JP2020100141A - 無機材料粉末、および構造体の製造方法 - Google Patents
無機材料粉末、および構造体の製造方法 Download PDFInfo
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- JP2020100141A JP2020100141A JP2019220766A JP2019220766A JP2020100141A JP 2020100141 A JP2020100141 A JP 2020100141A JP 2019220766 A JP2019220766 A JP 2019220766A JP 2019220766 A JP2019220766 A JP 2019220766A JP 2020100141 A JP2020100141 A JP 2020100141A
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- 239000000843 powder Substances 0.000 title claims abstract description 210
- 229910010272 inorganic material Inorganic materials 0.000 title claims abstract description 107
- 239000011147 inorganic material Substances 0.000 title claims abstract description 94
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- 239000000463 material Substances 0.000 claims abstract description 59
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- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 31
- -1 transition metal nitride Chemical class 0.000 claims abstract description 17
- 150000003624 transition metals Chemical class 0.000 claims abstract description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 12
- 229910021332 silicide Inorganic materials 0.000 claims abstract description 10
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims abstract description 9
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910006249 ZrSi Inorganic materials 0.000 claims description 3
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
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- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 abstract 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- HCDMJFOHIXMBOV-UHFFFAOYSA-N 3-(2,6-difluoro-3,5-dimethoxyphenyl)-1-ethyl-8-(morpholin-4-ylmethyl)-4,7-dihydropyrrolo[4,5]pyrido[1,2-d]pyrimidin-2-one Chemical compound C=1C2=C3N(CC)C(=O)N(C=4C(=C(OC)C=C(OC)C=4F)F)CC3=CN=C2NC=1CN1CCOCC1 HCDMJFOHIXMBOV-UHFFFAOYSA-N 0.000 description 1
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
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- 239000002182 crystalline inorganic material Substances 0.000 description 1
- 230000002950 deficient Effects 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
- 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
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
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- 229910001938 gadolinium oxide Inorganic materials 0.000 description 1
