JP2023009067A - 窒化ケイ素焼結体、それを用いた転動体、および軸受 - Google Patents
窒化ケイ素焼結体、それを用いた転動体、および軸受 Download PDFInfo
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- JP2023009067A JP2023009067A JP2022167870A JP2022167870A JP2023009067A JP 2023009067 A JP2023009067 A JP 2023009067A JP 2022167870 A JP2022167870 A JP 2022167870A JP 2022167870 A JP2022167870 A JP 2022167870A JP 2023009067 A JP2023009067 A JP 2023009067A
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- silicon nitride
- sintered body
- nitride sintered
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 145
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 238000005096 rolling process Methods 0.000 title claims abstract description 44
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 47
- 239000011148 porous material Substances 0.000 claims abstract description 35
- 239000002344 surface layer Substances 0.000 claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 78
- 238000005245 sintering Methods 0.000 description 62
- 238000000034 method Methods 0.000 description 54
- 239000002994 raw material Substances 0.000 description 51
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 44
- 238000012360 testing method Methods 0.000 description 35
- 239000011863 silicon-based powder Substances 0.000 description 24
- 229910052723 transition metal Inorganic materials 0.000 description 22
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- 238000004519 manufacturing process Methods 0.000 description 18
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
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- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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- 230000036316 preload Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- 238000004876 x-ray fluorescence 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
(窒化ケイ素焼結体)
本実施形態の窒化ケイ素焼結体は、希土類元素およびアルミニウム元素を含む。窒化ケイ素焼結体において、希土類元素の含有量は、窒化ケイ素焼結体の総重量に対して、酸化物換算で6重量%以上13重量%以下であり、アルミニウム元素の含有量は、窒化ケイ素焼結体の総重量に対して、酸化物換算で6重量%以上13重量%以下である。
収縮率[%]=〔{(圧粉体の寸法)-(窒化ケイ素焼結体の寸法)}/圧粉体の寸法〕×100
本実施形態の窒化ケイ素焼結体の収縮率は特に限定されないが、焼結体の寸法精度などの観点から、15%以下であることが好ましく、14%以下であってもよく、13%以下であってもよい。また、収縮率は例えば7%以上であり、8%以上であってもよく、10%以上であってもよい。
PS-RBSN法では、粉末の流動性を向上するために造粒することが多い。第1の手法は、希土類元素およびアルミニウム元素を含む窒化ケイ素焼結体を製造する方法であって、例えば、ケイ素粉末と焼結助剤を含む原料粉末を用いて造粒粉を得る造粒工程と、得られた造粒粉を圧粉体に成形する成形工程と、脱脂工程と、脱脂された圧粉体を焼結する焼結工程とを含む。焼結工程後、必要に応じて窒化ケイ素焼結体に対して研磨などを行ってもよい。
