JP6735163B2 - バナジウム化合物、薄膜形成用原料及び薄膜の製造方法 - Google Patents
バナジウム化合物、薄膜形成用原料及び薄膜の製造方法 Download PDFInfo
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- C23C16/45523—Pulsed gas flow or change of composition over time
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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
- C23C16/06—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 metallic material
- C23C16/18—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 metallic material from metallo-organic compounds
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
- H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
- H01L21/28562—Selective deposition
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- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76841—Barrier, adhesion or liner layers
Description
また、堆積速度は、原料の供給条件(気化温度、気化圧力)、反応温度、反応圧力によりコントロールすることができる。堆積速度は、大きいと得られる薄膜の特性が悪化する場合があり、小さいと生産性に問題を生じる場合があるので、0.01〜100nm/分が好ましく、1〜50nm/分がより好ましい。また、ALD法の場合は、所望の膜厚が得られるようにサイクルの回数でコントロールされる。
300ml4つ口フラスコに、塩化バナジウム(III)10.2g(0.0646mol)とテトラヒドロフラン52gを仕込み、室温下で撹拌した。その中に、N,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン32.6g(0.194mol)とリチウム1.35g(0.194mol)をテトラヒドロフラン110gへ溶かして調整した溶液を、ドライアイス−イソプロピルアルコール冷却下、液温−20〜−15℃で滴下した。滴下終了後、80℃加熱下で撹拌した後、微減圧下、オイルバス温度60℃にて脱溶媒を行なった。この残渣をトルエンに溶解させ、ろ過を行なった。得られたトルエン溶液を、減圧下、オイルバス温度100℃にて脱溶媒し、残渣を20Pa、160℃の条件下で蒸留精製して、目的物を得た。収量は17.1gであり、収率は68.4%であった。得られた目的物を大気中で放置することで自然発火性の有無を確認したところ、自然発火性は無かった。
(1)元素分析 V: 13.0質量%、C:61.1質量%、H:11.1質量%、N:14.4質量%)
(理論値 V: 13.1質量%、C:61.4質量%、H:11.3質量%、N:14.3質量%)
(2)常圧TG−DTA
質量50%減少温度:231℃(Ar流量:100ml/分、昇温10℃/分)
(3)減圧TG−DTA
質量50%減少温度: 151℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
300ml4つ口フラスコに、塩化バナジウム(III)3.54g(0.0225mol)とテトラヒドロフラン20gを仕込み、室温下で撹拌した。その中に、N,N’−ジ−tert−アミル−1,4−ジアザ−1,3−ブタジエン13.3g(0.0675mol)とリチウム0.47g(0.0675mol)をテトラヒドロフラン30gへ溶かして調整した溶液を、ドライアイス−イソプロピルアルコール冷却下、液温−20〜−15℃で滴下した。滴下終了後、80℃加熱下で撹拌した後、微減圧下、オイルバス温度60℃にて脱溶媒を行なった。この残渣をトルエンに溶解させ、ろ過を行なった。得られたトルエン溶液を、減圧下、オイルバス温度100℃にて脱溶媒し、残渣を15Pa、125℃の条件下で蒸留精製して、目的物を得た。収量は3.56gであり、収率は35.6%であった。得られた目的物を大気中で放置することで自然発火性の有無を確認したところ、自然発火性は無かった。
(1)元素分析 V: 11.6質量%、C:64.5質量%、H:10.9質量%、N:12.4質量%)
(理論値 V: 11.5質量%、C:64.4質量%、H:11.7質量%、N:12.5質量%)
(2)常圧TG−DTA
質量50%減少温度:263℃(Ar流量:100ml/分、昇温10℃/分)
(3)減圧TG−DTA
質量50%減少温度: 180℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
化合物No.5及び6並びに下記に示す比較化合物1について、DSC測定装置を用いて発熱ピークの温度を熱分解温度として測定することで、各化合物の熱安定性を確認した。結果を表2に示す。
化合物No.5及び6を化学気相成長用原料とし、図1に示すALD装置を用いて以下の条件のALD法により、シリコン基板上に窒化バナジウム薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は3〜6nmであり、膜組成は窒化バナジウム(XPS分析によるV2pピーク、N1sピークで確認)であった。炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。また、得られた窒化バナジウムの断面を観察したところ、化合物No.5を用いて製造した薄膜は、化合物No.6を用いて製造した薄膜よりも薄膜全体の膜厚のばらつきが非常に少なかった。
