JP6956086B2 - コバルト含有フィルム形成組成物、それらの合成およびフィルム析出における使用 - Google Patents
コバルト含有フィルム形成組成物、それらの合成およびフィルム析出における使用 Download PDFInfo
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- JP6956086B2 JP6956086B2 JP2018530087A JP2018530087A JP6956086B2 JP 6956086 B2 JP6956086 B2 JP 6956086B2 JP 2018530087 A JP2018530087 A JP 2018530087A JP 2018530087 A JP2018530087 A JP 2018530087A JP 6956086 B2 JP6956086 B2 JP 6956086B2
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- containing film
- film
- silylamide
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Images
Classifications
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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Description
本出願は、全ての目的のために、参照によって全体として本明細書に組み込まれる、2015年12月31日出願の米国特許出願第14/986,286号明細書の利益を請求する。
●各R1、R2およびR3は、H、メチル、エチル、イソプロピル、n−プロピル、n−ブチルまたはt−ブチルから独立して選択され;
●シリルアミド含有前駆体は、{Co[N(SiMe3)2]2}2であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(py)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(Me3N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(Et3N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(Me2EtN)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(MeEt2N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(1−Me−ピロリジン)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(PMe3)であり;
●シリルアミド含有前駆体は、{Co[N(SiMe2Et)2]2}2であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(py)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(Me3N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(Et3N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(Me2EtN)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(MeEt2N)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(1−Me−ピロリジン)であり;
●シリルアミド含有前駆体は、Co[N(SiMe2Et)2]2(PMe3)であり;
●コバルト含有フィルム形成組成物は、約99%w/w〜約100%w/wのシリルアミド含有前駆体を含んでなり;
●コバルト含有フィルム形成組成物は、50℃において4週間後、約99%w/w〜約100%w/wのシリルアミド含有前駆体を含んでなり;
●コバルト含有フィルム形成組成物は、室温(約23℃)において12週間後、約99%w/w〜約100%w/wのシリルアミド含有前駆体を含んでなり;
●コバルト含有フィルム形成組成物は、1トルのシリルアミド含有前駆体の蒸気圧を生じる温度における2週間の安定性試験後の熱重量分析下で3%未満の残渣質量を生じ;
●コバルト含有フィルム形成組成物は、1トルのシリルアミド含有前駆体の蒸気圧を生じる温度における3週間の安定性試験後の熱重量分析下で3%未満の残渣質量を生じ;
●コバルト含有フィルム形成組成物は、1トルのシリルアミド含有前駆体の蒸気圧を生じる温度における2カ月間の安定性試験後の熱重量分析下で3%未満の残渣質量を生じ;
●コバルト含有フィルム形成組成物は、約95%w/w〜約100%w/wのシリルアミド含有前駆体を含んでなり;
●Co含有フィルム形成組成物は、約5%w/w〜約50%w/wのシリルアミド含有前駆体を含んでなり;
●Co含有フィルム形成組成物は、水を含まず;
●Co含有フィルム形成組成物は、約0%w/w〜約5%w/wの不純物を含んでなり;
●Co含有フィルム形成組成物は、約0.0%w/w〜約2.0%w/wの不純物を含んでなり;
●Co含有フィルム形成組成物は、約0.0%w/w〜約1.0%w/wの不純物を含んでなり;
●不純物は、ハロゲン化物、アルカリ金属、アリル置換シラン、リチウム、ナトリウムまたはカリウムハロゲン化物;THF;エーテル;ペンタン;シクロヘキサン;ヘプタン;ベンゼン;トルエンを含み;
●Co含有フィルム形成組成物は、約0ppbw〜約1ppmwの金属不純物を含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約500ppbwの金属不純物を含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのAlを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのAsを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのBaを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのBeを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのBiを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのCdを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのCaを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのCrを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのCuを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのGaを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのGeを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのHfを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのZrを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのInを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのFeを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのPbを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのLiを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのMgを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのMnを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのWを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのNiを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのKを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのNaを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのSrを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのThを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのSnを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのTiを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのUを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのVを含んでなり;
●Co含有フィルム形成組成物は、約0ppbw〜約100ppbwのZnを含んでなり;
●Co含有フィルム形成組成物は、約0ppmw〜約100ppmwのClを含んでなり;
●Co含有フィルム形成組成物は、約0ppmw〜約100ppmwのBrを含んでなる。
●Co含有フィルム形成組成物は、10ppmw未満の金属汚染物全濃度を有し;
●入口導管の端部は、Co含有フィルム形成組成物の表面上に配置され、かつ出口導管の端部は、Co含有フィルム形成組成物の表面下に配置され;
●入口導管の端部はCo含有フィルム形成組成物の表面下に配置され、かつ出口導管の端部は、Co含有フィルム形成組成物の表面上に配置され;
●入口および出口上にダイヤフラムバルブをさらに含んでなり;
●キャニスターの内面上に1層またはそれ以上のバリア層をさらに含んでなり;
●キャニスターの内面上に1〜4層のバリア層をさらに含んでなり;
●キャニスターの内面上に1層または2層のバリア層をさらに含んでなり;
●各バリア層が、酸化ケイ素層、窒化ケイ素層、酸窒化ケイ素層、炭窒化ケイ素層、酸炭窒化ケイ素層またはその組合せを含んでなり;
●各バリア層が、1〜100nmの厚さであり;
●各バリア層が、2〜10nmの厚さであり;
●Co含有フィルム形成組成物が、Co[N(SiMe3)2]2(NMe2Et)を含んでなり;
●Co含有フィルム形成組成物が、Co[N(SiMe3)2]2(NMeEt2)を含んでなる。
●Co含有フィルム形成組成物は、Co[N(SiMe3)2]2(NMe2Et)、Co[N(SiMe3)2]2(NMeEt2)またはその組合せから選択されるシリルアミド含有前駆体を含んでなり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(NMe2Et)であり;
●シリルアミド含有前駆体は、Co[N(SiMe3)2]2(NMeEt2)であり;
●第2の前駆体を含んでなる蒸気を反応器に導入し;
●第2の前駆体の元素が、第2族、第13族、第14族、遷移金属、ランタノイドおよびその組合せからなる群から選択され;
●第2の前駆体の元素が、Mg、Ca、Sr、Ba、Zr、Hf、Ti、Nb、Ta、
Al、Si、Ge、Yまたはランタノイドから選択され;
●反応物を反応器に導入し;
●反応物が、O2、O3、H2O、H2O2、NO、NO2、カルボン酸、そのラジカルおよびその組合せからなる群から選択され;
●反応物が、プラズマ処理酸素であり;
●反応物が、オゾンであり;
●反応物が、H2、NH3、(SiH3)3N、(SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12などの)ヒドリドシラン、(SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8などの)クロロシランおよびクロロポリシラン、(Me2SiH2、Et2SiH2、MeSiH3、EtSiH3などの)アルキルシラン、(N2H4、MeHNNH2、MeHNNHMeなどの)ヒドラジン、(エタノールまたはメタノールなどの)アルコール、(NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NHなどの)有機アミン、ピラゾリン、ピリジン、(B2H6、9−ボラビシクロ[3,3,1]ノナン、トリメチルボロン、トリエチルボロン、ボラジンなどの)B含有分子、(トリメチルアルミニウム、トリエチルアルミニウム、ジメチル亜鉛、ジエチル亜鉛などの)アルキル金属、そのラジカル種およびその混合物からなる群から選択され;
●反応物が、H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、その水素ラジカルおよびその混合物からなる群から選択され;
●反応物が、NH3、N2H4、N(SiH3)3、N(CH3)H2、N(C2H5)H2、N(CH3)2H、N(C2H5)2H、N(CH3)3、N(C2H5)3、(SiMe3)2NH、(CH3)HNNH2、(CH3)2NNH2、その窒素含有ラジカル種およびその混合物からなる群から選択され;
●反応物が、HCDSまたはPCDSであり;
●反応物が、プラズマ処理N2であり;
●蒸着法が、化学蒸着(CVD)プロセスであり;
●蒸着法が、ALDプロセスであり;
●蒸着法が、PEALDプロセスであり;
●蒸着法が、空間的ALDプロセスであり;
●Co含有層が、酸化コバルト層であり;
●Co含有層が、窒化コバルト層であり;
●Co含有層が、Coであり;かつ
●Co含有層が、CoSiである。
特定の略語、記号および用語は、次の明細および請求項全体で使用され、かつ次のものを含む:
チタン(Ti)、ウラン(U)、バナジウム(V)および亜鉛(Zn)が含まれる。精製されたCo含有フィルム形成組成物中のX(X=Cl、Brである)の濃度は、約0ppmw〜約100ppmw、より好ましくは、約0ppmw〜10ppmwの範囲であり得る。
、H2O、H2O2の1つなどの酸素;O・またはOH ・ などの酸素含有ラジカル;ギ酸、酢酸、プロピオン酸などのカルボン酸、NO、NO2またはカルボン酸のラジカル種;パラホルムアルデヒド;およびその混合物を含有し得る。好ましくは、酸素含有反応物は、O2、O3、H2O、H2O2、O・またはOH・などのその酸素含有ラジカル、ならびにその混合物からなる群から選択される。好ましくは、ALDプロセスが実行される場合、反応物は、プラズマ処理酸素、オゾンまたはその組合せである。酸素含有反応物が使用される場合、得られるコバルト含有フィルムも酸素を含有するであろう。
フラスコに、CoCl2(7.08g)およびTHF(50ml)を充てんした。−78℃でNaN(SiMe3)2 THF溶液(100mL)を滴下し、次いで、混合物を室温(約23℃、RT)まで加温した。室温での一晩の反応後、溶液をCelite(商標)ブランド珪藻土を通してろ過し、そして全ての溶媒を減圧下で除去した。減圧(50ミリトル、70〜80℃)下での昇華によって、薄緑色の化合物を精製した。収率58%。XRD分析のために、生成物を−30℃においてヘキサンから再結晶化した。空気感応性の若草色の結晶が得られた。
1H NMR(δ,C6D6)−16.98(s)96.91(brs),DSC 58℃(融点),183℃(分解),蒸気圧 108℃で1トル.
