JP2020079431A - 粉末積層造形に用いるための粉末材料、これを用いた粉末積層造形法および造形物 - Google Patents
粉末積層造形に用いるための粉末材料、これを用いた粉末積層造形法および造形物 Download PDFInfo
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- JP2020079431A JP2020079431A JP2018212471A JP2018212471A JP2020079431A JP 2020079431 A JP2020079431 A JP 2020079431A JP 2018212471 A JP2018212471 A JP 2018212471A JP 2018212471 A JP2018212471 A JP 2018212471A JP 2020079431 A JP2020079431 A JP 2020079431A
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- 238000000465 moulding Methods 0.000 title claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims description 101
- 239000000654 additive Substances 0.000 claims description 39
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- 229910001887 tin oxide Inorganic materials 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
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- 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
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 1
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- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- 229910018605 Ni—Zn Inorganic materials 0.000 description 1
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- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
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- LRTTZMZPZHBOPO-UHFFFAOYSA-N [B].[B].[Hf] Chemical compound [B].[B].[Hf] LRTTZMZPZHBOPO-UHFFFAOYSA-N 0.000 description 1
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 1
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- 238000004220 aggregation Methods 0.000 description 1
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
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- 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
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000006185 dispersion Substances 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- 238000007561 laser diffraction method Methods 0.000 description 1
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- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
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- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
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- 239000010955 niobium Substances 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
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 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
- 239000011368 organic material Substances 0.000 description 1
- KJXBRHIPHIVJCS-UHFFFAOYSA-N oxo(oxoalumanyloxy)lanthanum Chemical compound O=[Al]O[La]=O KJXBRHIPHIVJCS-UHFFFAOYSA-N 0.000 description 1
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-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
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-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
- 239000013618 particulate matter Substances 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
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- 238000007493 shaping process Methods 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- 239000010944 silver (metal) Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- 230000003746 surface roughness Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- 238000011144 upstream manufacturing Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- 238000005550 wet granulation Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
そして他の一つは、粉末材料を薄層状に堆積させた後、この堆積層にインクジェットによりバインダ(結合剤)を目的の断面形状に噴射し、粉末粒子を接合させて接合層を形成する、インクジェット方式である(例えば、特許文献2参照)。
