melting point (glass transition point in the case of amorphous), if the step of forming a powder layer is performed one or more times, no preheating is performed. In addition, it was possible to produce a shaped article by a powder bed fusion method. In addition, no gas was generated during laser light irradiation.
On the other hand, in Comparative Examples 1 and 2 using a high melting point thermoplastic binder, if the molding is performed without preheating the powder layer, warpage or cracks occur in the molded object, and a normal molded object may be created. could not.
表２に示すように、実施例１２〜１９の造形用粉末を用いた場合、粉末層の予熱を行わなくても、粉末層形成工程を１回又は複数回行えば、予熱すること無しに、粉末床溶融結合法により造形物の作製が可能であった。造形物を作製するが可能であった。また、レーザー照射時にガスが発生することもなかった。 As shown in Table 2, when using the molding powders of Examples 12 to 19, without performing preheating of the powder layer, if the powder layer forming step is performed one or more times, without preheating, It was possible to produce a shaped article by the powder bed fusion method. It was possible to make a model. In addition, no gas was generated during laser irradiation.
＜造形用粉末の構造＞
実施例の造形用粉末を走査型電子顕微鏡で観察した結果、得られた模式図を図１に示す。以下に図１中の文言の意味を以下に示す。
・粗粒粉：粒度分布ピークが１０μｍ以上４００μｍ以下の範囲にある原料粉末。
・微粒粉：粒度分布ピークが０．１μｍ以上１０μｍ未満の範囲にある原料粉末。
・粉末粒子状：乾式混合で作製した造形用粉末であり、原料粉末と熱可塑性バインダーの粒子が別粒子状態であることを示す。
・膜状：湿式混合で作製した造形用粉末であり、原料粉末と熱可塑性バインダーが造形用粉末粒子に含まれ、熱可塑性バインダーが溶融固化した状態を示す。
・分散粒子状：湿式混合で作製した造形用粉末であり、原料粉末と熱可塑性バインダーが造形用粉末粒子に含まれ、エマルジョン化した熱可塑性バインダー粒子が原料粉末表面に吸着もしくは一部溶解した状態を示す。
<Structure of molding powder>
FIG. 1 shows a schematic diagram obtained as a result of observing the molding powder of the example with a scanning electron microscope. The meaning of the wording in FIG. 1 is shown below.
Coarse powder: Raw material powder having a particle size distribution peak in the range of 10 μm or more and 400 μm or less.
Fine powder: a raw material powder having a particle size distribution peak in the range of 0.1 μm or more and less than 10 μm.
-Powder particle shape: A molding powder produced by dry mixing, and indicates that the raw material powder and the particles of the thermoplastic binder are in different particle states.
Film form: a molding powder produced by wet mixing, in which the raw material powder and the thermoplastic binder are contained in the molding powder particles, and the thermoplastic binder is melted and solidified.
・ Dispersed particle form: Modeling powder produced by wet mixing, in which the raw material powder and thermoplastic binder are contained in the molding powder particles, and the emulsified thermoplastic binder particles are adsorbed or partially dissolved on the surface of the raw material powder. Is shown.
この発明は上記発明の実施の態様及び実施例の説明に何ら限定されるものではない。特許請求の範囲を逸脱せず、当業者が容易に想到できる範囲で種々の変形態様もこの発明に含まれる。 The present invention is not limited to the description of the embodiments and examples of the above invention. Various modifications are included in the present invention without departing from the scope of the claims and within the scope of those skilled in the art.
Claims (3)
融点又はガラス転移点が２０℃以上１３０℃以下である熱可塑性バインダーと、セラミックス及び／又は金属の原料粉末とを、Ｈａｕｓｎｅｒ比が１．１１以上１．２０以下の造形用粉末となるように混合する造形用粉末調製工程を行い、
前記造形用粉末を造形ステージ上に予熱を行うことなく粉末層を形成する粉末層形成工程と、
前記粉末層にレーザー光を照射して所定のパターン形状に固化させる照射工程と、
を繰り返すことによって造形物を得る造形物の製造方法。 A method for producing a shaped article using a powder bed fusion bonding method,
A thermoplastic binder having a melting point or a glass transition point of not less than 20 ° C. and not more than 130 ° C. and a raw material powder of ceramics and / or metal are mixed so as to form a molding powder having a Hausner ratio of 1.11 or more and 1.20 or less. Perform the molding powder preparation process to
A powder layer forming step of forming a powder layer without preheating the molding powder on a molding stage,
An irradiation step of irradiating the powder layer with laser light to solidify it into a predetermined pattern shape,
And a method for producing a modeled object by repeating the process.
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