JP2020012199A - 原子層堆積法で堆積させた耐浸食性金属フッ化物コーティング - Google Patents
原子層堆積法で堆積させた耐浸食性金属フッ化物コーティング Download PDFInfo
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- JP2020012199A JP2020012199A JP2019131878A JP2019131878A JP2020012199A JP 2020012199 A JP2020012199 A JP 2020012199A JP 2019131878 A JP2019131878 A JP 2019131878A JP 2019131878 A JP2019131878 A JP 2019131878A JP 2020012199 A JP2020012199 A JP 2020012199A
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- 238000000576 coating method Methods 0.000 title claims abstract description 264
- 239000011248 coating agent Substances 0.000 title claims abstract description 244
- 229910001512 metal fluoride Inorganic materials 0.000 title claims abstract description 59
- 238000000231 atomic layer deposition Methods 0.000 title claims description 100
- 238000000034 method Methods 0.000 title claims description 89
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- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 180
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 174
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 138
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 49
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 42
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 35
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 31
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- 239000010949 copper Substances 0.000 claims description 6
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
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- GOVWJRDDHRBJRW-UHFFFAOYSA-N diethylazanide;zirconium(4+) Chemical compound [Zr+4].CC[N-]CC.CC[N-]CC.CC[N-]CC.CC[N-]CC GOVWJRDDHRBJRW-UHFFFAOYSA-N 0.000 claims description 3
- DWCMDRNGBIZOQL-UHFFFAOYSA-N dimethylazanide;zirconium(4+) Chemical compound [Zr+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C DWCMDRNGBIZOQL-UHFFFAOYSA-N 0.000 claims description 3
- XGSXHQJGLSRGFR-UHFFFAOYSA-N methylcyclopentane;yttrium Chemical compound [Y].C[C]1[CH][CH][CH][CH]1.C[C]1[CH][CH][CH][CH]1.C[C]1[CH][CH][CH][CH]1 XGSXHQJGLSRGFR-UHFFFAOYSA-N 0.000 claims description 3
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- JRCMYZNYPKTOPG-UHFFFAOYSA-N butylcyclopentane;erbium Chemical compound [Er].CCCC[C]1[CH][CH][CH][CH]1.CCCC[C]1[CH][CH][CH][CH]1.CCCC[C]1[CH][CH][CH][CH]1 JRCMYZNYPKTOPG-UHFFFAOYSA-N 0.000 claims description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004841 transmission electron microscopy energy-dispersive X-ray spectroscopy Methods 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 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
