JP7211976B2 - 付加製造のための高強度金属ガラス系複合材料 - Google Patents
付加製造のための高強度金属ガラス系複合材料 Download PDFInfo
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- JP7211976B2 JP7211976B2 JP2019566364A JP2019566364A JP7211976B2 JP 7211976 B2 JP7211976 B2 JP 7211976B2 JP 2019566364 A JP2019566364 A JP 2019566364A JP 2019566364 A JP2019566364 A JP 2019566364A JP 7211976 B2 JP7211976 B2 JP 7211976B2
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Description
本明細書に記載の発明は、NASA契約NNN12AA01Cに基づく作業の履行において行われたものであって、契約者が所有権を保持することを選択した公法96-517(35USC202)の規定に従う。
バルク金属ガラス組成物の粉末を、少なくとも1つの追加の金属組成物の粉末と混合する工程であって、少なくとも1つの追加の金属組成物が、バルク金属ガラス組成物から形成されるバルク金属ガラスマトリックス中の亀裂の伝播を抑制するように構成された補強結晶質延性相を形成し、少なくとも1つの金属結晶質相の体積分率が、バルク金属ガラスマトリックス複合材料の15~95体積%である工程;
付加製造の熱源を用いて、バルク金属ガラス組成物と少なくとも1つの追加の金属組成物の混合粉末を、バルク金属ガラスマトリックス組成物内に配置された自然酸化物層が溶解するように少なくとも1つの追加の金属組成物を部分的に溶融させるように溶融する工程;及び
層プリント法によって混合粉末から形成された溶融物を層状に固化させて、2体積%以下の気孔率、バルク部分に形成されたときのバルク金属ガラス組成物の強度の少なくとも50%の総合強度、バルク金属ガラス組成物より少なくとも5%大きい破壊靭性、バルク金属ガラス組成物より少なくとも1%大きい引張延性、及びバルク金属ガラス組成物から形成された100μmの切欠き半径を有する部分で測定したときの切欠き靭性が40MPa・m1/2より大きい切欠き靭性、の群から選択される少なくとも1つの性質を有するバルク金属ガラスマトリックス複合材料を形成する工程を含む、
粉末を基とした付加製造を利用してバルク金属ガラスマトリックス複合材料を形成するための方法を対象とする。
実施形態は、一般に、優れた機械的特性、特に高い靭性及び強度を有する付加製造部品に使用することができる非Be系BMGマトリックス複合材料のための方法及び合金系を対象とする。上述のように、今日まで、BMGMCの開発は、主として、それらが鋳造に適用可能であるという要件によって制限されており、したがって、努力は、BMGマトリックスの良好なガラス形成能力、デンドライト相の容易な相分離、低融点、及び比較的低いデンドライト濃度を有する合金に焦点を当ててきた。しかしながら、やはり上述したように、そのような制約下で得られる合金は、それらの微細構造が致命的な亀裂の成長を阻止しないので、脆い傾向がある。
上述のように、成功したBMGMC材料の形成は、金属マトリックス中の粒子の濃度及びサイズを系統的に制御する技量を必要とする。従来、複合材料の結晶質デンドライト相は、鋳造中にその場(in situ)で形成される(鋳造溶融物の冷却及び固化時に特別に添加された不溶性合金成分が偏析するため)。図11に要約されるように、最良の複合材料は、デンドライトがガラス形成BMG液体と熱平衡状態にあり、そのサイズが図12に示されるように半固体処理によって制御されるような平衡複合材料を作り出すことによって達成された。これらの特性は、マトリックスの結晶化及び粒子の誤った選定のために、他の非BeBMGMCにおいて再現することがほとんど不可能であった。同様に、張力下における有意な延性及び破壊靭性は、Be含有BMGMCにおいてのみ達成される。さらに、文献は、BMGMCの優れた特性は、デンドライトを粗くするために固相線温度を超える半固体(又は等温)保持を使用してのみ得ることができることを示唆している。
上述のように、BMGMC材料の実施形態は、高体積分率で軟質介在物を組み込むが、先行技術の研究によって見出されるように、介在物の体積分率の増加はまた、合金をより高粘度にし、合金の溶融温度を有意に上昇させ、特にBe添加剤を排除した場合に、合金を鋳造することをより困難にする。最近、金属付加製造(AM)技術(3Dプリントとしても知られている)は、新規な金属合金からの正味寸法の部品を付加製造することにおいて急速な進歩を遂げている。典型的には、金属AMは、チタン、鋼板、鋳造アルミニウム合金、及びインコネルなどの従来の結晶質金属合金から構成部品を製造するために使用されてきた。しかしながら、多くのAM技術に固有の急冷速度は、バルク金属ガラス(BMG)及びナノ結晶金属などの準安定合金の製造も可能にした。具体的には、堆積層ごとの103Ks-1を超える冷却速度により、微細構造(又はその欠如)を有する合金から、鋳造又は他の方法では製造できない厚い正味寸法のコンポーネントをプリントすることが可能となった。