本実施形態における粉末材料は、造粒焼結法、溶融粉砕法などによって製造できるが、この限りではない。
造粒焼結法とは、原料粒子を二次粒子の形態に造粒した後、焼結して、原料粒子同士を強固に結合(焼結)させる手法である。この造粒焼結法において、造粒は、例えば、乾式造粒あるいは湿式造粒等の造粒方法を利用して実施することができる。造粒方法としては、具体的には、例えば、転動造粒法、流動層造粒法、撹枠造粒法、破砕造粒法、溶融造粒法、噴霧造粒法、マイクロエマルション造粒法等が挙げられる。なかでも好適な造粒方法として、噴霧造粒法が挙げられる。
粉末材料は、セラミックスと共に、金属、合金、またはそれらの混合物を含む。例えば、サーメットの粒子は、セラミックス粒子からなる原料粒子と金属粒子からなる原料粒子の混合物から得られる、セラミックス一次粒子と金属一次粒子が結合して間隙をもって三次元的に結合されてなる二次粒子であってもよい。原料粒子の組成については特に制限されない。製造したい目的の粉末材料(二次粒子)に合わせて適宜選択され、例えば、金属、合金、セラミックス、またはその混合物からなる材料である。
酸化物としては、特に限定されることなく各種の金属の酸化物とすることができる。酸化物系セラミックスを構成する金属元素としては、例えば、B、Si、Ge、Sb、Bi等の半金属元素、Mg、Ca、Sr、Ba、Zn、Al、Ga、In、Sn、Pb等の典型元素、Sc、Y、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ni、Cu、Ag、Au等の遷移金属元素、La、Ce、Pr、Nd、Sm、Er、Lu等のランタノイド元素から選択される1種または2種以上が挙げられる。なかでも、Mg、Y、Ti、Zr、Cr、Mn、Fe、Zn、Al、Erから選択される1種または2種以上の元素であることが好ましい。
本発明における粉末材料を用いた三次元造形物の粉末積層による製造方法は、例えば、次のような方法がある。図1は粉末積層造形のための積層造形装置の簡略図の一例を示しており、大まかな構成として、積層造形が行われる空間である積層エリア10と、粉末材料を貯留しておくストック12と、積層エリア10への粉末材料の供給を補助するワイパ11と、粉末材料を固化するための固化手段(インクジェットヘッド、レーザ発振器等)13と、を備えている。積層エリア10は、典型的には、外周が囲まれた造形空間内を造形面より下方に有し、この造形空間内に昇降可能な昇降テーブル14を備えている。この昇降テーブル14は、所定厚みΔt1ずつ降下することができ、この昇降テーブル14上に目的の造形物を造形してゆく。ストック12は、積層エリア10の傍に配置され、例えば、外周が囲まれた貯留空間内に、シリンダー等によって昇降可能な底板(昇降テーブル)を備えている。底板が上昇することで、所定量の粉末材料を造形面に供給(押し出し)することができる。
以下、本発明に関する実施例を説明するが、本発明を以下の実施例に示すものに限定することを意図したものではない。
実施例1〜6及び比較例1〜2の主粉末は、それぞれタングステンカーバイド(WC)からなる原料粒子(平均粒子径2μm)およびコバルト(Co)からなる原料粒子(平均粒子径2μm)をスラリー化しアトライダで混合した。その後、噴霧乾燥型造粒機(スプレードライヤ)で造粒し、その後焼結し、解砕、分級することにより、表1に示す平均粒子径のWC/12質量%Coサーメット粉末材料を構成している。なお、原料粒子の平均粒子径は、レーザ回折/散乱式粒度測定器(株式会社堀場製作製 LA−300)を用いて測定した。
実施例1〜6及び比較例2の添加粉末は、それぞれタングステンカーバイド(WC)からなる原料粒子およびコバルト(Co)からなる原料粒子を加熱溶融した後に冷却することにより固化物(インゴット)を形成し、該固化物を粉砕、分級することにより、表1に示す平均粒子径のWC/10質量%Coサーメット粉末材料を構成している。
得られた主粉末および添加粉末の体積基準の粒度分布における積算値50%におけるDv50粒径をそれぞれ測定した。Dv50粒径は、レーザ回折/散乱式粒度測定器(株式会社堀場製作製 LA−300)を用いて測定し、得られた結果を主粉末のDv50をA、添加粉末のDv50をBとして表1に示した。
得られた主粉末および添加粉末の空隙率を、任意に選択した粒子の断面を500倍の電子顕微鏡画像で観察して断面における空隙の面積を全断面積で除した値の平均値を算出し、表1に示した。
得られた主粉末と添加粉末を混合し、JIS R 1628:1997に基づいてタップ密度を測定した。また、得られたタップ密度(g/cm3)、理論密度(g/cm3)およびタップ密度を理論密度で除したタップ充填率(%)をそれぞれ表1に示した。理論密度は、具体的には、下記式にて求めた。
理論密度=[15.63(WCの密度)× 主粉末中のWC重量% + 8.9(Coの密度)× 主粉末中のCo 重量%] × 主粉末の重量% +[15.63(WCの密度)× 添加粉末中のWC重量% + 8.9(Coの密度)× 添加粉末中のCo 重量%] × 添加粉末の重量%
表1に示す主粉末と添加粉末の混合比率からなる粉末材料を使用して、(製品名:ProXDMP 200、3DSystem社製)により、平らに敷いた粉末にレーザを照射し、一層ずつ溶融させ、この工程を繰り返すことで造形物を製造した。この際、出力300W、走査速度300mm/s、ピッチ幅0.1mm、積層厚さ30μmとした。
得られた造形物の相対密度は、アルキメデス法による密度を理論密度で除した値をパーセント表示で表1に示した。
得られた造形物の気孔率は、次に式により求めた。
気孔率(%)=100(%)−相対密度(%)
実施例1〜6および比較例1においては、気孔率が7%を超えたため良○で評価した。これに対して比較例2は気孔率が7%であったため不良×とした。
平均気孔径の測定は、走査型電子顕微鏡(SEM;株式会社日立ハイテクノロジーズ製、S−3000N)による観察像(好適には、二次電子像、組成像あるいはX線像のいずれかであり得る。)に基づき、画像解析ソフト(株式会社日本ローパー製、Image−Pro Plus)を用いて画像解析すること行った。その結果に基づいて、個数基準で気孔の平均気孔径、標準偏差および半値幅をそれぞれ求め、小さい気孔径から数えた個数基準の分布における積算値10%、90%での気孔径をP10、P90とし、P90/P10の値を求め表1に示した。P90/P10が2以下のものは気孔径が均一であるため良○と評価し、P90/P10が2を超えるものは気孔径が不均一であるため不良×と評価した。実施例1〜6および比較例2は良○であったが、比較例1は×であった。
Claims (9)
- セラミックと金属を含み、(タップ密度/理論密度)×100%で定義されるタップ充填率が30%以上、40%未満である、粉末積層造形に用いられる粉末材料。
- 前記粉末材料は、主粉末と、添加粉末とを含み、前記主粉末の空隙率は前記添加粉末の空隙率より大きい請求項1に記載の粉末材料。
- 前記主粉末の体積基準の粒度分布における積算値50%における粒子径(Dv50)をAとし、前記添加粉末の体積基準の粒度分布における積算値50%における粒子径(Dv50)をBとするとき、A/Bが25以下である請求項1または2に記載の粉末材料。
- 前記主粉末の粒度範囲分布が5〜150μmであり、前記添加粉末の粒度範囲が0.1〜15μmである請求項1〜3のいずれか一項に記載の粉末材料。
- 前記粉末積層造形によりセラミックフィルターまたは触媒担体材料を製造するために用いられる請求項1〜4のいずれか一項に記載の粉末材料。
- 請求項1〜5のいずれか一項に記載の粉末材料が粉末積層造形されてなる造形物。
- セラミックフィルターまたは触媒担体材料である、請求項6に記載の造形物。
- 請求項1〜5のいずれか一項に記載の粉末材料を用いた粉末積層造形方法。
- 請求項8に記載の粉末積層造形方法を用いる、超硬合金の製造方法。
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