フラスコに、CoCl2およびTHFを充てんした。−78℃でNaN(SiMe2Et)2 THF溶液を滴下し、次いで、混合物を室温(約23℃、RT)まで加温した。濃緑色の液体が得られた。
1H NMR(δ,C6D6)−34.69(s),−19.67(s)2.11(brs)89.12(brs),DSC 215℃(分解),蒸気圧 100℃で1トル.
10等量の付加物配位子(乾燥ピリジン(py.)、ジメチルエチルアミン、ジエチルメチルアミン、トリエチルアミン、1−メチル−ピロリジン)を、窒素下、実施例1と同様に調整されたCo[N(SiMe3)2]2(THF)(1.0g)のヘキサン溶液(5mL)中に滴下した。一晩の反応後、溶媒および過剰量の付加物配位子を減圧下で除去した。粗製生成物を乾燥ヘキサンで抽出し、そしてPTFEフィルターを通してろ過した。標的化合物は、−30℃での乾燥ヘキサンからの再結晶化によって精製し、そして室温で減圧下、乾燥させた。それぞれの付加化合物は、青色〜緑色固体として単離された。ピリジン付加物(水色、収率78%)、ジメチルエチルアミン付加物(青色、収率87%)、ジエチルメチルアミン付加物(濃緑色、収率56%)、トリエチルアミン付加物(濃緑色、収率93%)、1−メチル−ピロリジン付加物(水色、収率86%)。
Py付加物:1H NMR(δ,C6D6)−18.84(s)67.04(brs),138.66(brs),DSC 100℃(m.p.),216℃(dec),蒸気圧 153℃で1トル.
ジメチルエチルアミン付加物 1H NMR(δ,C6D6)−24.91(s)71.77(brs),DSC 88℃(m.p.),203℃(dec),蒸気圧 88℃で1トル.
ジエチルメチルアミン付加物 1H NMR(δ,C6D6)−22.58(brs),59.40(brs),97.71(brs)DSC 90℃(m.p.),210℃(dec),蒸気圧 82℃で1トル.
トリエチルアミン付加物1H NMR(δ,C6D6)−17.01(s),96.68(brs),DSC 221℃(dec),蒸気圧 100℃で1トル.
1−メチル−ピロリジン付加物 1H NMR(δ,C6D6)−25.07(s),62.06(brs),76.22(brs),DSC 148℃(m.p.),210℃(dec),蒸気圧 114℃で1トル.
10等量のジメチルエチルアミンを、窒素下、実施例2と同様に調整されたCo[N(SiMe2Et)2]2(THF)(1.0g)のヘキサン溶液(5mL)中に滴下した。一晩の反応後、溶媒および過剰量の付加物配位子を減圧下で除去した。粗製生成物を乾燥ヘキサンで抽出し、そしてPTFEフィルターを通してろ過した。標的化合物は、減圧(30ミリトル)下での蒸留によって精製した。濃緑色液体が得られた(収率45%)。
1H NMR(δ,C6D6)−20.45(brs),−16.20(s),0.07(s)0.50(q,J=8Hz),0.96(t,J=8Hz),12.75(brs)94.02(brs).DSC 124℃(dec),蒸気圧 124℃で1トル.