以下の実施例は、当業者に対して、本発明を作り、また利用する方法の、完全な開示及び説明を与えるために提示され、また本発明者らが考えているその発明の範囲を限定するものではなく、また以下の実施例は、実施した全ての又は唯一の実施した実験のみを提示しているものでもない。使用した数値(例えば、量、温度等)に関する正確性を確認する努力をなされたが、いくつかの実験誤差及びずれを考慮すべきである。特に断らない限り、部は重量部であって、分子量は重量平均分子量であって、温度は摂氏度であって、圧力は大気圧又はその近傍である。
(Zr系BMG合金の機械的性質の改善)
一体構造のBMGを与えるZr52.5Ti5Cu17.9Ni14.6Al10を用いた付加製造(SLMによる)の実例は、LiらによってMaterials and Dsign112(2016)217-226において報告されており、その記載は、本明細書中で参考文献として援用される。Liらによって付随して報告された圧縮試験からのデータは、付加製造により得られたBMG部品が脆いことを示している。しかしながら、Liが使用するZi系合金は、Beを含有しない良好なガラス形成体であって、図14(a)の表に示したものと同様の組成物を有するため、本出願の付加製造方法に適した合金である。したがって、多くの実施形態において、本出願の方法によれば、Zr52.5Ti5Cu17.9Ni14.6Al10から製造された部品の可塑性、したがって靭性を、3Dプリント中に補強デンドライト相をその場(in situ)又は系外(ex situ)で加えることによって大幅に改善することができる。
(Fe系BMG合金の機械的性質の改善)
実施例1と同様に、安価な一体構造のBMG部品は、Fe系のBMG合金から(選択的レーザー溶融によっても)、これまでにも、Fe74Mo4P10C7.5B2.5Si2などが付加的に製造されており、例えばSimon Pauly,et al.,Materials Today,Vol.16,Numbers1/2,(2013),p.37-41;及びHyo Yun Jung,et al.,Materials&Design,Vol.86(2015),p.703-708.等によって報告されており、これらの開示は、参考文献として本明細書に援用されるが、これらの部品は、一体構造のBMGから予想されるように、脆いことが証明された。しかしながら、多くの実施形態では、Fe74Mo4P10C7.5B2.5Si2または類似の合金の破壊靭性及び延性は、本出願の方法に従って、3Dプリント中に補強デンドライト相をその場(in situ)または系外(ex situ)で付加することによって改善することができる。
本発明のこの説明は、例示及び説明の目的で提示されている。網羅的であること又は本発明を記載された正確な形態に限定することは意図されておらず、上記の教示に照らして多くの修正及び変形が可能である。実施形態は、本発明の原理及びその実用的な用途を最も良く説明するために選択され、説明した。この説明により、当業者は、様々な実施形態において、特定の用途に適した様々な修正を加えて、本発明を最良に利用し、実施することができる。本発明の範囲は、以下の特許請求の範囲によって定義される。
Claims (28)
- ガラス形成能を特徴とし、バルク金属ガラスマトリックスを形成するための、ベリリウムを含まない、バルク金属ガラス組成物の粉末と、
前記バルク金属ガラスマトリックス中に延性結晶相を形成するための、少なくとも1つの追加の金属組成物の粉末とを提供する工程;
前記バルク金属ガラス組成物の粉末と前記少なくとも1つの追加の金属組成物の粉末とを混合して粉末混合体を形成する工程であって、前記少なくとも1つの追加の金属組成物の体積分率は、粉末混合体の15~95体積%である工程;
付加製造の熱源を用いて、少なくともバルク金属ガラス組成物の粉末を、前記バルク金属ガラス組成物の粉末に固有の表面不動態化酸化物層を溶解するように、少なくとも部分的に溶融し、前記粉末混合体を含む層を溶融する工程;
前記層を固化して、前記バルク金属ガラス組成物を含む前記バルク金属ガラスマトリックス内に分散された少なくとも1つの追加の金属組成物を含む延性結晶相を含むバルク金属ガラスマトリックス複合材料を形成する工程であって、
前記延性結晶相の体積分率は、前記バルク金属ガラスマトリックス複合材料の15~95%を構成し、
前記延性結晶相は、前記バルク金属ガラスマトリックス内の亀裂伝播を抑制し、前記バルク金属ガラスマトリックス複合材料を補強し、
前記バルク金属ガラスマトリックス複合材料は、2体積%以下の気孔率、一体構造部分に形成されたときの前記バルク金属ガラス組成物の強度の少なくとも50%の総合強度、前記バルク金属ガラス組成物の破壊靭性よりも少なくとも5%大きい破壊靭性、前記バルク金属ガラス組成物の引張靭性より少なくとも1%大きい引張延性、及び100μmの切欠き半径を有する部分で測定したときの切欠き靭性が40MPa・m1/2より大きい切欠き靭性、からなる群から選択される少なくとも1つの性質を有する工程;及び、
付加製造工程において溶融ステップと固化ステップとを繰り返し、前記バルク金属ガラスマトリックス複合材料からなる複数の層を互いに堆積させて、バルク金属ガラスマトリックス複合材料部分を形成する工程;
とを含む、粉末を基とした付加製造を利用して前記金属複合材料部分を形成するための方法。 - 前記付加製造工程は、粉末床溶融結合、積層造形法、直接金属レーザー焼結法、指向性エネルギー堆積法、電子ビーム製造法及び溶射付加製造法からなる群から選択される工程である、請求項1に記載の方法。