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- LSWWNKUULMMMIL-UHFFFAOYSA-J zirconium(iv) bromide Chemical compound Br[Zr](Br)(Br)Br LSWWNKUULMMMIL-UHFFFAOYSA-J 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- C23C16/45531—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making ternary or higher compositions
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
Description
K*[m*(M1+M2+O)+n*(M2+M1+O)]
ここで、Kはゼロより大きい整数であって、目標厚さを達成するために実行されるスーパーサイクルの数を表す。K、m、nを調整することで、前駆体の化学的特性にかかわらず、所望の組成(例えば、第2金属に対する第1金属の所望の比率)のコーティングを達成し得る。
K*[a*(M1+M2+M3+F)+b*(M1+M3+M2+F)+c*(M2+M1+M3+F)+d*(M2+M3+M1+F)+e*(M3+M1+M2+F)+f*(M3+M2+M1+F)]
ここで、a、b、c、d、e、及びfは、負でない整数である。各共堆積法のM1、M2及びM3の各モル数は、実験によって決定されてもよい。同様に、4つの金属の共堆積の場合には、以下の共堆積法を混用して、目標組成のコーティングを達成してもよい。すなわち、M1+M2+M3+M4+F、M1+M3+M4+M2+F、M1+M4+M2+M3+F、M1+M3+M2+M4+F、M1+M4+M3+M2+F、M1+M2+M4+M3+F、M2+M1+M3+M4+F、M2+M3+M4+M1+F、M2+M4+M1+M3+F、M2+M1+M4+M3+F、M2+M3+M1+M4+F、M2+M4+M3+M1+F、M3+M1+M2+M4+F、M3+M2+M4+M1+F、M3+M4+M1+M2+F、M3+M1+M4+M2+F、M3+M2+M1+M4+F、M3+M4+M2+M1+F、M4+M1+M2+M3+F、M4+M2+M3+M1+F、M4+M3+M1+M2+F、M4+M1+M3+M2+F、M4+M2+M1+M3+F、M4+M3+M2+M1+Fである。よって、以下の式を用いて、目標組成を達成してもよい。
K*[a*(M1+M2+M3+M4+F)+b*(M1+M3+M4+M2+F)+c*(M1+M4+M2+M3+F)+d*(M1+M3+M2+M4+F)+e*(M1+M4+M3+M2+F)+f*(M1+M2+M4+M3+F)+g*(M2+M1+M3+M4+F)+h*(M2+M3+M4+M1+F)+i*(M2+M4+M1+M3+F)+j*(M2+M1+M4+M3+F)+k(M2+M3+M1+M4+F)+l*(M2+M4+M3+M1+F)+m*(M3+M1+M2+M4+F)+n*(M3+M2+M4+M1+F)+o*(M3+M4+M1+M2+F)+p*(M3+M1+M4+M2+F)+q*(M3+M2+M1+M4+F)+r*(M3+M4+M2+M1+F)+s*(M4+M1+M2+M3+F)+t*(M4+M2+M3+M1+F)+u*(M4+M3+M1+M2+F)+v*(M4+M1+M3+M2+F)+w*(M4+M2+M1+M3+F)+x*(M4+M3+M2+M1+F)]
ここで、aからxは負でない整数である。
原子層堆積法を用いてチャンバ構成要素に酸化イットリウムコーティングを堆積させた。コーティングされた基板を、450℃の温度で、3,000サイクルの三フッ化窒素(NF3)プラズマに化学気相堆積チャンバ内で曝した。基板上のY2O3コーティングの側断面透過型電子顕微鏡(TEM)像を得た。Y2O3コーティングの透過型電子顕微鏡エネルギー分散型X線分光法(TEM/EDS)ラインスキャンも得られた。Y2O3基板のNF3処理の間に、フッ素(F)のY2O3への制御されない拡散/反応により、コーティング及びその下にある基板は損傷した。フッ素は、(1)コーティングの表面劣化を引き起こし、(2)浸食し、ゆえに粒子を発生させ、(3)コーティングを通って拡散し、(4)コーティングの亀裂及び層間剥離の危険性を増大させた。
Al2O3、Y2O3又はYF3コーティングを有するサンプル切取り試片を、ALD堆積法を用いて作成した。Al2O3コーティングの厚さは500nm、Y2O3コーティングの厚さは100nm、YF3コーティングの厚さは100nmであった。各サンプルを、34RF時間、75℃の温度及び300Wの高周波電源電力でCF4誘導結合プラズマに曝した。
Claims (15)
- 物品であって、
本体と、
