JP5592327B2 - 誘電体膜の材料特性を高めるための活性化学的方法 - Google Patents
誘電体膜の材料特性を高めるための活性化学的方法 Download PDFInfo
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- JP5592327B2 JP5592327B2 JP2011213741A JP2011213741A JP5592327B2 JP 5592327 B2 JP5592327 B2 JP 5592327B2 JP 2011213741 A JP2011213741 A JP 2011213741A JP 2011213741 A JP2011213741 A JP 2011213741A JP 5592327 B2 JP5592327 B2 JP 5592327B2
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- 238000000034 method Methods 0.000 title claims description 226
- 239000000463 material Substances 0.000 title description 54
- 239000000126 substance Substances 0.000 title description 20
- 230000002708 enhancing effect Effects 0.000 title description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 231
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 225
- 239000010703 silicon Substances 0.000 claims description 225
- 239000003989 dielectric material Substances 0.000 claims description 169
- 239000012530 fluid Substances 0.000 claims description 105
- 230000008569 process Effects 0.000 claims description 91
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 claims description 39
- -1 trimethylsilylmethyl Chemical group 0.000 claims description 38
- RQVFGTYFBUVGOP-UHFFFAOYSA-N [acetyloxy(dimethyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(C)OC(C)=O RQVFGTYFBUVGOP-UHFFFAOYSA-N 0.000 claims description 31
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 30
- 239000011148 porous material Substances 0.000 claims description 27
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- 239000002904 solvent Substances 0.000 claims description 22
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 16
- NBBQQQJUOYRZCA-UHFFFAOYSA-N diethoxymethylsilane Chemical compound CCOC([SiH3])OCC NBBQQQJUOYRZCA-UHFFFAOYSA-N 0.000 claims description 15
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 15
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- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims description 11
- ZSMNRKGGHXLZEC-UHFFFAOYSA-N n,n-bis(trimethylsilyl)methanamine Chemical compound C[Si](C)(C)N(C)[Si](C)(C)C ZSMNRKGGHXLZEC-UHFFFAOYSA-N 0.000 claims description 11
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 10
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 10
- QHUNJMXHQHHWQP-UHFFFAOYSA-N trimethylsilyl acetate Chemical compound CC(=O)O[Si](C)(C)C QHUNJMXHQHHWQP-UHFFFAOYSA-N 0.000 claims description 10
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 claims description 9
- QULMGWCCKILBTO-UHFFFAOYSA-N n-[dimethylamino(dimethyl)silyl]-n-methylmethanamine Chemical compound CN(C)[Si](C)(C)N(C)C QULMGWCCKILBTO-UHFFFAOYSA-N 0.000 claims description 9