- 前記バルク金属ガラス組成物の粉末の粒径は第1の粒径であることを特徴とし、前記少なくとも1つの追加の金属組成物の粉末の粒径は第2の粒径であることを特徴とし、前記第1の粒径は前記第2の粒径の20%以内である、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料は、1GPaを超える前記全体的な強度を有することを特徴とする、請求項1に記載の方法。
- 前記引張延性は、4%を超える、請求項1に記載の方法。
- 前記破壊靭性は80MPa・m1/2を超える、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、前記バルク金属ガラス組成物のガラス形成能力を実質的に変化させない、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料部分の表面を滑らかにするために、前記表面に機械加工又は仕上げ加工することをさらに含む、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料部分は、結晶質金属表面に適用される、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、前記バルク金属ガラス組成物に対して硬度が少なくとも5%低いことを特徴とする、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、前記バルク金属ガラス組成物に対して剛性率が低いことを特徴とする、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、前記バルク金属ガラス組成物に対して剛性が低いことを特徴とする、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、一体構造の部品として張力において5%を超える延性を示す結晶質金属である、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物及び前記バルク金属ガラス組成物は、それらの最も豊富な元素として同じ金属元素を含む、請求項1に記載の方法。
- 前記バルク金属ガラス組成物は、その最も豊富な金属が、Ti、Zr、Hf、Fe、Co、Ni、Pd、Pt、Cu、Ag、Au、及びAlからなる群から選択される元素である、請求項1に記載の方法。
- 前記バルク金属ガラス組成物はZr-Cu-Alを含む、請求項1に記載の方法。
- 前記バルク金属ガラス組成物は、密度が5.5g/cm3未満のTi系の金属ガラスである、請求項1に記載の方法。
- 前記バルク金属ガラス組成物はZr系であって、前記少なくとも1つの追加の金属組成物は、V、Nb、Ta、Mo又はFeからなる群から選択される1つ又は複数と合金化されたTi又はZr系の合金である、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料は、Ti系で密度が6g/cm3未満である、請求項1に記載の方法。
- 前記バルク金属ガラス組成物は、Fe-Ni-B-Xを含み、前記少なくとも1つの追加の金属組成物は、Fe系である、請求項1に記載の方法。
- 前記バルク金属ガラス組成物及び少なくとも1つの追加の金属組成物の両方はAl、Fe及びTiからなる群から選択される元素系である、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料部分は、腕時計、宝飾品、電子ケース、構造部品、歯車、及び運動ラウンドからなる群から選択される物品である、請求項1に記載の方法。
- 前記延性結晶質相の体積分率は、前記バルク金属ガラスマトリックス複合材料部分全体にわたって変化する、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、W、Mo、Hf及びTaからなる群から選択される耐熱金属相を含む、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物が、バルク金属ガラス組成物中に低い溶解度を有する成分を含み、前記成分がバルク金属ガラス組成物を溶解していることから、デンドライト相が、前記バルク金属ガラスマトリックス中に形成される、請求項1に記載の方法。
- 前記バルク金属ガラスマトリックス複合材料は、前記バルク金属ガラスマトリックスを含むガラス相、前記延性結晶質相を含む結晶質相、及び前記成分を含むデンドライト相、の3つの相を含む、請求項25に記載の方法。
- 前記バルク金属ガラス組成物及び前記少なくとも1つの追加の金属組成物は、前記少なくとも1つの追加の金属組成物が前記バルク金属ガラス組成物に少なくとも部分的に溶解されたときに、前記バルク金属ガラス組成物のガラス形成能力が向上するように選択される、請求項1に記載の方法。
- 前記少なくとも1つの追加の金属組成物は、前記バルク金属ガラス組成物のガラス形成能力と比較してガラス形成能力が向上するように、溶解時に前記バルク金属ガラス組成物に成分を与える、請求項27に記載の方法。
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US11123797B2 (en) | 2021-09-21 |
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