JP2021036068A - 原子層堆積方法 - Google Patents
原子層堆積方法 Download PDFInfo
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- JP2021036068A JP2021036068A JP2019158128A JP2019158128A JP2021036068A JP 2021036068 A JP2021036068 A JP 2021036068A JP 2019158128 A JP2019158128 A JP 2019158128A JP 2019158128 A JP2019158128 A JP 2019158128A JP 2021036068 A JP2021036068 A JP 2021036068A
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- gas
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- material gas
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/452—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by activating reactive gas streams before their introduction into the reaction chamber, e.g. by ionisation or addition of reactive species
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Abstract
Description
図1は、本実施形態による係る樹脂のALD装置1の概略を示すものである。図1のALD装置1は、被成膜対象物10を出し入れ自在に収容可能であって、当該被成膜対象物10の被成膜面10aに所望の酸化膜(後述図2等では酸化膜11)を形成することが可能なチャンバ(反応容器)2を有している。チャンバ2内に収容された被成膜対象物10は、当該チャンバ2内に設けられている支持部3により、被成膜面10aに沿った長手方向(被成膜面二方向)において移動自在に支持される。
支持部3においては、チャンバ2内に収容された被成膜対象物10を被成膜面方向において移動自在に支持できる態様であれば良く、図1に示すようなロール to ロール方式によるものに限定されるものではない。例えば、被成膜対象物10を支持する支持台(例えば、特許6052470号公報の図1中の符号7で示すような支持台)を有した方式(以下、単に支持台方式と適宜称する)であって、当該支持台を被成膜面二方向に移動自在(被成膜面10aが後述のシャワーヘッド4と対向するように移動自在)にした構成が挙げられる。
図2は、シャワーヘッド4の一例を示すものである。図2のシャワーヘッド4において、搬送ロール33a,33bの両者間を移動する被成膜対象物10の被成膜面10aと対向する部位40には、原料供給装置51と連通(配管51aを介して連通)し原料ガスをチャンバ2内に噴き出す原料ガス噴出口41と、不飽和炭化水素供給装置52,オゾン発生装置53とそれぞれ連通(配管52a,53aを介して各々連通)しオゾンガスと不飽和炭化水素ガスとを各々噴き出すOH*形成ガス噴出口42と、がそれぞれ複数個設けられている。
原料ガス噴出口41,OH*形成ガス噴出口42,不活性ガス噴出口43,噴出口間排気口44それぞれ(以下、纏めて単に噴出口等と適宜称する)は、単に被成膜面二方向に沿って複数個配列して設けるだけでなく、当該被成膜面二方向と交差している交差方向(以下、単に交差方向と適宜称する)にも複数個配列して設けても良い。例えば、原料ガス噴出口41を交差方向に複数個配列して原料ガス噴出口群を構成したり、OH*形成ガス噴出口42を交差方向に複数個配列してOH*形成ガス噴出口群を構成することが挙げられる。
ガス排出部6は、チャンバ2内のガスを吸気して当該チャンバ2外に排出し、当該チャンバ2内を減圧状態に維持することが可能なものであれば、種々の態様を適用しても良く、その一例としては図1に示すように排気管6a,真空ポンプ6b等を備えた構成や、その他にオゾンキラー(オゾンを分解する除外筒等;図示省略),排気バルブ(開度調整可能なバルブ等;図示省略)等を備えた構成が挙げられる。
被成膜対象物10においては、支持部3により移動自在に支持可能(例えば、ロール to ロール方式や支持台方式により支持可能)なものであって、当該被成膜対象物10を被成膜面二方向において移動させながら被成膜面10aに酸化膜を形成できるものであれば、特に限定されるものではない。
