JP7472408B2 - 窒化珪素焼結体およびそれを用いた耐摩耗性部材 - Google Patents
窒化珪素焼結体およびそれを用いた耐摩耗性部材 Download PDFInfo
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- JP7472408B2 JP7472408B2 JP2023552579A JP2023552579A JP7472408B2 JP 7472408 B2 JP7472408 B2 JP 7472408B2 JP 2023552579 A JP2023552579 A JP 2023552579A JP 2023552579 A JP2023552579 A JP 2023552579A JP 7472408 B2 JP7472408 B2 JP 7472408B2
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- silicon nitride
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims description 262
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 259
- 239000013078 crystal Substances 0.000 claims description 157
- 239000001301 oxygen Substances 0.000 claims description 100
- 229910052760 oxygen Inorganic materials 0.000 claims description 100
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 99
- 238000002441 X-ray diffraction Methods 0.000 claims description 15
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- 229910052721 tungsten Inorganic materials 0.000 description 3
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- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
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- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
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- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
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- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- 238000003825 pressing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、このような課題に対処するためのものであり、固溶酸素量を制御した窒化珪素焼結体を提供するためのものである。
図1において、符号1は窒化珪素焼結体、符号2は窒化珪素結晶粒子、符号3は粒界相である。図1は、窒化珪素焼結体の断面組織の一例を示した模式図である。
窒化珪素焼結体1は、窒化珪素結晶粒子2と粒界相3を備える。粒界相3は、窒化珪素結晶粒子2同士の隙間に分布している。粒界相3は、後述する焼結助剤が反応して形成される。粒界相3が存在することにより、窒化珪素結晶粒子2が強固に結合し、強度の高い窒化珪素焼結体を形成することができる。また、窒化珪素焼結体には、図示しないポアが存在してもよい。
まず、第一のプロット図を作成する。第一のプロット図では、Siカウント数に対する酸素元素/珪素元素の原子比をプロットする。第一のプロット図では、横軸にSiカウント数(cps)を示し、縦軸にO/Si原子比を示す。続いて、第二のプロット図を作成する。第二のプロット図では、Siカウント数に対する窒素元素/珪素元素の原子比をプロットする。
ベアリングボール4は、窒化珪素焼結体1を球体に加工したものである。ベアリング10は、内輪5と外輪6の間に複数個のベアリングボール4を組込んだ構造を有する。ベアリング10に用いられるベアリングボール4の個数は任意である。
(実施例1~5、比較例1~2)
平均粒径が2.5μm以下、不純物酸素含有量が2質量%以下、α化率が90%以上の窒化珪素粉末を用意した。次に、焼結助剤を用意した。焼結助剤の成分、窒化珪素粉末の割合、および焼結助剤の割合は、表1に記載した通りである。
(付記1)
窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下である、窒化珪素焼結体。
(付記2)
20μm×20μmの前記領域に存在するそれぞれの窒化珪素結晶粒子の固溶酸素量が0.2wt%以上1.5wt%以下である、付記1記載の窒化珪素焼結体。
(付記3)
20μm×20μmの前記領域において、長径が3μm未満の前記窒化珪素結晶粒子の固溶酸素量の平均値と、長径が3μm以上の前記窒化珪素結晶粒子の固溶酸素量の平均値と、の差が0.1wt%以下である、付記1ないし付記2のいずれか1項に記載の窒化珪素焼結体。
(付記4)
