JPWO2018131331A1 - 樹脂組成物および立体造形物の製造方法 - Google Patents
樹脂組成物および立体造形物の製造方法 Download PDFInfo
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- JPWO2018131331A1 JPWO2018131331A1 JP2018561850A JP2018561850A JPWO2018131331A1 JP WO2018131331 A1 JPWO2018131331 A1 JP WO2018131331A1 JP 2018561850 A JP2018561850 A JP 2018561850A JP 2018561850 A JP2018561850 A JP 2018561850A JP WO2018131331 A1 JPWO2018131331 A1 JP WO2018131331A1
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- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- LVQPBIMCRZQQBC-UHFFFAOYSA-N methoxymethyl 2-methylprop-2-enoate Chemical compound COCOC(=O)C(C)=C LVQPBIMCRZQQBC-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- OINMATXWPCYGSR-UHFFFAOYSA-N n-methylidenebuta-2,3-dienamide Chemical compound C=NC(=O)C=C=C OINMATXWPCYGSR-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229940117969 neopentyl glycol Drugs 0.000 description 1
- 125000002868 norbornyl group Chemical group C12(CCC(CC1)C2)* 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- QUANRIQJNFHVEU-UHFFFAOYSA-N oxirane;propane-1,2,3-triol Chemical compound C1CO1.OCC(O)CO QUANRIQJNFHVEU-UHFFFAOYSA-N 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920005650 polypropylene glycol diacrylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- POSICDHOUBKJKP-UHFFFAOYSA-N prop-2-enoxybenzene Chemical compound C=CCOC1=CC=CC=C1 POSICDHOUBKJKP-UHFFFAOYSA-N 0.000 description 1
- CDXZRBLOGJXGTN-UHFFFAOYSA-N prop-2-enoxycyclohexane Chemical compound C=CCOC1CCCCC1 CDXZRBLOGJXGTN-UHFFFAOYSA-N 0.000 description 1
- UFUASNAHBMBJIX-UHFFFAOYSA-N propan-1-one Chemical compound CC[C]=O UFUASNAHBMBJIX-UHFFFAOYSA-N 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 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
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000011122 softwood Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- MDDUHVRJJAFRAU-YZNNVMRBSA-N tert-butyl-[(1r,3s,5z)-3-[tert-butyl(dimethyl)silyl]oxy-5-(2-diphenylphosphorylethylidene)-4-methylidenecyclohexyl]oxy-dimethylsilane Chemical compound C1[C@@H](O[Si](C)(C)C(C)(C)C)C[C@H](O[Si](C)(C)C(C)(C)C)C(=C)\C1=C/CP(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MDDUHVRJJAFRAU-YZNNVMRBSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005409 triarylsulfonium group Chemical group 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 125000006839 xylylene group Chemical group 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