原料ガスは、酸化膜を形成する元素(例えば、リチウム(Li)、マグネシウム(Mg)、ケイ素(Si)、チタン(Ti)、バナジウム(V)、クロム(Cr)、マンガン(Mn)、鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、亜鉛(Zn)、ガリウム(Ga)、ゲルマニウム(Ge)、イットリウム(Y)、ジルコニウム(Zr)、モリブデン(Mo)、ルテニウム(Ru)、ロジウム(Rh)、インジウム(In)、錫(Sn)、ハフニウム(Hf)、タンタル(Ta)、タングステン(W)、イリジウム(Ir)、白金(Pt)、鉛(Pb)等、以下これらの元素を金属または金属元素という)を構成元素として含む態様が挙げられる。例えば、Si−O結合若しくはSi−C結合を有する有機シリコンまたは金属元素−酸素結合若しくは金属元素−炭素結合を有する有機金属を含有する原料ガスや、有機金属錯体またはケイ素や金属の水素化物等の原料ガスが挙げられる。
オゾンガスは、種々の濃度のものを適用することが可能であるが、オゾン濃度が高いほど好ましい。例えば、高濃度のオゾンガスのオゾン濃度(体積%濃度)は、20〜100体積%が好ましく、80〜100体積%がより好ましい。これは、オゾン濃度が100体積%に近いほど、オゾンから生成される反応活性種(OH)をより高密度で被成膜面に到達させることができるためである。
不飽和炭化水素ガスは、エチレン等の2重結合を有する炭化水素(アルケン)やアセチレン等の3重結合を有する炭化水素(アルキン)といった不飽和炭化水素を含有するガスが挙げられる。不飽和炭化水素としては、エチレンやアセチレンの他に、プロピレン、ブチレン等の低分子量の不飽和炭化水素(例えば、炭素数nが4以下の不飽和炭化水素)が好ましく用いられる。これら不飽和炭化水素を含有する不飽和炭化水素ガスを原料ガスや高濃度のオゾンガスとの反応に供する際、不飽和炭化水素ガス中の水分量が少ない方が好ましい。これは、反応に供されるガス中に水分が多く含まれていると、水分と原料ガスとの反応により発塵するおそれがあるためである。例えば、JIS Z 8806に基づいて算出される大気圧露点(霜点)が−50℃以下(大気圧1013.25hPa)の不飽和炭化水素ガスを用いることが好ましい。同様に、後に詳細に説明するパージガスも大気圧露点(霜点)が−50℃以下のガスを用いることが好ましい。
不活性ガスは、例えば後述の原料ガスパージ工程や酸化剤パージ工程において適用可能なものであれば良い。その一例としては、N2,Ar,He等の不活性ガスが挙げられる。
原料ガス,オゾンガス,不飽和炭化水素ガス,不活性ガスの各ガス流量や、当該各ガスによる圧力(噴出口等と被成膜面10aとの間の圧力)等は、適宜設定することが可能なものであり、例えば被成膜面10aに供給する反応活性種(OH)、各噴出口等間のピッチ、被成膜対象物10の被成膜面二方向への移動速度等を考慮して、設定することが挙げられる。
ALD装置1による酸化膜形成の一例を図1〜図4に基づいて説明する。なお、図4においては、原料ガスとしてTMAを用い、被成膜面10aにAl2O3による酸化膜11を形成する場合の反応模式図を示すものとする。
10…被成膜対象物、10a…被成膜面、10b…吸着可能領域、11…酸化膜
2…チャンバ、3…支持部、4…シャワーヘッド
41…原料ガス噴出口、42…OH*形成ガス噴出口、43…不活性ガス噴出口、44…噴出口間排気口
42a,42b…第1,第2噴出口
51…原料ガス供給装置、52…不飽和炭化水素供給装置、53…オゾン発生装置、54…不活性ガス供給装置
6…ガス排出部
図1は、本実施形態によるALD装置1の概略を示すものである。図1のALD装置1は、被成膜対象物10を出し入れ自在に収容可能であって、当該被成膜対象物10の被成膜面10aに所望の酸化膜(後述図2等では酸化膜11)を形成することが可能なチャンバ(反応容器)2を有している。チャンバ2内に収容された被成膜対象物10は、当該チャンバ2内に設けられている支持部3により、被成膜面10aに沿った長手方向(被成膜面二方向)において移動自在に支持される。
Claims (18)
- 被成膜対象物の被成膜面に酸化膜を形成する装置であって、
被成膜対象物を収容可能なチャンバと、
チャンバ内に収容された被成膜対象物を、被成膜面に沿った四方向のうち相対する二方向において移動自在に支持する支持部と、
チャンバにおいて被成膜対象物の被成膜面と対向して備えられたシャワーヘッドと、
チャンバ内のガスを吸気して当該チャンバ外に排出し、当該チャンバ内の減圧状態を維持するガス排出部と、を備え、
シャワーヘッドは、
原料ガスをチャンバ内に噴き出す原料ガス噴出口と、オゾンガスと不飽和炭化水素ガスとを噴き出すOH*形成ガス噴出口と、が被成膜対象物の被成膜面と対向して前記二方向に所定間隔を隔てて交互に設けられており、
OH*形成ガス噴出口は、オゾンガスを噴き出す第1噴出口と、不飽和炭化水素ガスを噴き出す第2噴出口と、を有してなる、