- UUAHJDYTCBLNOM-UHFFFAOYSA-N 1-ethoxy-1-methylsilolane Chemical compound CCO[Si]1(C)CCCC1 UUAHJDYTCBLNOM-UHFFFAOYSA-N 0.000 claims description 8
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- KAHVZNKZQFSBFW-UHFFFAOYSA-N n-methyl-n-trimethylsilylmethanamine Chemical compound CN(C)[Si](C)(C)C KAHVZNKZQFSBFW-UHFFFAOYSA-N 0.000 claims description 7
- JKDNLUGVHCNUTB-UHFFFAOYSA-N 1,1,3,3-tetramethyl-1,3-disiletane Chemical compound C[Si]1(C)C[Si](C)(C)C1 JKDNLUGVHCNUTB-UHFFFAOYSA-N 0.000 claims description 6
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- PEGHITPVRNZWSI-UHFFFAOYSA-N [[bis(trimethylsilyl)amino]-dimethylsilyl]methane Chemical compound C[Si](C)(C)N([Si](C)(C)C)[Si](C)(C)C PEGHITPVRNZWSI-UHFFFAOYSA-N 0.000 claims description 6
- RBHUHOJMUHMRDK-UHFFFAOYSA-N [diethoxy(phenyl)silyl]methyl-diethoxy-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C[Si](OCC)(OCC)C1=CC=CC=C1 RBHUHOJMUHMRDK-UHFFFAOYSA-N 0.000 claims description 6
- JWVHPGDCFVOYMQ-UHFFFAOYSA-N [dimethoxy(methyl)silyl]oxy-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)O[Si](C)(OC)OC JWVHPGDCFVOYMQ-UHFFFAOYSA-N 0.000 claims description 6
- PWDHJVSLINAQFE-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methyl-dimethoxy-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C[Si](OC)(OC)C1=CC=CC=C1 PWDHJVSLINAQFE-UHFFFAOYSA-N 0.000 claims description 6
- KCCVBXQGWAXUSD-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]oxy-dimethoxy-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)O[Si](OC)(OC)C1=CC=CC=C1 KCCVBXQGWAXUSD-UHFFFAOYSA-N 0.000 claims description 6
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- NYROPPYCYUGLLK-UHFFFAOYSA-N diethoxymethyl(diethoxymethylsilylmethyl)silane Chemical compound CCOC(OCC)[SiH2]C[SiH2]C(OCC)OCC NYROPPYCYUGLLK-UHFFFAOYSA-N 0.000 claims description 6
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- NVOGZRLXCWJNIK-UHFFFAOYSA-N ethoxy-[[ethoxy(diphenyl)silyl]methyl]-diphenylsilane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(OCC)C[Si](OCC)(C=1C=CC=CC=1)C1=CC=CC=C1 NVOGZRLXCWJNIK-UHFFFAOYSA-N 0.000 claims description 6
- NPOYZXWZANURMM-UHFFFAOYSA-N ethoxy-[ethoxy(dimethyl)silyl]oxy-dimethylsilane Chemical compound CCO[Si](C)(C)O[Si](C)(C)OCC NPOYZXWZANURMM-UHFFFAOYSA-N 0.000 claims description 6
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 6
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- TZPAJACAFHXKJA-UHFFFAOYSA-N methoxy-[[methoxy(dimethyl)silyl]methyl]-dimethylsilane Chemical compound CO[Si](C)(C)C[Si](C)(C)OC TZPAJACAFHXKJA-UHFFFAOYSA-N 0.000 claims description 6