反応温度(基板温度):320℃、反応性ガス:アンモニアガス
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、150サイクル繰り返した。
(1)原料容器加熱温度70℃、原料容器内圧力100Paの条件で気化させた化学気相成長用原料の蒸気を導入し、系圧100Paで30秒間堆積させる。
(2)10秒間のアルゴンパージにより、未反応原料を除去する。
(3)反応性ガスを導入し、系圧力100Paで30秒間反応させる。
(4)10秒間のアルゴンパージにより、未反応原料を除去する。
比較化合物1を用いて、実施例3と同様の方法で窒化バナジウム薄膜を製造した。この結果、シリコン基板上に形成されたバナジウム含有薄膜中の炭素含有量は20atom%以上であった。
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JP2016123398A JP6735163B2 (ja) | 2016-06-22 | 2016-06-22 | バナジウム化合物、薄膜形成用原料及び薄膜の製造方法 |
PCT/JP2017/018235 WO2017221586A1 (ja) | 2016-06-22 | 2017-05-15 | バナジウム化合物、薄膜形成用原料及び薄膜の製造方法 |
US16/308,900 US10882874B2 (en) | 2016-06-22 | 2017-05-15 | Vanadium compound |
KR1020197000881A KR102280110B1 (ko) | 2016-06-22 | 2017-05-15 | 바나듐 화합물, 박막 형성용 원료 및 박막의 제조 방법 |
EP17815056.1A EP3476827B1 (en) | 2016-06-22 | 2017-05-15 | Vanadium compound, starting material for thin film formation, and method for producing thin film |
TW106117423A TWI713747B (zh) | 2016-06-22 | 2017-05-25 | 釩化合物、薄膜形成用原料及薄膜之製造方法 |
IL263665A IL263665B (en) | 2016-06-22 | 2018-12-12 | Vanadium compound, raw material for forming thin film, and method for manufacturing thin film |
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KR (1) | KR102280110B1 (ja) |
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TW202140831A (zh) * | 2020-04-24 | 2021-11-01 | 荷蘭商Asm Ip私人控股有限公司 | 形成含氮化釩層及包含該層的結構之方法 |
KR20240021770A (ko) * | 2021-04-23 | 2024-02-19 | 버슘머트리얼즈 유에스, 엘엘씨 | 바나듐-함유 막의 증착 |
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RS61699B1 (sr) * | 2014-11-25 | 2021-05-31 | Versalis Spa | Fosfinski kompleks vanadijuma, katalitički sistem koji sadrži navedeni fosfinski kompleks vanadijuma i postupak za (ko)polimerizaciju konjugovanih diena |
JP6465699B2 (ja) | 2015-03-06 | 2019-02-06 | 株式会社Adeka | ジアザジエニル化合物、薄膜形成用原料、薄膜の製造方法及びジアザジエン化合物 |
JP6675159B2 (ja) | 2015-06-17 | 2020-04-01 | 株式会社Adeka | 新規な化合物、薄膜形成用原料及び薄膜の製造方法 |
CN108064225A (zh) | 2015-06-18 | 2018-05-22 | 英特尔公司 | 用于第二或第三行过渡金属薄膜的沉积的固有地选择性前驱体 |
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KR20190020738A (ko) | 2019-03-04 |
EP3476827A4 (en) | 2019-12-25 |
KR102280110B1 (ko) | 2021-07-20 |
TW201815803A (zh) | 2018-05-01 |
WO2017221586A1 (ja) | 2017-12-28 |
TWI713747B (zh) | 2020-12-21 |
US20190177346A1 (en) | 2019-06-13 |
JP2017226614A (ja) | 2017-12-28 |
EP3476827A1 (en) | 2019-05-01 |
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US10882874B2 (en) | 2021-01-05 |
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