- B29C64/129—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask
- B29C64/135—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask the energy source being concentrated, e.g. scanning lasers or focused light sources
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/08—Printing inks based on natural resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/14—Printing inks based on carbohydrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
- B29K2033/04—Polymers of esters
Abstract
Description
[1]液体状の樹脂組成物に活性エネルギー線を選択的に照射して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、立体造形物の製造に使用される樹脂組成物であって、活性エネルギー線硬化性の化合物と、ナノファイバーと、を含有し、前記ナノファイバーの全個数に対する、枝分かれ構造を有するナノファイバーの個数の割合は、5%以上である、樹脂組成物。
[2]前記ナノファイバーの全個数に対する、前記枝分かれ構造を有するナノファイバーの個数の割合は、20%以上である、[1]に記載の樹脂組成物。
[3]前記ナノファイバーの平均繊維径は2nm以上100nm以下である、[1]または[2]に記載の樹脂組成物。
[4]前記ナノファイバーの平均繊維長は0.2μm以上100μm以下である、[1]〜[3]のいずれかに記載の樹脂組成物。
[5]前記ナノファイバーのアスペクト比は10以上10000以下である、[1]〜[4]のいずれかに記載の樹脂組成物。
[6]前記活性エネルギー線硬化性の化合物の全質量に対する、前記ナノファイバーの質量の割合は、0.05質量%以上90質量%以下である、[1]〜[5]のいずれかに記載の樹脂組成物。
[7]前記ナノファイバーは、ナノセルロースを主成分とする、[1]〜[6]のいずれかに記載の樹脂組成物。
[8]前記ナノセルロースは、セルロースナノファイバーを含む、[7]に記載の樹脂組成物。
[9]前記ナノセルロースは、セルロースナノクリスタルを含む、[7]に記載の樹脂組成物。
[10][1]〜[9]のいずれかに記載の樹脂組成物に活性エネルギー線を選択的に照射して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、立体造形物の製造方法。
[11]造形槽中で、前記樹脂組成物に活性エネルギー線を選択的に照射して第1の造形物層を形成し、前記第1の造形物層の表面に前記樹脂組成物を供給し、前記供給された前記樹脂組成物に活性エネルギー線を選択的に照射して、前記供給された樹脂組成物が硬化してなる第2の造形物層を形成して前記第1の造形物層に積層し、前記樹脂組成物の供給および造形物層の積層を繰り返して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、[10]に記載の製造方法。
[12]造形槽中で、重合阻害剤により前記樹脂組成物の硬化が阻害されるバッファ領域を透過した活性エネルギー線を、前記重合阻害剤の濃度がより低く前記樹脂組成物が硬化可能な硬化領域に選択的に照射して、前記硬化領域が含有する前記樹脂組成物を硬化させ、前記硬化した樹脂組成物を前記造形槽中の鉛直上下方向に移動させながら前記活性エネルギー線を連続的に照射して、前記樹脂組成物が硬化してなる造形物を立体的かつ連続的に形成する、[10]に記載の製造方法。
[13]前記活性エネルギー線は、前記造形槽の底面方向から前記硬化領域に照射される、[12]に記載の製造方法。
上記樹脂組成物は、活性エネルギー線硬化性の化合物と、多糖類のナノファイバーと、を含有する。
活性エネルギー線硬化性の化合物は、活性エネルギー線を照射されて重合および架橋し、硬化する液体状の化合物であればよい。