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- SFJIKRAOANCCRX-UHFFFAOYSA-N trimethoxy(pentan-2-yl)silane Chemical compound CCCC(C)[Si](OC)(OC)OC SFJIKRAOANCCRX-UHFFFAOYSA-N 0.000 description 1
- HILHCDFHSDUYNX-UHFFFAOYSA-N trimethoxy(pentyl)silane Chemical compound CCCCC[Si](OC)(OC)OC HILHCDFHSDUYNX-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
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- IXJNGXCZSCHDFE-UHFFFAOYSA-N triphenoxy(phenyl)silane Chemical compound C=1C=CC=CC=1O[Si](C=1C=CC=CC=1)(OC=1C=CC=CC=1)OC1=CC=CC=C1 IXJNGXCZSCHDFE-UHFFFAOYSA-N 0.000 description 1
- FNNJGIKXHZZGCV-UHFFFAOYSA-N triphenoxy(propan-2-yl)silane Chemical compound C=1C=CC=CC=1O[Si](OC=1C=CC=CC=1)(C(C)C)OC1=CC=CC=C1 FNNJGIKXHZZGCV-UHFFFAOYSA-N 0.000 description 1
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- AABYOUNGNSKTRH-UHFFFAOYSA-N triphenoxy(triphenoxysilylmethyl)silane Chemical compound C=1C=CC=CC=1O[Si](OC=1C=CC=CC=1)(OC=1C=CC=CC=1)C[Si](OC=1C=CC=CC=1)(OC=1C=CC=CC=1)OC1=CC=CC=C1 AABYOUNGNSKTRH-UHFFFAOYSA-N 0.000 description 1
- SRFNOOYBAUZCIF-UHFFFAOYSA-N triphenylsilyloxysilicon Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(O[Si])C1=CC=CC=C1 SRFNOOYBAUZCIF-UHFFFAOYSA-N 0.000 description 1
- OZWKZRFXJPGDFM-UHFFFAOYSA-N tripropoxysilane Chemical compound CCCO[SiH](OCCC)OCCC OZWKZRFXJPGDFM-UHFFFAOYSA-N 0.000 description 1
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- FCTKBQXOGURHPR-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-pentan-2-ylsilane Chemical compound CCCC(C)[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C FCTKBQXOGURHPR-UHFFFAOYSA-N 0.000 description 1
- JICSGUKZEPKYFR-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-pentylsilane Chemical compound CCCCC[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C JICSGUKZEPKYFR-UHFFFAOYSA-N 0.000 description 1
- KGOOITCIBGXHJO-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-phenylsilane Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)C1=CC=CC=C1 KGOOITCIBGXHJO-UHFFFAOYSA-N 0.000 description 1
- MJIHPVLPZKWFBL-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-propan-2-ylsilane Chemical compound CC(C)(C)O[Si](C(C)C)(OC(C)(C)C)OC(C)(C)C MJIHPVLPZKWFBL-UHFFFAOYSA-N 0.000 description 1
- DIZPPYBTFPZSGK-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]-propylsilane Chemical compound CCC[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C DIZPPYBTFPZSGK-UHFFFAOYSA-N 0.000 description 1
- QCKKBOHAYRLMQP-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[SiH](OC(C)(C)C)OC(C)(C)C QCKKBOHAYRLMQP-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000003631 wet chemical etching Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- 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