本体の表面に希土類金属含有フッ化物コーティングとを備え、
希土類金属含有フッ化物コーティングは、約1mol%から約40mol%の第1金属と、約1mol%から約40mol%の第2金属とを含み、第1金属及び第2金属は独立に、希土類金属、ジルコニウム、ハフニウム、アルミニウム及びタンタルからなる群から選択され、第1金属は第2金属とは異なり、
希土類金属含有フッ化物コーティングは、第1金属と第2金属との均質混合物を含んでいる物品。 - 希土類金属含有フッ化物コーティングは、約5nmから約10μmの厚さを有する、又は
物品は、チャンバ壁、シャワーヘッド、ノズル、プラズマ生成ユニット、高周波電極、電極ハウジング、ディフューザー、ガスラインからなる群から選択される処理チャンバの構成要素である、又は
本体は、アルミニウム、鋼、シリコン、銅及びマグネシウムからなる群から選択される材料を含んでいる、又は
第1金属は、イットリウム、エルビウム、ランタン、ルテチウム、スカンジウム、ガドリニウム、サマリウム及びジスプロシウムからなる群から選択される希土類金属を含んでいる、又は
第1金属はイットリウムを含み、希土類金属含有フッ化物コーティングは、約1mol%から約40mol%の濃度のジルコニウムを含んでいる、又は
希土類金属含有フッ化物コーティングは、YxZryFz、YxZryFz、ErxZryFz、YwZrxHfyFz、ErwZrxHfyFz、YvErwZrxHfyFz、YxHfyFz、ErxHfyFz、YxTayFz、ErxTayFz、YwTaxHfyFz、ErwTaxHfyFz及びYvErwTaxHfyFzからなる群から選択される組成を含んでいる、請求項1に記載の物品。 - 本体の表面上のバッファ層をさらに備え、希土類金属含有フッ化物コーティングはバッファ層を覆い、バッファ層は、酸化アルミニウム、酸化シリコン及び窒化アルミニウムからなる群から選択される材料を含んでいる、請求項1に記載の物品。
- 原子層堆積法を使用して、物品の表面に希土類金属含有フッ化物コーティングを共堆積させる工程を含む方法であって、
希土類金属含有フッ化物コーティングを共堆積させる工程は、
第1期間の間に表面を第1金属含有前駆体又は第2金属含有前駆体と接触させて、第1金属(M1)又は第2金属(M2)を含む部分的金属吸着層を形成する工程であって、第1金属含有前駆体又は第2金属含有前駆体は、希土類金属含有前駆体、ジルコニウム含有前駆体、ハフニウム含有前駆体、アルミニウム含有前駆体、及びタンタル含有前駆体からなる群から選択される工程と、
第2期間の間に部分的金属吸着層を第2金属含有前駆体又は第1金属含有前駆体と接触させて、第1金属(M1)と第2金属(M2)とを含む共吸着層を形成する工程であって、第1金属は第2金属とは異なっている工程と、
共吸着層を反応物質と接触させて、希土類金属含有フッ化物コーティングを形成する工程とを含み、
希土類金属含有フッ化物コーティングは、約1mol%から約40mol%の第1金属と、約1mol%から約40mol%の第2金属とを含み、
希土類金属含有フッ化物コーティングは、第1金属と第2金属との均質混合物を含んでいる方法。 - 希土類金属含有フッ化物コーティングを共堆積させる工程は、
少なくとも1回のM1−M2共堆積サイクルを実行する工程であって、
表面を第1金属含有前駆体と接触させて、部分的金属吸着層を形成する工程と、
続いて、部分的金属吸着層を第2金属含有前駆体と接触させて、M1−M2共吸着層を形成する工程と、
M1−M2共吸着層を反応物質と接触させる工程とを含む工程を含み、
少なくとも1回のM1−M2共堆積サイクルにより、第1割合の第1金属と第2割合の第2金属とを含む層が得られている、請求項4に記載の方法。 - 希土類金属含有フッ化物コーティングを共堆積させる工程は、
少なくとも1回のM2−M1共堆積サイクルを実行する工程であって、
表面を第2金属含有前駆体と接触させて、第2部分的金属吸着層を形成する工程と、
続いて、第2部分的金属吸着層を第1金属含有前駆体と接触させて、M2−M1共吸着層を形成する工程と、
M2−M1共吸着層を反応物質と接触させる工程とを含む工程をさらに含み、
少なくとも1回のM2−M1共堆積サイクルにより、第3割合の第1金属と第4割合の第2金属とを含む追加層が得られ、第3割合は第1割合よりも低く、第4割合は第2割合よりも高くなっている、請求項5に記載の方法。 - M1−M2共堆積サイクルの第1回数とM2−M1共堆積サイクルの第2回数の比を選択する工程であって、選択の結果として、第1金属の第1目標mol%及び第2金属の第2目標mol%が得られる工程と、
複数の堆積スーパーサイクルを実行する工程であって、各堆積スーパーサイクルは、第1回数のM1−M2共堆積サイクルを実行する工程と、第2回数のM2−M1共堆積サイクルを実行する工程とを含んでいる工程とをさらに含む、請求項6に記載の方法。 - 少なくとも1回のM1−M2共堆積サイクルを実行する工程は、
表面を第1金属含有前駆体と約50ミリ秒から約60秒の間、接触させる工程と、
部分的金属吸着層を第2金属含有前駆体と約50ミリ秒から約60秒の間、接触させる工程と、
M1−M2共吸着層を反応物質と約50ミリ秒から約60秒の間、接触させる工程とを含み、
少なくとも1回のM2−M1共堆積サイクルを実行する工程は、
表面を第2金属含有前駆体と約50ミリ秒から約60秒の間、接触させる工程と、
第2部分的金属吸着層を第1金属含有前駆体と約50ミリ秒から約60秒の間、接触させる工程と、
