JPWO2015093389A1 - 酸化物薄膜の形成方法および装置 - Google Patents
酸化物薄膜の形成方法および装置 Download PDFInfo
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- JPWO2015093389A1 JPWO2015093389A1 JP2015553507A JP2015553507A JPWO2015093389A1 JP WO2015093389 A1 JPWO2015093389 A1 JP WO2015093389A1 JP 2015553507 A JP2015553507 A JP 2015553507A JP 2015553507 A JP2015553507 A JP 2015553507A JP WO2015093389 A1 JPWO2015093389 A1 JP WO2015093389A1
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- Prior art keywords
- thin film
- gas
- oxide thin
- forming
- reaction vessel
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- 239000001301 oxygen Substances 0.000 claims abstract description 34
- NPEOKFBCHNGLJD-UHFFFAOYSA-N ethyl(methyl)azanide;hafnium(4+) Chemical compound [Hf+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C NPEOKFBCHNGLJD-UHFFFAOYSA-N 0.000 claims abstract description 31
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- SRLSISLWUNZOOB-UHFFFAOYSA-N ethyl(methyl)azanide;zirconium(4+) Chemical compound [Zr+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C SRLSISLWUNZOOB-UHFFFAOYSA-N 0.000 claims abstract description 10
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
ハフニウム酸化物膜を原子層堆積法で形成するためには、原料ガスとしてテトラキス(エチルメチルアミノ)ハフニウム(Hf[NCH3C2H5]4)を用いる。ジルコニウム酸化物薄膜を形成積層するには、原料ガスとしてハフニウム原料と全く同じ分子構造とほぼ近い物性をもつテトラキス(エチルメチルアミノ)ジルコニウム(Zr[NCH3C2H5]4)を用いる。以降、ハフニウム酸化物薄膜を例に説明するが、ジルコニウム酸化物薄膜では、原料以外全く同じ手順で行うことができる。
M−M + O → M−O−M
M−O−M + H + OH → 2M−OH
が起きる。仮に被処理材が有機ポリマーである場合、そこに含まれるアルキル基が次のような反応をとおして、部分酸化され、表面にハイドロキシル基ができる。
−・・CH3 + O → −・・CH2OH
本実施例においては、原料ガスとしてテトラキス(エチルメチルアミノ)ハフニウムを用いた。HfO2膜を被処理基板3の表面に形成を試みた。被処理基板3の温度は23℃とした。被処理基板3にシリコン単結晶板を用い、面方位は(100)のものを用いた。成膜の手順であるが、最初の表面処理として、反応容器1にプラズマガスを導入した。このとき、プラズマガスの導入時間は5分とした。プラズマガスの発生方法であるが、図2に示される装置を用い、水バブラー11に酸素ガスを7sccmの流量で流し、このとき水バブラー11中の水の温度を60℃とすることで、加湿された酸素ガスを作り、続いてガラス管13の中で、誘導コイル14でプラズマを発生させて、水蒸気と酸素の混合ガスをプラズマ化し、活性化させた。誘導コイル14に導入される高周波電力は20Wとした。このときに、被処理基板3の表面は酸化され、このときに油脂汚れが除去され、表面にはハイドロキシル基が形成される。これにより、その後テトラキス(エチルメチルアミノ)ハフニウムを導入した時の、吸着確率を高めることができる。
実施例1とほぼ同じ手順で、プラズマガスの発生方法であるが、図2に示される装置を用い、水バブラー11に酸素の代わりにアルゴンを流し、加湿したアルゴンを励起させて反応容器に導入する手順で試験を行ったところ、100サイクルのALDサイクルを行っても、被処理基板からハフニウム酸化物を検出することができなかった。検出方法は光電子分光法であったが、表面からハフニウムを含む膜であること示すHf4fの光電子ピークを検出することはできず、この方法ではHfO2は形成できないと結論付けられた。
