JP7235044B2 - SiC-Siコンポジット部材の製造方法およびSiC-Siコンポジット部材 - Google Patents
SiC-Siコンポジット部材の製造方法およびSiC-Siコンポジット部材 Download PDFInfo
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- JP7235044B2 JP7235044B2 JP2020512239A JP2020512239A JP7235044B2 JP 7235044 B2 JP7235044 B2 JP 7235044B2 JP 2020512239 A JP2020512239 A JP 2020512239A JP 2020512239 A JP2020512239 A JP 2020512239A JP 7235044 B2 JP7235044 B2 JP 7235044B2
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Description
(I)3D印刷法により、SiC粒子を含む第1の成形体を調製する工程であって、前記第1の成形体は、第1の平均細孔径M1を有する、工程と、
(II)前記第1の成形体を、炭素粒子を含む分散液と接触させることにより、ポアに前記炭素粒子が含浸された第2の成形体を形成する工程であって、前記炭素粒子は、二次粒子の平均粒径をM2として、M2≦M1/10を満たす、工程と、
(III)前記第2の成形体に金属Siを含浸させ、前記第2の成形体を反応焼結させることにより、SiC-Siコンポジット部材を得る工程と、
を有し、
前記(III)の工程後に得られるSiC-Siコンポジット部材は、5質量%~40質量%の範囲のSiを含む、製造方法が提供される。
SiC-Siコンポジット部材であって、
平均粒径が30μm~200μmのα-SiC粒子、平均粒径が1μm~20μmのβ-SiC粒子、および金属Siを含む、海島構造を有し、
前記金属Siは、前記海島構造の海部を構成し、前記金属Siで構成される海部の中に、前記α-SiC粒子からなる第1の島部と、前記β-SiC粒子からなる第2の島部とが存在する、SiC-Siコンポジット部材が提供される。
SiC-Siコンポジット部材の製造方法であって、
(I)3D印刷法により、SiC粒子を含む第1の成形体を調製する工程であって、前記第1の成形体は、第1の平均細孔径M1を有する、工程と、
(II)前記第1の成形体を、炭素粒子を含む分散液と接触させることにより、ポアに前記炭素粒子が含浸された第2の成形体を形成する工程であって、前記炭素粒子は、二次粒子の平均粒径をM2として、M2≦M1/10を満たす、工程と、
(III)前記第2の成形体に金属Siを含浸させ、前記第2の成形体を反応焼結させることにより、SiC-Siコンポジット部材を得る工程と、
を有し、
前記(III)の工程後に得られるSiC-Siコンポジット部材は、5質量%~40質量%の範囲のSiを含む、製造方法が提供される。
以下、図1を参照して、本発明の一実施形態によるSiC-Siコンポジット部材の製造方法の一例について、詳しく説明する。
(1)3D印刷法により、SiC粒子を含む第1の成形体を調製する工程(工程S110)と、
(2)前記第1の成形体のポアに、炭素粒子を含浸させ、第2の成形体を形成する工程(工程S120)と、
(3)前記第2の成形体を乾燥する工程(工程S130)と、
(4)前記第2の成形体にSiを含浸させ、前記第2の成形体を反応焼結させることにより、SiC-Siコンポジット部材を得る工程(工程S140)と、
を有する。
工程S110では、3D印刷法を用いて、SiC粒子を含む第1の成形体が形成される。
まず、第1の製造方法で使用され得る3D印刷法について説明する。
粉体層に含まれるSiC粒子の平均粒径は、例えば、30μm~200μmの範囲である。SiC粒子の平均粒径は、50μm~180μmの範囲であることが好ましい。
3D印刷法により製造される第1の成形体は、通常、多孔質体であり、多数のポアを有する。
次に、工程S120では、第1の成形体のポアに炭素粒子が含浸され、第2の成形体が形成される。
次に、必要な場合、第2の成形体が乾燥処理される。
次に、工程S140では、乾燥された第2の成形体から、SiC-Siコンポジット部材が製造される。
以下、図2を参照して、本発明の一実施形態によるSiC-Siコンポジット部材の一例について、詳しく説明する。
(i)微細組織の第2の島部において、複数のβ-SiC粒子が相互に連結されて構成された領域において、いずれかのβ-SiC粒子を中心Xとする直径200μmの円Zを描く。例えば、図3には、そのような操作により、微細組織上に描かれた円Zの一例が示されている。
(ii)次に、円Z内に、中心Xを通る長さ200μmの第1の直線を引く。例えば、図4には、そのような操作により、円Z内に描かれた第1の直線Lの一例が示されている。
(iii)円Z内に、中心Xを中心軸として、第1の直線Lに対する回転角が1°の、長さ200μmの第2の直線を引く。
(iv)(iii)と同様の操作を、回転角180°まで繰り返し、円Z内に合計180本の直線を引く。
(v)各直線において、金属Siの「海部」を横断する1または複数の線分のそれぞれの寸法を測定し、得られた線分の寸法の平均値Saveを求める。これにより、直線180本のそれぞれに対応する平均値Saveが得られる。
(vi)直線180本の中から、前記平均値Saveが最大となる直線を選定し、該直線の前記平均値Saveを最大寸法Smaxとする。また、直線180本の中から、前記平均値Saveが最小となる直線を選定し、該直線の前記平均値Saveを最小寸法Sminとする。以下の(1)式
P=Smax/Smin (1)式
から、P値を算出する。
以下のように、前述の第1の製造方法に従って、SiC-Siコンポジット部材を製造した。
例1と同様の方法により、焼結体(以下、「例2に係る焼結体」と称する)を製造した。