トリエチレングリコールジ(メタ)アクリレート、テトラエチレングリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、トリプロピレングリコールジ(メタ)アクリレート、ポリプロピレングリコールジ(メタ)アクリレート、1,4−ブタンジオールジ(メタ)アクリレート、1,6−ヘキサンジオールジ(メタ)アクリレート、1,9−ノナンジオールジ(メタ)アクリレート、シクロヘキサンジ(メタ)アクリレート、シクロヘキサンジメタノールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、トリシクロデカンジイルジメチレンジ(メタ)アクリレート、ジメチロール−トリシクロデカンジ(メタ)アクリレート、ポリエステルジ(メタ)アクリレート、ビスフェノールAのPO付加物ジ(メタ)アクリレート、ヒドロキシピバリン酸ネオペンチルグリコールジ(メタ)アクリレート、ポリテトラメチレングリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、トリプロピレングリコールジ(メタ)アクリレート、およびトリシクロデカンジメタノールジ(メタ)アクリレートなどを含む2官能のアクリレート、ならびに、
トリメチロールプロパントリ(メタ)アクリレート、ペンタエリスリトールトリ(メタ)アクリレート、ペンタエリスリトールテトラ(メタ)アクリレート、ジペンタエリスリトールペンタ(メタ)アクリレート、ジペンタエリスリトールヘキサ(メタ)アクリレート、ジトリメチロールプロパンテトラ(メタ)アクリレート、ジペンタエリスリトールモノヒドロキシペンタ(メタ)アクリレート、グリセリンプロポキシトリ(メタ)アクリレート、およびペンタエリスリトールエトキシテトラ(メタ)アクリレートなどを含む3官能以上のアクリレートなどが含まれる。
ナノファイバーは、平均繊維径が1000nm以下のファイバー状の充填剤である。ナノファイバーは、枝分かれ構造を有するナノファイバーを含む。
上記樹脂組成物は、光重合開始剤を含有してもよい。光重合開始剤は、上記活性エネルギー線硬化性の化合物がラジカル重合性の官能基を有する化合物であるときは光ラジカル開始剤を含み、上記活性エネルギー線硬化性の化合物がカチオン重合性の官能基を有する化合物であるときは光酸発生剤を含む。光重合開始剤は、上記樹脂組成物中に、一種のみが含まれていてもよく、二種類以上が含まれていてもよい。光重合開始剤は、光ラジカル開始剤と光酸発生剤の両方の組み合わせであってもよい。
上述した液体状の樹脂組成物は、活性エネルギー線を選択的に照射して上記樹脂組成物が硬化してなる造形物を立体的に形成して、立体造形物を製造するために用いることができる。
積層造形法では、上記活性エネルギー線を、製造しようとする立体造形物を平面方向に微分割(スライス)した断面形状データに含まれる各層のパターンを上記樹脂組成物に投影することで、上記立体造形物を構成する造形物層し、上記造形物層を積層していくことで、上記立体造形物を形成することができる。
連続造形法では、上記活性エネルギー線を、製造しようとする立体造形物のうち造形中の高さを構成する平面パターンを上記樹脂組成物に投影しながら、上記活性エネルギー線の照射によって硬化した上記樹脂組成物の深さ方向の位置を変えていくことで、上記立体造形物を形成することができる。
なお、上記の説明において、積層造形法では、樹脂組成物の上面側から活性エネルギー線を照射しているが、造形槽の底面側から照射した活性エネルギー線によって立体造形物の各層を形成し、形成された層を剥離して持ち上げて次の層を形成していってもよい。
1−1.ナノファイバーの作製
スギノマシン社製のセルロースナノファイバー分散液であるBiNFi−sを、吉田機械興業社製の湿式高圧分散装置であるナノヴェイタを用いて150MPaの圧力で解繊した。解繊処理の回数を増すごとに、枝分れが増加する様子が確認されたが、繊維長、繊維径にほとんど違いはみられなかった。所定の枝分れ率になるまで解繊処理を繰り返して、セルロースナノファイバー1〜セルロースナノファイバー4の水分散液を得た。
得られた酸化パルプ50gを蒸留水で希釈することにより、5Lの混合溶液を得た。この混合液を吉田機械興業社製の湿式高圧分散装置であるナノヴェイタを用いて150MPaの圧力で解繊した。解繊処理の回数を増すごとに、繊維長が短くなるとともに、枝分れが増加する様子が確認された。一定の平均繊維長となるところまで解繊処理の回数を重ねることにより、セルロースナノファイバー5およびセルロースナノファイバー6の水分散液を得た。
上記得られたセルロースナノファイバー1〜セルロースナノファイバー8およびセルロースナノクリスタル1〜セルロースナノクリスタル2を、メチルエチルケトンで溶媒置換し、セルロースナノファイバーまたはセルロースナノクリスタルの濃度が0.001〜0.0001質量%程度になるまでメチルエチルケトンでさらに希釈した。20μLの上記得られた希釈液をガラス板に滴下して乾燥させ、透過型電子顕微鏡(TEM)で撮像した。撮像された画像から任意に選択された100本のナノファイバーをもとに、枝分かれ構造を有するナノファイバーの個数の割合、ナノファイバーの平均繊維径、ナノファイバーの平均繊維長およびナノファイバーのアスペクト比を測定した。
上記得られたセルロースナノファイバー1〜セルロースナノファイバー8ならびにセルロースナノクリスタル1およびセルロースナノクリスタル2をメチルエチルケトンで溶媒置換して得られた分散液に、活性エネルギー線硬化性の化合物としてトリメチロールプロパントリアクリレートと光重合開始剤としてジフェニル(2,4,6−トリメチルベンゾイル)ホスフィンオキシドとを、ナノファイバーがトリメチロールプロパントリアクリレートに対して表1の濃度となるようにして混合した。この混合液をホモジナイザーで分散させた後、エバポレーターでメチルエチルケトンを脱揮させて、樹脂組成物1〜樹脂組成物12を得た。
