JP5661262B2 - 成膜方法および成膜装置 - Google Patents
成膜方法および成膜装置 Download PDFInfo
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- JP5661262B2 JP5661262B2 JP2009177382A JP2009177382A JP5661262B2 JP 5661262 B2 JP5661262 B2 JP 5661262B2 JP 2009177382 A JP2009177382 A JP 2009177382A JP 2009177382 A JP2009177382 A JP 2009177382A JP 5661262 B2 JP5661262 B2 JP 5661262B2
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- 238000000034 method Methods 0.000 title claims description 43
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 76
- 239000007800 oxidant agent Substances 0.000 claims description 58
- 230000001590 oxidative effect Effects 0.000 claims description 41
- 239000013078 crystal Substances 0.000 claims description 21
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 150000002902 organometallic compounds Chemical class 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 149
- 238000010926 purge Methods 0.000 description 29
- 235000012431 wafers Nutrition 0.000 description 28
- 239000006185 dispersion Substances 0.000 description 18
- 238000003860 storage Methods 0.000 description 14
- 239000007788 liquid Substances 0.000 description 9
- 239000010453 quartz Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000006200 vaporizer Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- CGRVKSPUKAFTBN-UHFFFAOYSA-N N-silylbutan-1-amine Chemical compound CCCCN[SiH3] CGRVKSPUKAFTBN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02189—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing zirconium, e.g. ZrO2
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- C—CHEMISTRY; METALLURGY
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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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- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- 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
- C23C16/455—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]
- C23C16/45527—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
- C23C16/45529—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 a layer stack of alternating different compositions or gradient compositions
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- 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
- C23C16/455—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]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
- C23C16/45546—Atomic layer deposition [ALD] characterized by the apparatus specially adapted for a substrate stack in the ALD reactor
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- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/022—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being a laminate, i.e. composed of sublayers, e.g. stacks of alternating high-k metal oxides
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/314—Inorganic layers
- H01L21/316—Inorganic layers composed of oxides or glassy oxides or oxide based glass
- H01L21/31604—Deposition from a gas or vapour
- H01L21/31641—Deposition of Zirconium oxides, e.g. ZrO2
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- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
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- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02181—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing hafnium, e.g. HfO2
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- H01L21/02107—Forming insulating materials on a substrate
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- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02356—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment to change the morphology of the insulating layer, e.g. transformation of an amorphous layer into a crystalline layer
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Description
図1は本発明の成膜方法を実施するための成膜装置の一例を示す縦断面図、図2は図1の成膜装置を示す横断面図、図3は本発明の成膜方法の一例におけるガスの供給のタイミングを示すタイミングチャートである。なお、図2においては、加熱装置を省略している。
ここでは、まず、ZrソースとしてTEMAZを用い、Siソースとして3DMASを酸化剤としてO3を用いて、図3のタイミングチャートで図1の成膜装置によりウエハ上に成膜を行った。
5;ウエハボート(供給手段)
14;酸化剤供給機構
15;Zrソースガス供給機構
16;Siソースガス供給機構
19;酸化剤分散ノズル
24;Zrソースガス分散ノズル
27;Siソースガス分散ノズル
40;加熱機構
100;成膜装置
W;半導体ウエハ(被処理体)
Claims (6)
- 真空保持可能な処理容器内に被処理体を挿入し、前記処理容器内を真空に保持した状態とし、
前記処理容器内にジルコニウム原料ガスと酸化剤ガスとを交互的に複数回供給して基板上にZrO2膜を成膜する工程と、前記処理容器内にシリコン原料ガスと酸化剤ガスとを交互的に1回または複数回供給して基板上にSiO2膜を成膜する工程とを、膜中のSi濃度が1〜4atm%になるように供給回数を調整して行い、
前記ZrO2膜成膜の繰り返し回数をx回(xは複数)とし、前記SiO2膜成膜の繰り返し回数をy回(yは1以上)として、前記x回のZrO2膜成膜と前記y回のSiO2膜成膜とを1サイクルとし、このサイクルをz回(zは1以上)行い所定膜厚のジルコニア系膜を成膜するとともに、
前記xと前記yとを合計した回数に対する前記yの比率y/(x+y)×100%とジルコニア系膜の膜中のSi濃度との関係を予め把握しておき、ジルコニア系膜の膜中のSi濃度が1〜4atm%になるように前記xおよび前記yを調整し、
前記ジルコニウム原料ガスおよび前記シリコン原料ガスを、それぞれ有機金属化合物ガスとし、
前記ジルコニア系膜を成膜する際のプロセス温度を、200〜300℃の範囲とし、
前記成膜されたジルコニア系膜を、450℃以下の温度でアニールし、
比誘電率がSiを含まないジルコニア系膜よりも高い、ジルコニア結晶を有したジルコニア系膜を形成することを特徴とする成膜方法。 - 前記ジルコニア系膜の膜中のSi濃度が2〜4atm%になるように前記xおよび前記yを調整することを特徴とする請求項1に記載の成膜方法。
- 前記ジルコニア系膜は、電圧1Vをかけた際のリーク電流が10 −9 A/cm2 オーダー以下となることを特徴とする請求項2に記載の成膜方法。
- 前記ジルコニウム原料ガスの供給と前記酸化剤ガスの供給との間、および前記シリコン原料ガスの供給と前記酸化剤ガスの供給との間で、前記処理容器内のガスを排出することを特徴とする請求項1から請求項3のいずれか一項に記載の成膜方法。
- 前記酸化剤ガスは、O3ガス、H2Oガス、O2ガス、NO2ガス、NOガス、N2Oガス、O2ガスとH2ガスのラジカルから選択された少なくとも1種であることを特徴とする請求項1から請求項4のいずれか1項に記載の成膜方法。
- 被処理体に対して金属酸化膜を成膜する成膜装置であって、
真空保持可能な縦型で筒体状をなす処理容器と、
前記被処理体を複数段に保持した状態で前記処理容器内に保持する保持部材と、
前記処理容器内を排気する排気機構と、
前記処理容器の外周に設けられた加熱装置と、
ジルコニウム原料ガスを前記処理容器内に供給するジルコニウム原料ガス供給機構と、
シリコン原料ガスを前記処理容器内に供給するシリコン原料ガス供給機構と、
前記処理容器内へ酸化剤ガスを供給する酸化剤ガス供給機構と、
前記排気機構、前記加熱装置、前記ジルコニウム原料ガス供給機構、前記シリコン原料ガス供給機構および前記酸化剤ガス供給機構を制御する制御機構と
を具備し、
前記制御機構は、請求項1から請求項5のいずれか1項に記載の成膜方法が行なわれるように前記排気機構、前記加熱装置、前記ジルコニウム原料ガス供給機構、前記シリコン原料ガス供給機構および前記酸化剤ガス供給機構を制御することを特徴とする成膜装置。
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US8336487B2 (en) | 2012-12-25 |
US20110197813A1 (en) | 2011-08-18 |
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