例1と同様の方法により、焼結体(以下、「例3に係る焼結体」と称する)を製造した。
例1と同様の方法により、焼結体(以下、「例4に係る焼結体」と称する)を製造した。
例1と同様の方法により、焼結体(以下、「例5に係る焼結体」と称する)を製造した。
各焼結体の物性を測定した。具体的には、各焼結体に含まれる未反応の金属Siの量、嵩密度、およびポロシティを測定した。
例1~例3に係る焼結体の強度を、4点曲げ試験により評価した。
例2と同様の方法により、焼結体(以下、「例6に係る焼結体」と称する)を製造した。
例6に係る焼結体を用いて、以下の評価を行った。
例6に係る焼結体を切断して得られた断面に対して、組織観察を行った。
P=Smax/Smin (1)式
から得られるP値は、4.6となった。
例6に係る焼結体の強度を、4点曲げ試験により評価した。その結果、強度は、280MPaであった。
例6に係る焼結体の熱伝導率を、キセノンフラッシュ法により評価した。その結果、25℃での熱伝導率は、226W/m・Kであった。
Claims (16)
- SiC-Siコンポジット部材の製造方法であって、
(I)3D印刷法により、SiC粒子を含む第1の成形体を調製する工程であって、前記第1の成形体は、第1の平均細孔径M1を有する、工程と、
(II)前記第1の成形体を、炭素粒子を含む分散液と接触させることにより、ポアに前記炭素粒子が含浸された第2の成形体を形成する工程であって、前記炭素粒子は、二次粒子の平均粒径をM2として、M2≦M1/10を満たす、工程と、
(III)前記第2の成形体に金属Siを含浸させ、前記第2の成形体を反応焼結させることにより、SiC-Siコンポジット部材を得る工程と、
を有し、
さらに、前記(II)の工程の後、
(IV)前記第2の成形体を真空凍結乾燥させるステップ
を有し、
前記(III)の工程後に得られるSiC-Siコンポジット部材は、5質量%~40質量%の範囲のSiを含む、製造方法。 - 前記(II)の工程は、前記第1の成形体を、前記炭素粒子を含む分散液中に浸漬することにより実施される、請求項1に記載の製造方法。
- 前記第1の平均細孔径M1は、20μm~100μmの範囲である、請求項1または2に記載の製造方法。
- 前記SiC粒子は、30μm~200μmの範囲の平均粒径を有する、請求項1乃至3のいずれか一つに記載の製造方法。
- 前記平均粒径M2は、100nm~200nmの範囲である、請求項1乃至4のいずれか一つに記載の製造方法。
- 前記分散液中の炭素粒子の含有量は、20質量%~60質量%の範囲である、請求項1乃至5のいずれか一つに記載の製造方法。
- 前記(I)の工程は、前記SiC粒子を含む粉体層に対して、バインダをインクジェット印刷する工程を含む、請求項1乃至6のいずれか一つに記載の製造方法。
- 前記粉体層は、さらに、硬化剤を有する、請求項7に記載の製造方法。
- 前記(III)の工程では、前記第2の成形体に、溶融金属Siが含浸される、請求項1乃至8のいずれか一つに記載の製造方法。
- 前記(III)の工程は、前記金属Siと前記第2の成形体の共存下、金属Siの融点以上の温度で実施される、請求項1乃至9のいずれか一つに記載の製造方法。
- 前記(III)の工程後に得られるSiC-Siコンポジット部材は、嵩密度が2.79g/cm3以上である、請求項1乃至10のいずれか一つに記載の製造方法。
- SiC-Siコンポジット部材であって、
平均粒径が30μm~200μmのα-SiC粒子、平均粒径が1μm~20μmのβ-SiC粒子、および金属Siを含む、海島構造を有し、
前記金属Siは、前記海島構造の海部を構成し、前記金属Siで構成される海部の中に、前記α-SiC粒子からなる第1の島部と、前記β-SiC粒子からなる第2の島部とが存在し、
前記第2の島部の少なくとも一部は、複数の前記β-SiC粒子が相互に連結されて構成されており、
当該SiC-Siコンポジット部材の断面を20倍で撮影した際に、以下の手順:
(I)前記複数のβ-SiC粒子が相互に連結されて構成された前記第2の島部において、いずれかのβ-SiC粒子を中心とする直径200μmの円を描く;
(II)前記円内に、前記中心を通る長さ200μmの第1の直線を引く;
(III)前記円内に、前記中心を中心軸として、前記第1の直線に対する回転角が1°の、長さ200μmの第2の直線を引く;
(IV)前記(III)と同様の操作を、回転角180°まで繰り返し、前記円内に合計180本の直線を引く;
(V)各直線において、前記海部を横断する1または複数の線分のそれぞれの寸法を測定し、前記線分の寸法の平均値S ave を求める;
(VI)前記直線180本の中から、前記平均値S ave が最大となる直線を選定し、該直線の前記平均値S ave を最大寸法S max とするとともに、前記直線180本の中から、前記平均値S ave が最小となる直線を選定し、該直線の前記平均値S ave を最小寸法S min とし、
以下の(1)式
P=S max /S min (1)式
から、比Pを算出する;
で求められる比Pが3以上である、SiC-Siコンポジット部材。 - 前記α-SiC粒子と前記β-SiC粒子の合計の含有量は、60質量%以上95質量%以下である、請求項12に記載のSiC-Siコンポジット部材。
- 前記β-SiC粒子の体積に対する前記α-SiC粒子の体積の比(α-SiC/β-SiC)は、0.5~10である、請求項12または13に記載のSiC-Siコンポジット部材。
- 前記金属Siの体積に対する前記β-SiC粒子の体積の比(β-SiC/金属Si)は、0.4~12である、請求項12乃至14のいずれか一つに記載のSiC-Siコンポジット部材。
- 熱伝導率が200W/m・K以上である、請求項12乃至15のいずれか一つに記載のSiC-Siコンポジット部材。
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