- H01L21/3105—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- 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
- H01L21/02112—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
- H01L21/02126—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 containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Description
この出願は、35U.S.C.§119(e)の下、先に出願された2007年2月15日付米国特許出願公開第60/890、137号の明細書の優先権を主張し、それらの開示は、参照により本明細書中に全体を取り込む。
本明細書中で使用される場合、“層”または“該層”の語は、誘電体材料を示すので、パターン化されているかまたはいないかに係らず、誘電体材料の少なくとも1つの層の少なくとも一部分を意味する。
R7が−(CH2)n−によって表される化合物の具体例は、ビス(トリメトキシシリル)メタン、ビス(トリエトキシシリル)メタン、ビス(トリフェノキシシリル)メタン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、ビス(エトキシジフェニルシリル)メタン、1、2−ビス(トリメトキシシリル)エタン、1、2−ビス(トリエトキシシリル)エタン、1、2−ビス(トリフェノキシシリル)エタン、1、2−ビス(ジメトキシメチルシリル)エタン、1、2−ビス(ジエトキシメチルシリル)エタン、1、2−ビス(ジメトキシフェニルシリル)エタン、1、2−ビス(ジエトキシフェニルシリル)エタン、1、2−ビス(メトキシジメチルシリル)エタン、1、2−ビス(エトキシジメチルシリル)エタン、1、2−ビス(メトキシジフェニルシリル)エタン、1、2−ビス(エトキシジフェニルシリル)エタン、1、3−ビス(トリメトキシシリル)プロパン、1、3−ビス(トリエトキシシリル)プロパン、1、3−ビス(トリフェノキシシリル)プロパン、1、3−ビス(ジメトキシメチルシリル)プロパン、1、3−ビス(ジエトキシメチルシリル)プロパン、1、3−ビス(ジメトキシフェニルシリル)プロパン、1、3−ビス(ジエトキシフェニルシリル)プロパン、1、3−ビス(メトキシジメチルシリル)プロパン、1、3−ビス(エトキシジメチルシリル)プロパン、1、3−ビス(メトキシジフェニルシリル)プロパン、および1、3−ビス(エトキシジフェニルシリル)プロパンを含む。これらの中で好ましい化合物は、ビス(トリメトキシシリル)メタン、ビス(トリエトキシシリル)メタン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、およびビス(エトキシジフェニルシリル)メタンである。
UV硬化(ガス相)
PDEMS(商標)2.5ATRP膜(DEMS(商標)およびポロゲンから調製されたCVD誘電体膜)をエッチ、アッシング、および湿式洗浄工程で損傷させ、炭素を膜から取り除いて、膜の誘電率を2.57(第1の誘電率)から2.87(第2の誘電率)(膜厚さ2791Å、RI=1.385)まで上昇させた。サンプルを、400℃、真空の第1の真空のチャンバーに、5分間入れた。ウェハーを冷却後、ウェハーを45℃の第2の真空のチャンバーに移した。チャンバーを、12トールまで、ジエトキシメチルシラン(担体なし)で加圧した。試薬の孔系への拡散を補助するために、サンプルを試薬蒸気と2〜3分間平衡にさせた。ウェハーを次に、広帯域スイープUV源(H+電球を有するフュージョンI−600ランプ)を備えた300℃の第3の真空のチャンバーに移した。サンプルを、紫外線照射に1分間曝した。サンプルを、チャンバーから取り除いた。膜の誘電率は、2.61(第3の誘電率)(膜厚さ2758Å、RI=1.367)まで低下した。PE−CVD膜、例えば、DEMS(商標)の堆積に使用可能である同一の前駆体は、膜内に吸着され次にDEMS(商標)分子を活性化でき、一体化処理によって導入されたPDEMS(商標)ネットワーク中の欠陥と相互作用する。
UV硬化(液相)
2−ヘキサノン中ヘプタメチルジシラザンの10wt%溶液を、ポリプロピレン瓶中で混合した。PDEMS(商標)2.5ATRP膜(DEMS(商標)およびポロゲンから調製されたCVD誘電体膜)を、エッチ、アッシング、および湿式洗浄工程で損傷させ、炭素を膜から除いて、膜の誘電率を2.53(第1の誘電率)から2.8(第2の誘電率)(膜厚さ3322Å、RI=1.338)に上昇させた。この膜の一片をスピンコーターの上に置いた。約3mlの溶液を膜の上に置いた。スピン乾燥で修復試薬が除去される前に、試薬は膜と90秒接触した。サンプルを、広帯域スイープUV源を備えた300℃の真空のチャンバーに移した。サンプルを、100%出力のUV光に1分間曝した。処理後、膜の誘電率は、2.46(第3の誘電率)(膜厚さ3215Å、RI=1.346)であった。この例は、試薬、例えば、シラザンの選択が膜の誘電率を100%まで回復させるのに効果的であることを示す。例1および例2の組み合わせは、UV工程が誘電特性の回復のために、ガスおよび液相工程の両者で可能であることを具体的に示す。
プラズマ処理