第2の手法は、希土類元素およびアルミニウム元素を含む窒化ケイ素焼結体を製造する方法であって、例えば、ケイ素粉末と焼結助剤を含む原料粉末を乾式で混合する混合工程と、混合された原料粉末を圧粉体に成形する成形工程と、圧粉体を焼結する焼結工程とを含む。第2の手法は、第1の手法と異なり、PS-RBSN法の全工程を乾式で行うことを特徴としている。なお、焼結工程後、必要に応じて窒化ケイ素焼結体に対して研磨などを行ってもよい。
PS-RBSN法で全工程を乾式で行うことで、例えば、水溶媒を用いた場合のケイ素粉末の酸化を防止することができ、またエタノールなどの有機溶媒による環境負荷を軽減できる。
PS-RBSN法で有機バインダを用いずに、窒化ケイ素焼結体を作製することで、焼結による収縮を小さくし、焼結体の寸法精度を向上できる。第1の手法の場合、造粒するために有機バインダなどを用いていることから、その後に脱脂工程が必要になるが、脱脂工程によって有機バインダが抜けた後には空隙が生じるため、焼結による収縮がその分大きくなるおそれがある。
また、収縮が小さくなることで、後続の研磨工程の研磨時間の短縮化などを図ることができる。
PS-RBSN法でバインダ成分を用いずに、窒化ケイ素焼結体を作製することで、脱脂工程を省略でき、その脱脂工程においてバインダ成分の分解により発生し得るCO2などの温室効果ガスの発生を防止できるので、環境負荷を小さくできる。
(1)上記混合工程は、バインダ成分を使用せずに上記原料粉末を混合する工程である。
(2)上記焼結工程は、1000℃~1200℃の範囲内の温度から焼結温度まで昇温させる過程において、1時間以上所定の温度を保持せずに、15℃/min以下の速度で昇温させる工程を含む。
(3)上記焼結温度が1600℃~1900℃の範囲である。
(4)上記焼結助剤は希土類酸化物と酸化アルミニウムを含み、上記原料粉末は、上記希土類酸化物を上記原料粉末全体に対して9.5重量%以上17重量%以下含み、上記酸化アルミニウムを上記原料粉末全体に対して9.5重量%以上17重量%以下含む。
(5)上記希土類酸化物が、Y2O3、CeO2、Nd2O3、およびEu2O3からなる群より選ばれる1種以上を含む。
(6)上記焼結助剤は遷移金属化合物を含み、上記原料粉末は、上記遷移金属化合物を上記原料粉末全体に対して0.1重量%以上5重量%以下含む。
(7)上記遷移金属元素が、Ti、Cr、およびMnからなる群より選ばれる1種以上を含む。
本実施形態の窒化ケイ素焼結体の用途は特に限定されないが、機械特性および熱伝導性に優れることから、軸受部材、圧延用ロール材、コンプレッサ用ベーン、ガスタービン翼、エンジン部品などに用いることができる。軸受部材として、例えば、転がり軸受、直動案内軸受、ボールねじ、直動ベアリングなどの軸受部材に用いることができ、特に軸受の転動体として好適に用いることができる。
本実施形態の軸受の用途は、特に限定されないが、窒化ケイ素焼結体からなる転動体を用いることで、絶縁軸受としての機能を果たすため、使用上、軸受内部に電流が流れるおそれがある構造への適用に適している。例えば、鉄道車両の主電動機、汎用モータ、発電機などの用途に適用できる。また、近年、自動車に代わる移動手段として注目されている空飛ぶクルマにも適用できる。空飛ぶクルマは、種々の社会的問題の解消に期待されており、地域内移動、地域間移動、観光・レジャー、救急医療、災害救助など、様々な場面での活用が期待されている。
表2に示す配合比で原料粉末を準備し、これに有機バインダを3重量%添加し、メディアとして窒化ケイ素ボールを用い、溶媒としてエタノールを用いて、ボールミルにより回転数200rpmで48時間混合した。混合後のスラリーをスプレードライ法により乾燥して造粒して造粒粉を得た。なお、造粒粉を得るために用いた材料の仕様を表1に示す。
上記で得た造粒粉を用い、ゴム型を用いた冷間等圧加圧法により、直径11mmの球状の圧粉体に成形した。圧粉体を窒素雰囲気中、温度800℃で48時間脱脂した後、2.5℃/minの昇温速度で温度1400℃まで昇温し、窒素雰囲気中(圧力:0.9MPa)、温度1400℃で4時間保持して窒化させた。その後、窒化させた圧粉体を、2.5℃/min~20℃/minの昇温速度で温度1550℃~1950℃まで昇温し、窒素雰囲気中(圧力:0.9MPa)、その焼結温度で4時間保持して窒化ケイ素焼結体を得た。
上記で得た造粒粉を用い、ゴム型を用いた冷間等圧加圧法により、直径11mmの球状の圧粉体に成形した。圧粉体を窒素雰囲気中、温度800℃で48時間脱脂した後、20℃/minの昇温速度で温度1800℃まで昇温し、窒素雰囲気中(圧力:0.9MPa)、焼結温度1800℃で4時間保持して窒化ケイ素焼結体を得た。実施例27~実施例29では、温度1400℃で4時間窒化させる工程(温度保持)を省略した。
収縮率[%]=〔{(圧粉体の直径)-(窒化ケイ素焼結体の直径)}/圧粉体の直径〕×100