- 229940075613 gadolinium oxide Drugs 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
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- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本実施形態の無機材料粉末は、複数の化合物を含み、吸収体である化合物を少なくとも1種類含む。具体的には、粉末に含まれる各粒子が1種類の化合物からなっていても良いし、一つの粒子が複数の化合物からなっていても良い。以下に場合分けをして、順に説明する。
吸収体は、無機材料粉末を含む母材に比べて、造形に使用される波長の光に対して相対的に高い光吸収能を有する。従って、本実施形態にかかる粉末を構造体の造形に用いると、粉末に含まれる吸収体がレーザー光を吸収し発熱する。その熱量によってレーザー光が照射された部分の母材の焼結または溶融が生じ、構造体が造形される。
多くの金属酸化物は赤外線の光吸収能が低いが、Ti2O3、TiO、SiO、ZnO、アンチモンドープ酸化スズ(ATO)、インジウムドープ酸化スズ(ITO)、MnO、MnO2、Mn2O3、Mn3O4、FeO、Fe2O3、Fe3O4、Cu2O、CuO、Cr2O3、CrO3、NiO、V2O3、VO2、V2O5、V2O4、Co3O4、CoOは、赤外線の光吸収能が高いため、吸収体として好適である。
遷移金属はd軌道またはf軌道が閉殻になっていないため、遷移金属炭化物はレーザー光と相互作用を持ちやすい。そのため、遷移金属炭化物は、レーザー光の光吸収能が高く、無機材料粉末内の光拡散を抑えることができるとともに、レーザー光の吸収によって発生した多くの熱を母材に伝え、少ない投入熱量で局所的な溶融が可能となる。即ち、製造プロセスにおいて、レーザー光の照射が低出力や高速スキャンで行われても、精密な構造体を造形することができる。また、レーザー光の光吸収能が高いため、少ない添加量であっても、吸収体として十分に機能する。
遷移金属はd軌道またはf軌道が閉殻になっていないため、遷移金属窒化物はレーザー光と相互作用を持ちやすい。そのため、遷移金属窒化物は、レーザー光の光吸収能が高く、粉末内の光拡散を抑えることができるとともに、レーザー光の吸収によって発生した多くの熱を母材に伝達し、少ない投入熱量で局所的な溶融が可能となる。即ち、製造プロセスにおいて、レーザー光の照射が低出力や高速スキャンで行われても、精密な構造体を造形することができる。また、レーザー光の光吸収能が高いため、少ない添加量であっても、吸収体として十分に機能する。さらに、遷移金属窒化物は、融点が高いため、母材が熔融するまで吸収体としての形状を維持でき、吸収体として機能するため、好ましい。
ケイ化物は、バンドギャップが狭く金属に近い特性を有しているため光吸収能が高く、吸収体として好適である。さらに、ケイ化物は、他の成分と結合してガス化する成分を含んでいないため、レーザー光の照射によって発生するガスがほとんどない。従って、レーザー光を吸収して雰囲気中の酸素や母材と反応し、生じた酸化物は構造体に取り込まれるので、造形不良が生じにくく好ましい。
ホウ化物は、他の成分と結合してガス化する成分が含まれていないため、レーザー光の照射によって発生するガスがほとんどない。そのため、レーザー光を吸収して雰囲気の酸素や母材との反応により酸化物を生じる。さらに、生じた酸化物が溶融し、構造体に取り込まれるので、造形不良が生じにくく好ましい。
本実施形態の粉末に含まれる吸収体の構成元素比は、SEM−EDX、TEM−EDX、電子線回折、X線回折、ICP−AES、ICP−MS、蛍光X線分析、不活性ガス融解法などを組み合わせることで特定することができる。なお、SEM−EDXは走査電子顕微鏡−エネルギー分散型X線分光、TEM−EDXは透過電子顕微鏡−エネルギー分散型X線分光、ICP−AESは誘導結合プラズマ発光分析、ICP−MSは誘導結合プラズマ質量分析のことである。
母材は、吸収体以外の、粉末の主成分をなす化合物であり、構造体の強度等の特性に大きく関与するため、用途に応じて適宜選択される。従って、母材として、構造体に求められる特性を達成するために必要な化合物を1種あるいは複数種選定し、製造に用いられるレーザー光の波長に対する母材の光吸収能に応じて、吸収体としての化合物を選択するとよい。製造する構造体に、特定の特性が求められない場合は、先に構造体の製造時に用いられるレーザー光の波長に適した吸収体の組成を選定し、相対的にレーザー光の波吸収効果が低い金属酸化物を、母材となる化合物として選択するのも好ましい。
本実施形態の無機材料粉末は、造形する構造体の三次元データに基づいて生成されたスライスデータに従って無機材料粉末にレーザー光を照射して造形する付加製造法に好適に用いられる。具体的には、粉末床溶融結合法やクラッディング法を用いた製造方法において使用される。その製造プロセスは、下記の工程(i)と工程(ii)とを繰り返し行うことにより、構造体の製造を行う。
工程(i)無機材料粉末をレーザー光照射部に配置する工程
工程(ii)無機材料粉末にレーザー光を照射し、無機材料粉末を焼結、または溶融および凝固させる工程