PDEMS(商標)2.5ATRP膜(DEMS(商標)とポロゲンから調製されたCVD誘電体膜)を、エッチ、アッシング、および湿式洗浄工程で損傷させ、炭素を膜から除いて、誘電率を2.57(第1の誘電率)から2.87(第2の誘電率)(膜厚さ2791Å、RI=1.385)まで上昇させた。サンプルを400℃の第1の真空のチャンバーにとり、そして5分間真空にした。ウェハーを冷ました後で、ウェハーを、45℃の第2の真空のチャンバーに移した。チャンバーを、ジエトキシメチルシラン(担体なし)で15トールまで加圧した。サンプルを、孔系への試薬の拡散を補助するために、試薬蒸気と2〜3分間平衡にさせた。ジエトキシメチルシランを、チャンバーの外に排出させ、そして200mg/分のジエトキシメチルシランの流れを開始させた。流れが一旦安定化すると、プラズマ(75ワット)を10秒間当てた。プラズマステップの完了時に、チャンバーのポンプを止めそしてサンプルを取り出した。膜の誘電率は、2.8(第3の誘電率)(膜厚さ2820Å、RI=1.386)まで低下した。プラズマ工程は、また化学的種を活性化できるが、プラズマ工程からの活性化学的種は、損傷した多孔性膜の誘電率を回復できない。
プラズマ+UV(ガス相)
PDEMS(商標)2.5ATRP膜(DEMS(商標)とポロゲンから調製されたCVD誘電体膜)を、エッチ、アッシング、および湿式洗浄工程で損傷させ、炭素を膜から除いて、誘電率を2.57(第1の誘電率)から2.87(第2の誘電率)(膜厚さ2791Å、RI=1.385)まで上昇させた。サンプルを400℃、真空下の第1のチャンバー5分間入れた。ウェハーを冷ました後で、ウェハーを、250℃の第2の真空のチャンバーに移した。チャンバーを、ジエトキシメチルシラン(担体なし)で18トールまで加圧した。サンプルを、孔系への試薬の拡散を補助するために試薬蒸気と2〜3分間平衡にさせた。ジエトキシメチルシランを、チャンバーの外に排出させ、そして200mg/分のジエトキシメチルシランのフローを開始させた。フローが一旦安定化すると、プラズマ(75ワット)を10秒間当てた。プラズマステップの完了時に、チャンバーのポンプを止めた。サンプルを、広帯域スイープUV源を備えた300℃の第3の真空のチャンバーに移した。サンプルを、100%出力UV光に1分間曝した。サンプルをチャンバーから取り出した。膜の誘電率は、2.63(第3の誘電率)(膜厚さ2790Å、RI=1.368)まで低下した。プラズマ工程からの化学的活性工程と、UV光を使用した硬化の組み合わせを使用すると、膜の誘電率を充分に回復させることができる。2つの工程の組み合わせなしでは、初期の損傷していない膜特性を充分に回復させることはできない。
溶媒中でのシリル化剤の濃度および誘電率回復の効果
ケイ素含有流体の適用は、ブランケット膜またはパターン化された構造のいずれかと接触できるため、デバイスメーカーは、シリカ含有流体を適用した後で、洗浄ステップを使用したくない場合がある。パターン化された構造の典型的な湿式化学的クリーニングにおいて、ウェハー上に残るエッチおよびアッシング工程からのあらゆる残留する試薬および/または破片を除去するために、基材を多量の水で洗浄する。新しい工程を保有するコストを低下させるために、任意の処理ステップを除くことは、資金および汚染への潜在性を節約するであろう。ケイ素含有流体中でシリル化剤の濃度を最適化できる場合、洗浄ステップの工程を除くことができる場合がある。下記表1中のものより高い濃度は、またCH3−Si結合の取り込みおよび誘電率の回復に有益である可能性があるため、この例は上限を決めることを意図しない。
表1
PDEMS(商標)2.5ATRP膜(DEMS(商標)とポロゲンから調製されたCVD誘電体膜)を、エッチ、アッシング、および湿式洗浄工程で損傷させ、炭素を膜から除いて、膜の誘電率を2.50(第1の誘電率)から2.99(第2の誘電率)(膜厚さ4468Å、RI=1.391)まで上昇させた。サンプルを、400℃、真空下の第1の真空のチャンバーに5分間入れた。
この例では、修復剤として種々のシリル化剤および硬化工程の効果を見る。曝露の条件は、300℃、真空下で、UV1分間、または窒素フロー下、熱(400℃)5分間いずれかであった。
表2
損傷した多孔性誘電体ケイ素含有薄膜の修繕の間、トレンチおよびビアを作るために用いられる全ての工程の後で、中間層誘電体膜を修繕することが好ましい。そうした工程は、エッチング、アッシング、および湿式化学的ストリッピング、誘電率の増加および低下した疎水性を起こすもの全てを含む。好ましくは、修復試薬は、また湿式化学的剥離剤に曝した後の膜を乾燥するために使用される、液体または蒸気のいずれかの、水およびアルコール類に曝した後で、表面を修復できる。
表3
修復試薬は、エッチングおよびアッシングで起こるサイドウォールの損傷を修繕するために用いることができる。そうした試薬および工程は、小さい構造に浸透し、孔系に浸透し、膜の組成および電気の特性を修復し、そして構造の臨界寸法の何らかの変化を最小化できなければならないであろう。分子の反応性によって、洗浄溶媒は、パターン化された構造から残留物を除去するために使用されなければならないが、修復試薬がターゲットとする活性な欠陥から試薬を除いてはならないであろう。
表4:
多くのUV硬化チャンバーは、真空にできない、したがって大気圧対真空の効果は、成功する修復工程において重要な因子であることができる。比較として、熱処理を、不活性ガスのパージ下、種々の温度で行って修復試薬が任意の特定の温度で活性化するか否かを見た。
表5
誘電体膜の誘電特性は、集積回路中でトレンチおよびビアを製造するために用いられる多くの工程によって損傷されるので、これらの工程から生じる損傷を修繕することが必要である。多孔性誘電体膜が損傷した場合、表面は次の層の接着を大幅に改善する炭素種の損失により親水性になる。修復試薬を完了させた後、表面は、好ましくは損傷した膜より、さらに疎水性であり、金属バリアーと誘電体層との接着の問題に繋がる。接着の失敗は、銅の誘電体層への浸透、および貧弱なデバイスの信頼性を生じることができる。
表6
広帯域および単色光源を含む膜の化学的修復を活性化できる多くの異なるUV光源がある。この例は、より低い波長、すなわち、185nm以下が、損傷した膜の修復に非常に効果的であることができることを示す。