前記粒界相を1質量%以上20質量%以下含有している、付記1ないし付記3のいずれか1項に記載の窒化珪素焼結体。
(付記5)
任意の断面の300μm×300μmの領域において、前記窒化珪素結晶粒子の長径の最大値が25μm以下である、付記1ないし付記4のいずれか1項に記載の窒化珪素焼結体。
(付記6)
任意の断面をXRD分析したとき、42.4±0.3°に検出される最強ピーク強度をI42.4°とし、β-Si3N4結晶に応じた27.1±0.3°、33.6±0.3°、36.1±0.3°に検出される最強ピーク強度をI27.1°、I33.6°、I36.1°とした場合に、(I42.4°)/(I27.1°+I33.6°+I36.1°)の値が0.005以上0.030以下である、付記1ないし付記5のいずれか1項に記載の窒化珪素焼結体。
(付記7)
破壊靭性値が6MPa・m1/2以上である、付記1ないし付記6のいずれか1項に記載の窒化珪素焼結体。
(付記8)
付記1ないし付記7のいずれか1項に記載の窒化珪素焼結体が用いられた耐摩耗性部材。
(付記9)
ベアリングボール、ころ、ローラ、摩擦攪拌接合用ツール部材から選択される1種である、付記8記載の耐摩耗性部材。
2…窒化珪素結晶粒子
3…粒界相
4…ベアリングボール
5…内輪
6…外輪
10…ベアリング
Claims (16)
- 窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下であり、
破壊靭性値が6MPa・m 1/2 以上である、窒化珪素焼結体。 - 20μm×20μmの前記領域に存在するそれぞれの前記窒化珪素結晶粒子の固溶酸素量が0.2wt%以上1.5wt%以下である、請求項1記載の窒化珪素焼結体。
- 20μm×20μmの前記領域において、長径が3μm未満の前記窒化珪素結晶粒子の固溶酸素量の平均値と、長径が3μm以上の前記窒化珪素結晶粒子の固溶酸素量の平均値と、の差が0.1wt%以下である、請求項1ないし請求項2のいずれか1項に記載の窒化珪素焼結体。
- 前記粒界相を1質量%以上20質量%以下含有している、請求項1ないし請求項2のいずれか1項に記載の窒化珪素焼結体。
- 任意の断面の300μm×300μmの領域において、前記窒化珪素結晶粒子の長径の最大値が25μm以下である、請求項1ないし請求項2のいずれか1項に記載の窒化珪素焼結体。
- 任意の断面をXRD分析したとき、42.4±0.3°に検出される最強ピーク強度をI42.4°とし、β-Si3N4結晶に応じた27.1±0.3°、33.6±0.3°、36.1±0.3°に検出される最強ピーク強度をI27.1°、I33.6°、I36.1°とした場合に、(I42.4°)/(I27.1°+I33.6°+I36.1°)の値が0.005以上0.030以下である、請求項1ないし請求項2のいずれか1項に記載の窒化珪素焼結体。
- 窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下であり、
20μm×20μmの前記領域において、長径が3μm未満の前記窒化珪素結晶粒子の固溶酸素量の平均値と、長径が3μm以上の前記窒化珪素結晶粒子の固溶酸素量の平均値と、の差が0.1wt%以下である、窒化珪素焼結体。 - 窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下であり、
前記粒界相を1質量%以上20質量%以下含有している、窒化珪素焼結体。 - 窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下であり、
任意の断面の300μm×300μmの領域において、前記窒化珪素結晶粒子の長径の最大値が25μm以下である、窒化珪素焼結体。 - 窒化珪素結晶粒子および粒界相を備えた窒化珪素焼結体であって、
任意の断面の20μm×20μmの領域において、前記窒化珪素結晶粒子の固溶酸素量の平均値は0.2wt%以上であり、
任意の断面の50μm×50μmの領域において、前記窒化珪素結晶粒子の長径の平均値は0.1μm以上10μm以下、前記窒化珪素結晶粒子のアスペクト比の平均値は1.5以上10以下であり、
任意の断面をXRD分析したとき、42.4±0.3°に検出される最強ピーク強度をI 42.4° とし、β-Si 3 N 4 結晶に応じた27.1±0.3°、33.6±0.3°、36.1±0.3°に検出される最強ピーク強度をI 27 . 1 °、I 33 . 6 °、I 36 . 1 °とした場合に、(I 42 . 4 °)/(I 27 . 1 °+I 33 . 6 °+I 36 . 1 °)の値が0.005以上0.030以下である、窒化珪素焼結体。 - 請求項1ないし請求項2のいずれか1項に記載の窒化珪素焼結体が用いられた耐摩耗性部材。
- ベアリングボール、ころ、ローラ、摩擦攪拌接合用ツール部材から選択される1種である、請求項11記載の耐摩耗性部材。
- 請求項8に記載の窒化珪素焼結体が用いられた耐摩耗性部材。
- ベアリングボール、ころ、ローラ、摩擦攪拌接合用ツール部材から選択される1種である、請求項13記載の耐摩耗性部材。
- 請求項10に記載の窒化珪素焼結体が用いられた耐摩耗性部材。
- ベアリングボール、ころ、ローラ、摩擦攪拌接合用ツール部材から選択される1種である、請求項15記載の耐摩耗性部材。
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WO2006118003A1 (ja) | 2005-04-28 | 2006-11-09 | Hitachi Metals, Ltd. | 窒化珪素基板、その製造方法、それを用いた窒化珪素配線基板及び半導体モジュール |
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