2−1.積層造形法
図2に示す構成を有する立体造形物の製造装置が有する造形槽に樹脂組成物1〜樹脂組成物12を投入し、半導体レーザー光(出力100mW、波長355nm)の照射および造形ステージの降下を繰り返して、長さ(以下、造形槽の深さ方向:立体造形物の高さ方法の長さを、単に「長さ」とも表記する。)4mm、幅80mm、厚さ10mmの立体造形物1A〜立体造形物12Aを製造した。
図3に示す構成を有する立体造形物の製造装置が有する造形槽に樹脂組成物3を投入し、半導体レーザー光(出力100mW、波長355nm)を照射しながらサポートステージを上昇させて、長さ4mm、幅80mm、厚さ10mmの立体造形物13Aを製造した。
3−1.方向による強度の比
JIS K 7171に準じて、立体造形物1A〜立体造形物13Aおよび立体造形物1B〜立体造形物13Bの曲げ強さを測定された。支点間距離Lは64mm、試験速度vは2mm/min、圧子の半径R1は5mmとした。
◎◎ Y/X は0.98以上である
◎ Y/X は0.95以上0.98未満である
○ Y/X は0.90以上0.95未満である
△ Y/X は0.85以上0.90未満である
× Y/X は0.85未満である
立体造形物Cから上記方法で測定された曲げ強さZと、立体造形物1B〜立体造形物13Bから測定された曲げ強さYとから得られる、Y/Zの値を用いて、以下の基準でナノファイバーの添加による立体造形物1〜立体造形物12の強度の向上率を評価した。
◎ X/A は1.2より大きい
○ X/A は1.05より大きく1.2以下である
△ X/A は1.05以下である
110、210、310、410 主枝
220、320、420、430 側枝
500 製造装置
510 造形槽
520 造形ステージ
530 ベース
540 照射源
550 ガルバノミラー
600 製造装置
610 造形槽
615 窓部
620 サポートステージ
630 照射源
642 バッファ領域
644 硬化領域
Claims (13)
- 液体状の樹脂組成物に活性エネルギー線を選択的に照射して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、立体造形物の製造に使用される樹脂組成物であって、
活性エネルギー線硬化性の化合物と、ナノファイバーと、を含有し、
前記ナノファイバーの全個数に対する、枝分かれ構造を有するナノファイバーの個数の割合は、5%以上である、樹脂組成物。 - 前記ナノファイバーの全個数に対する、前記枝分かれ構造を有するナノファイバーの個数の割合は、20%以上である、請求項1に記載の樹脂組成物。
- 前記ナノファイバーの平均繊維径は2nm以上100nm以下である、請求項1または2に記載の樹脂組成物。
- 前記ナノファイバーの平均繊維長は0.2μm以上100μm以下である、請求項1〜3のいずれか1項に記載の樹脂組成物。
- 前記ナノファイバーのアスペクト比は10以上10000以下である、請求項1〜4のいずれか1項に記載の樹脂組成物。
- 前記活性エネルギー線硬化性の化合物の全質量に対する、前記ナノファイバーの質量の割合は、0.05質量%以上90質量%以下である、請求項1〜5のいずれか1項に記載の樹脂組成物。
- 前記ナノファイバーは、ナノセルロースを主成分とする、請求項1〜6のいずれか1項に記載の樹脂組成物。
- 前記ナノセルロースは、セルロースナノファイバーを含む、請求項7に記載の樹脂組成物。
- 前記ナノセルロースは、セルロースナノクリスタルを含む、請求項7に記載の樹脂組成物。
- 請求項1〜9のいずれか1項に記載の樹脂組成物に活性エネルギー線を選択的に照射して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、立体造形物の製造方法。
- 造形槽中で、前記樹脂組成物に活性エネルギー線を選択的に照射して第1の造形物層を形成し、
前記第1の造形物層の表面に前記樹脂組成物を供給し、
前記供給された前記樹脂組成物に活性エネルギー線を選択的に照射して、前記供給された樹脂組成物が硬化してなる第2の造形物層を形成して前記第1の造形物層に積層し、
前記樹脂組成物の供給および造形物層の積層を繰り返して、前記樹脂組成物が硬化してなる造形物を立体的に形成する、
請求項10に記載の製造方法。 - 造形槽中で、重合阻害剤により前記樹脂組成物の硬化が阻害されるバッファ領域を透過した活性エネルギー線を、前記重合阻害剤の濃度がより低く前記樹脂組成物が硬化可能な硬化領域に選択的に照射して、前記硬化領域が含有する前記樹脂組成物を硬化させ、
前記硬化した樹脂組成物を前記造形槽中の鉛直上下方向に移動させながら前記活性エネルギー線を連続的に照射して、前記樹脂組成物が硬化してなる造形物を立体的かつ連続的に形成する、
請求項10に記載の製造方法。 - 前記活性エネルギー線は、前記造形槽の底面方向から前記硬化領域に照射される、請求項12に記載の製造方法。
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