表7
装置の中断時間および処理の問題は、膜の処理で遅延を生じることができ、したがって硬化前にエージングされるので、膜の効果において変動性がある場合がある。
表8
一旦膜が修繕されると、追加の処理をされる前の時間を延ばすことができる。修復された膜は、クリーンルーム条件下において、可能な限り、電気的におよび組成的に好ましくは安定なままである。膜が安定なままである場合、試薬は、膜内の欠陥に化学結合し、膜が非常に疎水性であり、そして大気水分が修繕された表面と強く相互作用しないことを示唆する。
表9
PDEMS(商標)2.5ATRP膜を、エッチガスに曝露した後、酸化アッシング工程を通して損傷させた。多くの他の工程と同様に、この工程は、典型的には同等以上の屈折率と、膜からの炭素の除去、および膜の誘電率の増加となる。表10中で、“損傷していない”は、UV硬化後だが、任意の追加の処理前のPDEMS(商標)2.5膜(すなわち、第1の誘電率)をいい、そして“損傷した”は、エッチおよびアッシング処理によって損傷した膜(すなわち、第2の誘電率)をいう。
比較のために、熱でそして、広帯域UV源で別々に、膜を硬化させた。熱硬化サンプルを、400℃窒素気流下で5〜10分間硬化させ、UV硬化サンプルを、300℃真空下で1分間硬化させた。硬化後、クリーンルーム環境(40〜45%RH、72華氏度)でサンプルを3日間平衡にさせ、膜に水を再吸収させた。Hgプローブおよび反射率測定法を、リーク電流密度、および絶縁破壊電圧“%回復”として規定される上記の式から計算されるように、誘電体の回復を評価するために使用した。膜を再加熱して電気測定前に、あらゆる吸着水を除いた。接触角は、水の液滴と膜表面との接触角である。
表10
この例は、米国特許出願公開第2006/0057855号明細書に開示された強化剤活性成分、DMDASプラズマ中のガス相のアセトキシシランの使用とUV曝露、およびプラズマとUV曝露とを比較する。
表11
(態様)
(態様1)
第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率を回復させる方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面と、ケイ素含有流体とを接触させるステップ、そして、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を、紫外線照射、熱、および電子ビームからなる群から選択されるエネルギー源に曝すステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有する、方法。
(態様2)
該ケイ素含有流体の第2の部分が、ケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、該ケイ素含有流体の第1の部分を除去するステップをさら含む態様1の方法であって、該除去ステップが、該接触ステップと、該曝露ステップとの間で起こる方法。
(態様3)
ケイ素含有誘電体材料の該層を、該エネルギー源に曝す前に、ケイ素含有誘電体材料の該層を、低エネルギープラズマ源に曝すステップをさらに含む、態様1の方法。
(態様4)
ケイ素含有誘電体材料の該層が、該プラズマエネルギー源、並びに紫外線照射、熱エネルギー、および電子ビームからなる群から選択される少なくとも1種のエネルギー源に同時に曝される、態様3の方法。
(態様5)
ケイ素含有誘電体材料の該層が紫外線照射、熱エネルギー、および電子ビームからなる群から選択される該少なくとも1種のエネルギー源に曝される前に、ケイ素含有誘電体材料の該層が該プラズマエネルギー源に曝される、態様3の方法。
(態様6)
該エネルギー源が、紫外線照射を含む、態様1の方法。
(態様7)
該エネルギー源が、熱エネルギーをさらに含む、態様6の方法。
(態様8)
該紫外線照射が、単色紫外線照射である、態様6の方法。
(態様9)
該接触ステップが、化学気相堆積工程によって行われる、態様1の方法。
(態様10)
該ケイ素含有流体が、メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリ−n−プロポキシシラン、メチルトリイソプロポキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジメトキシシラン、ジエチルジエトキシシラン、ジエトキシメチルシラン、1、1、3、3−テトラメトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラエトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラメトキシ−1、3−ジフェニルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラフェニルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラフェニルジシロキサン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシラン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、ビス(エトキシジフェニルシリル)メタン、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、メチルトリアセトキシシラン、メチルエトキシシラシクロプロパン、ヘキサメチルシラブタン、ジメチルジアセトキシシラン、およびジ−tert−ブトキシジアセトキシシランからなる群から選択される少なくとも1種である、態様9の方法。
(態様11)