次に、上述した各実施例の粉末の三次元造形性について検討した。検討には、造形装置として3D systems社のProX(商品名)シリーズのDMP100を用いた。本粉末1から77および粉末80から88を用いた実施例64〜149、並びに吸収体を含まない粉末79を用いた比較例2を、それぞれ表7、8に示す造形条件で6×6×6mmの構造体を造形した。また、実施例64〜149および比較例2において、粉末層の厚みを20μmとし、基材はアルミナ板を使用した。粉末層の厚みは、図2の造形ステージ部12を下降させる値のことである。レーザー光の照射により粉末層は溶融して厚み方向に縮むため、見かけ上の粉末層の厚みは積層を繰り返すうちに次第に厚みを増し、やがて67〜133μmの範囲に収束する。また、表3および4に記載した粒子径は粒子群の中央値である。従って、表3および4に記載の化合物を含む粒子の平均粒径が、製造プロセスでの粉末層20μmよりも大きいが、使用上問題とならない。造形可能であった構造体は、KLA Tencor社製のAlpha−Step D500(商品名)を用いて、表面粗さRaを計測し、造形精度の確認を行った。構造体の表面よりも側面の方で、相対的に荒れが大きいため、側面で評価を行った。また、表面粗さ計測時のスキャン幅は、1mmである。
A:Raが20μm以下の高い造形精度で指定寸法通りの構造体が得られる。
B:表面や側面にRaが20μm以上の荒れが生じる。
C:形状をなしていない。
12 造形ステージ部
13 リコーター部
14 スキャナ部
15 レーザー光の光源
21 クラッディングノズル
22 粉末供給孔
23 レーザー光
Claims (19)
- レーザー光を照射して造形を行う付加製造法に用いられる無機材料粉末であって、前記無機材料粉末が、母材である無機化合物と、吸収体と、を含み、
前記吸収体が、前記レーザー光に含まれる波長の光に対して前記母材よりも高い光吸収能を有し、Ti2O3、TiO、SiO、ZnO、アンチモンドープ酸化スズ(ATO)、インジウムドープ酸化スズ(ITO)、MnO、MnO2、Mn2O3、Mn3O4、FeO、Fe2O3、Fe3O4、Cu2O、CuO、Cr2O3、CrO3、NiO、V2O3、VO2、V2O5、V2O4、Co3O4、CoOからなる群から選ばれる少なくとも一つから選択されることを特徴とする無機材料粉末。 - レーザー光を照射して造形を行う付加製造法に用いられる無機材料粉末であって、前記無機材料粉末が、母材である無機化合物と、吸収体と、を含み、
前記吸収体が、前記レーザー光に含まれる波長の光に対して前記母材よりも高い光吸収能を有し、遷移金属炭化物、遷移金属窒化物、Si3N4、AlN、ホウ化物、ケイ化物のいずれか一つから選択されることを特徴とする無機材料粉末。 - 前記遷移金属炭化物が、TiCまたはZrCであることを特徴とする請求項2に記載の無機材料粉末。
- 前記遷移金属窒化物が、TiNまたはZrNであることを特徴とする請求項2に記載の無機材料粉末。
- 前記ホウ化物が、TiB2、ZrB2、LaB6のいずれかであることを特徴とする請求項2に記載の無機材料粉末。
- 前記ケイ化物が、TiSi2、ZrSi2、MoSi2のいずれかであることを特徴とする請求項2に記載の無機材料粉末。
- 前記吸収体が、遷移金属炭化物、遷移金属窒化物、Si3N4、AlNのいずれかであり、前記吸収体は、0.5vol%以上10vol%以下の量で前記無機材料粉末に含有されていることを特徴とする、請求項2に記載の無機材料粉末。
- 前記レーザー光の照射により、前記吸収体の少なくとも一部が、前記レーザー光に含まれる波長の光に対する光吸収能が前記吸収体より低い化合物へと変化することを特徴とする請求項1から7のいずれか一項に記載の無機材料粉末。
- 前記光吸収能が前記吸収体より低い化合物の光吸収能は、前記吸収体の光吸収能の5/6倍以下であることを特徴とする請求項8に記載の無機材料粉末。
- 前記光吸収能が前記吸収体より低い化合物の光吸収能は、前記吸収体の光吸収能の1/2倍以下であることを特徴とする請求項9に記載の無機材料粉末。
- 前記母材が、SiO2、Al2O3、ZrO2のいずれかを含むことを特徴とする請求項1から10のいずれか一項に記載の無機材料粉末。
- 前記母材が、さらに希土類酸化物または母材との複合酸化物を含むことを特徴とする請求項11に記載の無機材料粉末。
- 共晶組成であることを特徴とする請求項11または12に記載の無機材料粉末。
- 前記吸収体が、単独で粒子を構成していることを特徴とする請求項1から13のいずれか一項に記載の無機材料粉末。
- 前記粒子の粒子径が、前記母材を含む粒子の粒子径の1/5以下であることを特徴とする、請求項14に記載の無機材料粉末。
- 前記粒子の粒子径が、1μm以上10μm以下であることを特徴とする請求項14または15に記載の無機材料粉末。
- 構造体の製造方法であって、
工程(i)請求項1〜16のいずれか一項に記載の無機材料粉末を前記レーザー光照射部に配置する工程と、
工程(ii)前記無機材料粉末の所定の箇所に前記レーザー光を照射することにより、前記無機材料粉末を焼結、または溶融および凝固させる工程と、
を繰り返し行って構造体を製造することを特徴とする構造体の製造方法。 - 前記工程(i)が、前記無機材料粉末を敷き均す工程であることを特徴とする請求項17に記載の構造体の製造方法。
- 前記工程(i)が、前記無機材料粉末を所定の箇所に噴出させる工程であることで行うことを特徴とする請求項17に記載の構造体の製造方法。
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