ことを特徴とする原子層堆積装置。 - シャワーヘッドは、原料ガス噴出口とOH*形成ガス噴出口との両者間に、不活性ガスをチャンバ内に噴き出す不活性ガス噴出口が設けられていることを特徴とする請求項1記載の原子層堆積装置。
- シャワーヘッドの各噴出口間のうち少なくとも何れかに、噴出口間排気口が設けられていることを特徴とする請求項1または2に記載の原子層堆積装置。
- 支持部は、予め被成膜対象物が巻回される一端側ロールと、当該一端側ロールから送り出された被成膜対象物を巻き取る他端側ロールと、を有してなることを特徴とする請求項1〜3の何れかに記載の原子層堆積装置。
- 支持部は、被成膜対象物を支持する支持台を有し、当該支持台を被成膜対象物の被成膜面に沿って移動自在であることを特徴とする請求項1〜4の何れかに記載の原子層堆積装置。
- シャワーヘッドは、互いに隣接する原料ガス噴出口およびOH*形成ガス噴出口による噴出口対が、前記二方向に所定間隔を隔てて複数個配列されていることを特徴とする請求項1〜5の何れかに記載の原子層堆積装置。
- シャワーヘッドは、
被成膜面に沿った四方向のうち前記二方向と交差している交差方向に、原料ガス噴出口が複数個配列されて原料ガス噴出口群を構成し、
前記交差方向に、OH*形成ガス噴出口が複数個配列されてOH*形成ガス噴出口群を構成していることを特徴とする請求項1〜6の何れかに記載の原子層堆積装置。 - シャワーヘッドの各噴出口は、前記二方向の寸法が1mm〜50mmの範囲内であり、被成膜対象物の被成膜面との間の距離が1mm〜20mmの範囲内であることを特徴とする請求項1〜7の何れかに記載の原子層堆積装置。
- シャワーヘッドの各噴出口のうち少なくとも何れかは、被成膜面に沿った四方向のうち前記二方向と交差している交差方向に長いスリット形状であることを特徴とする請求項1〜8の何れかに記載の原子層堆積装置。
- 請求項1〜9の何れかに記載の原子層堆積装置を用い、チャンバ内に収容された被成膜対象物を前記二方向において移動させている状態で、当該被成膜面に酸化膜を形成する方法であって、
被成膜対象物の被成膜面に、酸化膜を構成する元素を含む原料ガスを原料ガス噴出口から供給して、当該被成膜面に原料ガスの吸着層を形成する原料ガス供給工程と、
原料ガス供給工程で供された原料ガスの余剰ガスと、当該原料ガスが被成膜面に吸着することで生じたガスと、を除去する原料ガスパージ工程と、
被成膜対象物の被成膜面に、20体積%以上のオゾンガスと不飽和炭化水素ガスをOH*形成ガス噴出口から供給し、当該被成膜面に形成された吸着層を酸化する酸化剤供給工程と、
酸化剤供給工程で供されたオゾンガスおよび不飽和炭化水素ガスの余剰ガスと、原料ガスの吸着層を酸化することで生じたガスと、を除去する酸化剤パージ工程と、を有し、
被成膜面に対し、被成膜対象物の移動に伴って前記各工程を行うことを特徴とする原子層堆積方法。 - 原子層堆積装置のガス排出部により、チャンバの内圧を大気圧よりも低圧に制御することを特徴とする請求項10記載の原子層堆積方法。
- 原料ガスパージ工程、酸化剤パージ工程において、チャンバの内圧を1000Pa以下に制御することを特徴とする請求項10または11記載の原子層堆積方法。
- 原料ガス供給工程、原料ガスパージ工程、酸化剤供給工程、酸化剤パージ工程の各工程によるサイクル複数回行い、
各原料ガス供給工程のうち少なくとも1工程と残りの工程とにおいて、それぞれ異なる種類の原料ガスを被成膜対象物に供給することを特徴とする請求項10〜12の何れかに記載の原子層堆積方法。 - 酸化膜は、Al2O3、HfO2、TiO2、ZnO、Ta2O3、Ga2O3、MoO3、RuO2、SiO2、ZrO2、Y2O3のいずれかの吸着層を含む、ことを特徴とする請求項10〜13の何れかに記載の原子層堆積方法。
- 不飽和炭化水素ガスは、エチレンガスであることを特徴とする請求項10〜14の何れかに記載の原子層堆積方法。
- 被成膜対象物を100℃以下の範囲内で加熱、または当該被成膜対象物を加熱しないことを特徴とする請求項10〜15の何れかに記載の原子層堆積方法。
- 原料ガスのガス供給量は、原料ガス噴出口における前記二方向と垂直方向の単位長さ当たり0.0001〜1sccmとし、
オゾンガスの供給量は、第1噴出口における前記二方向と垂直方向の単位長さ当たり0.1sccm〜10sccmとし、
不飽和炭化水素ガスの供給量は、第2噴出口における前記二方向と垂直方向の単位長さ当たり0.1sccm〜10sccmとすることを特徴とする請求項10〜16の何れかに記載の原子層堆積方法。 - 被成膜面における各噴出口と対向する表面の圧力は、0.1Pa〜1000Paの範囲内であることを特徴とする請求項10〜17の何れかに記載の原子層堆積方法。
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