M2−M1共吸着層を反応物質と約50ミリ秒から約60秒の間、接触させる工程とを含んでいる、請求項6に記載の方法。 - 第1金属含有前駆体及び第2金属含有前駆体は独立に、シクロペンタジエニル系前駆体、トリス(メチルシクロペンタジエニル)イットリウム((CH3Cp)3Y)、トリス(ブチルシクロペンタジエニル)イットリウム、トリス(シクロペンタジエニル)イットリウム、トリス(エチルシクロペンタジエニル)イットリウム、トリス−メチルシクロペンタジエニルエルビウム(III)(Er(MeCp)3)、トリス(ブチルシクロペンタジエニル)エルビウム(III)、アミジナート系前駆体、トリス(N,N’−ジイソプロピルホルムアミジナート)イットリウム、トリス(2,2,6,6−テトラメチル−ヘプタン−3,5−ジオナート)イットリウム、トリス(ビス(トリメチルシリル)アミド)ランタン)、アミド系前駆体、エルビウムボランアミド(Er(BA)3)、β−ジケトナート系前駆体、エルビウム(III)、トリス(2,2,6,6−テトラメチル−3,5−ヘプタンジオナート)、トリス(ジメチルアミノ)(シクロペンタジエニル)ジルコニウム、テトラキス(ジメチルアミド)ジルコニウム、テトラキス(ジエチルアミド)ジルコニウム、テトラキス(N,N’−ジメチルホルムアミジナート)ジルコニウム、テトラ(エチルメチルアミド)ハフニウム、及びペンタキス(ジメチルアミド)タンタルからなる群から選択される、請求項4に記載の方法。
- 共吸着層を第3前駆体と接触させて、第3金属を吸着した後に、共吸着層を反応物質と接触させる工程であって、第3前駆体は、イットリウム前駆体、エルビウム前駆体、ジルコニウム前駆体、ハフニウム前駆体、シリコン前駆体、タンタル前駆体、ランタン前駆体、ルテチウム前駆体、スカンジウム前駆体、ガドリニウム前駆体、サマリウム前駆体、ジスプロシウム前駆体からなる群から選択されている工程をさらに含む、請求項4に記載の方法。
- 物品の表面に原子層堆積法によってバッファ層を堆積する工程と、希土類金属含有コーティングをバッファ層上に共堆積する工程とをさらに含み、バッファ層は、酸化アルミニウム、酸化シリコン、又は窒化アルミニウムのうちの少なくとも1つを含んでいる、請求項4に記載の方法。
- 希土類金属含有フッ化物コーティングは、YxZryFz、YxEryFz、ErxZryFz、LaxZryFz、LuxZryFz、ScxZryFz、GdxZryFz、SmxZryFz、DYxZryFz、YxHfyFz、ErxHfyFz、LaxHfyFz、LuxHfyFz、ScxHfyFz、GdxHfyFz、SmxHfyFz、DYxHfyFz及びそれらの組み合わせからなる群から選択される組成を含んでいる、請求項4に記載の方法。
- 原子層堆積法を使用して、物品の表面に希土類金属含有フッ化物コーティングを共堆積させる工程を含む方法であって、
希土類金属含有フッ化物コーティングを共堆積させる工程は、
少なくとも1回の共注入サイクルを実行する工程であって、
第1期間の間に表面を、第1前駆体及び第2前駆体の混合物と接触させて、共吸着層を形成する工程であって、第1前駆体及び第2前駆体はそれぞれ、希土類金属含有前駆体、ジルコニウム含有前駆体、ハフニウム含有前駆体、アルミニウム含有前駆体、及びタンタル含有前駆体からなる群から選択されている工程と、
共吸着層をフッ素含有反応物質と接触させて、希土類金属含有フッ化物コーティングを形成する工程とを含む工程を含み、
希土類金属含有フッ化物コーティングは、約1mol%から約40mol%の第1金属と、約1mol%から約40mol%の第2金属とを含み、第1金属及び第2金属は独立に、希土類金属、ジルコニウム、ハフニウム、アルミニウム及びタンタルからなる群から選択され、第1金属は第2金属とは異なり、
希土類金属含有フッ化物コーティングは、第1金属と第2金属の均質混合物を含んでいる方法。 - 混合物は、第1前駆体の第1金属及び第2前駆体の第2金属とは異なる金属を含む第3前駆体をさらに含み、第3前駆体の金属は、イットリウム、エルビウム、ランタン、ルテチウム、スカンジウム、ガドリニウム、サマリウム、ジスプロシウム、ジルコニウム、ハフニウム及びタンタルからなる群から選択され、均質混合物はさらに第3前駆体の金属を含んでいる、請求項13に記載の方法。
- 原子層堆積法を用いて、物品の表面に希土類金属含有フッ化物コーティングを堆積させる工程を含む方法であって、
希土類金属含有フッ化物コーティングを堆積する工程は、
第1期間の間に表面を第1前駆体と接触させて、第1金属吸着層を形成する工程と、
第1金属吸着層をフッ素含有反応物質と接触させて、第1金属フッ化物層を形成する工程と、
第2期間の間に第1金属層を第2前駆体と接触させて、第2金属吸着層を形成する工程と、
第2金属吸着層を前記フッ素含有反応物質又は代替のフッ素含有反応物質と接触させて、第2金属フッ化物層を形成する工程と、
第1金属フッ化物層及び第2金属フッ化物層から希土類金属含有フッ化物コーティングを形成する工程とを含み、
希土類金属含有フッ化物コーティングは、約1mol%から約40mol%の第1金属と、約1mol%から約40mol%の第2金属とを含み、第1金属及び第2金属は独立に、希土類金属、ハフニウム及びタンタルからなる群から選択され、第1金属は第2金属とは異なっている方法。
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