実施例1とほぼ同じ手順であるが、プラズマガスの発生方法であるが、図2に示される装置において、水バブラー11を通さず、乾燥した酸素のみをガラス管13に通し、プラズマ化させて導入する手法でHfO2膜の形成を試みた。その結果、被処理基板3の表面に酸化膜は形成されたが、図7に示されるように、成膜速度とALDサイクル数に比例関係が得られず、1サイクルあたりの成膜速度についても、0.27nm/cycleから、0.089nm/cycleと変動し、膜厚の制御が困難であることが示された。
実施例1とほぼ同じ手順で、水バブラー11の温度を0℃にすると、水自体が凍結し、水バブラーへの通ガスが困難であった。さらに水バブラー11の温度が80℃を超えると、ガラス管13や排気管5に水滴が付着し、反応容器1の排気が困難であることがわかり、水バブラーの温度は80℃より低く、室温の23℃より高い温度に設定することが有効であることを見出した。
実施例1とほぼ同じ手順で、プラズマガスを発生させるときの誘導コイル14に投入する高周波電力について、20W,30Wで試験した結果、酸化特性に特段の変化はみられなかった。10Wから15Wの領域では放電が困難である問題が生じた。本比較例より、誘導コイルに投入する高周波電力について、20、30Wが適当であることが分かった。このとき用いたガラス管は13mmであり、流量面積当たり3.8W/cm2以上とすることが適当であることがわかった。
2…温度調整台
3…被処理基板
4…排気ポンプ
5…排気管
6…原料タンク
7…流量制御器
8…酸素タンク
10…プラズマガス発生装置
11…水バブラー
12…プラズマ発生器
13…ガラス管
14…誘導コイル
15…プラズマの発生した領域
Claims (7)
- 固体基板上に酸化物薄膜を形成する酸化物薄膜の形成方法において、反応容器内に固体基板を設置し、固体基板の温度を、0℃より高く、150℃以下に保持し、反応容器内にテトラキス(エチルメチルアミノ)ハフニウムあるいは、テトラキス(エチルメチルアミノ)ジルコニウムを含む有機金属ガスを充満させる工程と、前記有機金属ガスを前記反応容器から排気するか又は前記反応容器内に不活性ガスを充満させる工程と、酸素と水蒸気とを含むガスをプラズマ化して酸素及び水蒸気を励起したプラズマガスを生成し、当該プラズマガスを前記反応容器に導入する工程と、前記反応容器からプラズマガスを排気するか又は前記反応容器内に不活性ガスを充満させる工程とを含む一連の工程を繰り返すことにより酸化物薄膜を形成することを特徴とする酸化物薄膜の形成方法。
- 請求項1の酸化物薄膜の形成方法において、前記プラズマ化したガスは、水蒸気を含有させた酸素を絶縁管に導入し、その周りから高周波磁界を、絶縁管内の断面積当たり3.8W/cm2以上の電力で印加して、前記絶縁管内部にプラズマを発生させることにより生成したものであることを特徴とした酸化物薄膜の形成方法。
- 請求項2の酸化物薄膜の形成方法において、前記水蒸気を含有させた酸素は、酸素を0℃より高く、80℃を超えない水温の水と接触させることにより生成することを特徴とした酸化物薄膜の形成方法。
- 請求項1〜3の何れか一項の酸化物薄膜の形成方法において、固体基板上に一番最初に有機金属ガスを接触する前に、少なくとも水蒸気を含有するガスをプラズマ化したガスで処理する工程を具備することを特徴とした酸化物薄膜の形成方法。
- 請求項1〜4の何れか一項の酸化物薄膜の形成方法において、テトラキス(エチルメチルアミノ)ハフニウムあるいは、テトラキス(エチルメチルアミノ)ジルコニウムの有機金属ガスの照射量を、被処理基板表面において1.0×10-2Torr・s以上、あるいは1.0×105ラングミュア以上とすることを特徴とした酸化物薄膜の形成方法。
- 請求項1〜5の何れか一項の酸化物薄膜の形成方法において、プラズマガスの照射量を、被処理基板表面において、0.15Torr・s以上、あるいは1.5×105ラングミュア以上とすることを特徴とした酸化物薄膜の形成方法。
- 基板を保持する機構を備えた反応容器と、前記基板の温度を、0℃より高く、150℃以下に保持する温度調整機構と、テトラキス(エチルメチルアミノ)ハフニウムあるいは、テトラキス(エチルメチルアミノ)ジルコニウムを供給する原料供給装置と、水蒸気を含有させ酸素をガラス管に導入し、その周りから高周波磁界を印加して、ガラス管内部にプラズマを発生させてプラズマガスを得るプラズマガス発生装置とを具備し、反応容器内においてテトラキス(エチルメチルアミノ)ハフニウムの供給時に該物質の照射量を判定する判定機構と、反応容器内においてプラズマガスの照射量を判定する判定機構とを具備することを特徴とする酸化物薄膜形成装置。
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JP6813824B2 (ja) * | 2016-02-05 | 2021-01-13 | 国立大学法人山形大学 | 酸化物薄膜形成方法及び酸化物薄膜形成装置 |
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JP2019220647A (ja) * | 2018-06-22 | 2019-12-26 | 株式会社アルバック | 表面処理方法、プリント配線板の製造方法、および、表面処理装置 |
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