窒素(220sccm)下、TGA(熱重量分析、METTLER、TGA/SDTA851)によって揮発度を監視した。温度は10℃/分で増加させた。試験試料を窒素下、アルミパン中で調製した。結果を図4および5に示す。
2週間〜3カ月、1トルの蒸気圧に相当する温度で試料を加熱した。特定の温度で維持された試料に対する、特定の期間でのいずれかの変化を示す1010ミリバール(大気圧)で実行されたTGAグラフを図6〜10に示す。図6は、150℃で0および1週間のCo[N(SiMe3)2]2(py)の結果を示す。図7は、90℃で0;1、2および3週間ならびに1および2カ月のCo[N(SiMe3)2]2(NMe2Et)の結果を示す。図8は、80℃で0、1、2および3週間のCo[N(SiMe3)2]2(NEt2Me)の結果を示す。図9は、110℃で0、1および2週間のCo[N(SiMe3)2]2(1−Me−ピロリジン)の結果を示す。図10は、120℃で0、1および2週間のCo[N(SiMe2Et)2]2(NMe2Et)の結果を示す。
Claims (14)
- 基体上にCo含有層を析出する方法であって、
Co[N(SiMe3)2]2(NMe2Et)、Co[N(SiMe3)2]2(NMeEt2)またはその組合せから選択されるシリルアミド含有前駆体を含んでなるCo含有フィルム形成組成物の蒸気を、その中に基体が配置された反応器中に導入することと、
蒸着法を使用して、前記シリルアミド含有前駆体の少なくとも一部を前記基体上に析出させ、前記Co含有層を形成することと
を含んでなる方法。 - 前記シリルアミド含有前駆体がCo[N(SiMe3)2]2(NMe2Et)である、請求項1に記載の方法。
- 前記シリルアミド含有前駆体がCo[N(SiMe3)2]2(NMeEt2)である、請求項1に記載の方法。
- 前記Co含有層がCoである、請求項1〜3のいずれか一項に記載の方法。
- 前記Co含有層がCoSi2である、請求項1〜3のいずれか一項に記載の方法。
- 前記基体がSiO2である、請求項4または5に記載の方法。
- 前記基体がSiである、請求項5に記載の方法。
- 基体上にCo含有層を析出する方法であって、
Co[N(SiMe3)2]2(NMe2Et)、Co[N(SiMe3)2]2(NMeEt2)またはその組合せから選択されるシリルアミド含有前駆体を含んでなるCo含有フィルム形成組成物を含んでなるCo含有フィルム形成組成物デリバリーデバイスを
蒸着チャンバーに流体連結することと、
前記Co含有フィルム形成組成物デリバリーデバイスを、約0.2トル(約27パスカル)〜約1.5トル(約200パスカル)の前記Co含有フィルム形成組成物の蒸気圧を発生する温度まで加熱することと;
Co含有フィルム形成組成物の蒸気を、その中に基体が配置された前記蒸着チャンバー中に送達することと、
蒸着法を使用して、前記シリルアミド含有前駆体の少なくとも一部を前記基体上に析出させ、前記Co含有層を形成することと
を含んでなる方法。 - 前記Co含有フィルム形成組成物デリバリーデバイスを、前記温度に、2週間〜12カ月の期間維持することをさらに含んでなる、請求項8に記載の方法。
- 前記シリルアミド含有前駆体がCo[N(SiMe3)2]2(NMe2Et)である、請求項8または9に記載の方法。
- Co[N(SiMe3)2]2(NMe2Et)、Co[N(SiMe3)2]2(NMeEt2)またはその組合せから選択されるシリルアミド含有前駆体を含んでなり、かつ80℃において2週間後に残渣質量が5%未満の熱重量分析によって実証された熱安定性を有するコバルト含有フィルム形成組成物。
- 前記シリルアミド含有前駆体がCo[N(SiMe3)2]2(NMe2Et)であり、かつ90℃において2カ月後に残渣質量が5%未満の熱重量分析によって実証された熱安定性を有する、請求項11に記載のコバルト含有フィルム形成組成物。
- 前記Co含有フィルム形成組成物が、Co[N(SiMe3)2]2(NMe2Et)、Co[N(SiMe3)2]2(NMeEt2)またはその組合せから選択されるシリルアミド含有前駆体から本質的になる、請求項11に記載のコバルト含有フィルム形成組成物。
- 前記Co含有フィルム形成組成物が、Co[N(SiMe3)2]2(NMe2Et)から本質的になる、請求項11に記載のコバルト含有フィルム形成組成物。
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