実施例および比較例で得た試験片を、その中心を通る断面で切断して、切断面を鏡面研磨した。鏡面研磨した切断面を、株式会社キーエンス製「VHX5000」を用いて撮影し、その撮影画像を、三谷商事株式会社製「WinRoof」を用いて解析し、球状の試験片の表面から2mm以内の範囲に相当する領域である表層部に存在する介在物(I)の最大径および空孔の最大径を測定した。介在物(I)および空孔の径は、介在物(I)および空孔の包絡面積の平方根として求めた(介在物(I)および空孔の径=√(介在物(I)および空孔の包絡面積))。表層部に、径が50μm超の介在物(I)が存在しないものを「A」と評価し、存在するものを「B」として評価した。また、表層部に径が50μm超の空孔が存在しないものを「A」と評価し、存在するものを「B」として評価した。介在物(I)および空孔は、表層部に介在物(I)および空孔の全体が存在するものを測定対象とした。また、表層部の総断面積に対する介在物(I)の総断面積の割合を算出した(介在物(I)の総断面積の割合=介在物(I)の包絡面積÷表層部の総断面積×100)。結果を表4に示す。
実施例および比較例で得た試験片を、その中心を通る断面で切断して、切断面を鏡面研磨し、JIS R 1607に準拠し、破壊靱性の値を測定した。
実施例および比較例で得た試験片を用いて2球圧砕試験を行った。圧砕試験はJIS B 1501に準拠した。
実施例および比較例で得た試験片を用い、軸受外輪、軸受内輪、および保持器としてNTN株式会社製「6206」を用いて、回転数を3000rpm、負荷荷重1.5GPa、試験時間を168時間として転動疲労試験を行い、製品寿命を評価した。潤滑油は、JXTGエネルギー株式会社製の無添加タービンオイル「VG56」を用いた。試験時間内に試験片が剥離しなかったものを「a」と評価し、剥離したものを「b」と評価した。結果を表4に示す。
実施例6で得た試験片の切断面について、走査電子顕微鏡((株)日立製作所製、S300)を用い、EDX分析によって、表層部に含まれる介在物(I)の元素の種類および含有量を測定した。介在物(I)はクロムのケイ化物を含んでおり、介在物(I)に含まれる元素およびその含有量は、クロム(Cr)が56重量%であり、ケイ素(Si)が44重量%であった。
試験例2では、実施例30を除いて、乾式混合によって造粒粉を得た。まず、上記表1に示した原料粉末を、上記表2に示した配合比で準備した。
メディアとして窒化ケイ素ボールを用いて、ボールミルにより回転数200rpmで48時間、乾式混合した。得られた混合粉末を用い、ゴム型を用いた冷間等圧加圧法により、直径11mmの球状の圧粉体に成形した。この圧粉体を、室温から、表2に示す2.5℃/min~20℃/minの昇温速度で温度1550℃~1950℃まで昇温し、窒素雰囲気中(圧力:0.9MPa)、その焼結温度で4時間保持して窒化ケイ素焼結体を得た。
原料粉末に、有機バインダを原料粉末全体に対して3重量%添加し、メディアとして窒化ケイ素ボールを用い、溶媒としてエタノールを用いて、ボールミルにより回転数200rpmで48時間混合した。混合後のスラリーをスプレードライ法により噴霧して乾燥して造粒粉を得た。得られた造粒粉を用い、ゴム型を用いた冷間等圧加圧法により、直径11mmの球状の圧粉体に成形した。圧粉体を窒素雰囲気中、温度800℃で48時間脱脂した後、2.5℃/minの昇温速度で温度1800℃まで昇温し、窒素雰囲気中(圧力:0.9MPa)、焼結温度1800℃で4時間保持して窒化ケイ素焼結体を得た。
実施例27の各試験片を用いて、上記試験例1と同様に、表層部に存在する空孔の最大径を測定した。上記表4および表5の結果より、各試験片には、表層部に径が50μm超の空孔は存在していない。今回は、さらに径が10μm以上の空孔が存在するか否かの評価を行った。結果を表6に示す。
実施例27の各試験片を用いて、上記試験例1よりも高荷重条件の転動疲労試験を行った。上記試験例1の試験条件を、負荷荷重3.5GPa、試験時間630時間に変更した以外は同様の条件を用いた。試験時間内における試験片の剥離の有無を評価した。結果を表6に示す。
2 内輪
3 外輪
4 転動体
5 保持器
6 シール部材
7 グリース
8a、8b 開口部
11 電動垂直離着陸機
12 本体部
13 駆動部
14 回転翼
15 モータ
16 ハウジング
17 回転軸
18 内輪間座
19 外輪間座
20 ノズル部材
21 転がり軸受
22 内輪
23 外輪
24 玉
Claims (6)
- 希土類元素およびアルミニウム元素を含む窒化ケイ素焼結体であって、
前記希土類元素の含有量は、前記窒化ケイ素焼結体の総重量に対して、酸化物換算で6重量%以上13重量%以下であり、
前記アルミニウム元素の含有量は、前記窒化ケイ素焼結体の総重量に対して、酸化物換算で6重量%以上13重量%以下であり、
前記窒化ケイ素焼結体の表面から2mm以内の領域である表層部に空孔を有し、該空孔の最大径が50μm以下であることを特徴とする窒化ケイ素焼結体。 - 前記希土類元素が、Y、Ce、NdおよびEuからなる群より選ばれる1種以上を含むことを特徴とする請求項1記載の窒化ケイ素焼結体。
- 前記希土類元素がCeを含むことを特徴とする請求項1または請求項2記載の窒化ケイ素焼結体。
- 請求項1から請求項3までのいずれか1項記載の窒化ケイ素焼結体を用いたことを特徴とする転動体。
- 請求項4記載の転動体を用いたことを特徴とする軸受。
- 前記軸受は、回転翼および該回転翼を回転させるモータを有する駆動部を複数備え、前記回転翼の回転によって飛行する電動垂直離着陸機に搭載され、前記駆動部における回転軸を支持する軸受であることを特徴とする請求項5記載の軸受。
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