該ケイ素含有流体が、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、ヘキサメチルシクロトリシロキサン、デカメチルシクロペンタシラン、ドデカメチルシクロヘキサシラン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、メチルトリエトキシシラン、メチルトリメトキシシラン、および(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシランからなる群から選択される少なくとも1種である、態様10の方法。
(態様12)
該ケイ素含有流体が、ジエトキシメチルシラン、ジメチルジアセトキシシラン、メチルトリアセトキシシラン、ジ−tert−ブトキシジアセトキシシラン、ジメチルジメトキシシラン、およびメチルトリエトキシシランからなる群から選択される少なくとも1種である、態様llの方法。
(態様13)
該ケイ素含有流体が、オクタメチルシクロテトラシロキサンまたはテトラメチルシクロテトラシロキサンの少なくとも一つを含む、態様10の方法。
(態様14)
該ケイ素含有流体が、ジメチルジアセトキシシラン、メチルトリアセトキシシラン、およびアセトキシトリメチルシランを含む、態様12の方法。
(態様15)
該接触ステップがスピンオン堆積工程によって行われる、態様1の方法。
(態様16)
ケイ素含有誘電体材料の該層が、多孔性である、態様1の方法。
(態様17)
該第1の誘電率が、約1.5〜約3.5であり、該第2の誘電率が該第1の誘電率より約5%〜約200%高く、そして該第3の誘電率が該第2の誘電率に比較して、約10%〜約150%回復する、態様1の方法。
(態様18)
該第1の誘電率が、約1.5〜約2.8である、態様17の方法。
(態様19)
該第1の誘電率が、約1.8〜約2.7である、態様18の方法。
(態様20)
ケイ素含有誘電体材料の該層が、少なくとも400℃の温度に曝した後で、該第3の誘電率の10%以内である誘電率を有する、態様1の方法。
(態様21)
該ケイ素含有流体が、直鎖シラザン、環状シラザン、環状有機シロキサン、有機シロキサン、アルキルアルコキシシラン、アルキルアセトキシシラン、アルキルクロロシラン、カルボシラン、アミノアルキルシラン、アルキルアミノアルキルシラン、およびアミノアルキルアルコキシシランからなる群から選択される少なくとも1種を含む、態様1の方法。
(態様22)
該ケイ素含有流体が、アルキルアセトキシシランを含む、態様21の方法。
(態様23)
第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率を回復させる方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面とケイ素含有流体とを接触させるステップ、
該ケイ素含有流体の第2の部分がケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、該ケイ素含有流体の第1の部分を除去するステップ、そして、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を、紫外線照射および熱エネルギーに曝すステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有する、方法。
(態様24)
ケイ素含有誘電体材料の該層を、該エネルギー源に曝す前に、ケイ素含有誘電体材料の該層を、低エネルギープラズマ源に曝すステップをさらに含む、態様23の方法。
(態様25)
該紫外線照射が、単色紫外線照射である、態様23の方法。
(態様26)
該接触ステップを化学気相堆積工程によって行う、態様23の方法。
(態様27)
該ケイ素含有流体が、メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリ−n−プロポキシシラン、メチルトリイソプロポキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジメトキシシラン、ジエチルジエトキシシラン、ジエトキシメチルシラン、1、1、3、3−テトラメトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラエトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラメトキシ−1、3−ジフェニルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラフェニルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラフェニルジシロキサン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシラン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、ビス(エトキシジフェニルシリル)メタン、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、メチルトリアセトキシシラン、メチルエトキシシラシクロプロパン、ヘキサメチルシラブタン、ジメチルジアセトキシシラン、およびジ−tert−ブトキシジアセトキシシランからなる群から選択される少なくとも1種である、態様26の方法。
(態様28)
該ケイ素含有流体が、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、ヘキサメチルシクロトリシロキサン、デカメチルシクロペンタシラン、ドデカメチルシクロヘキサシラン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、メチルトリエトキシシラン、メチルトリメトキシシラン、および(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシランからなる群から選択される少なくとも1種である、態様27の方法。
(態様29)
該ケイ素含有流体が、ジエトキシメチルシラン、ジメチルジアセトキシシラン、メチルトリアセトキシシラン、ジ−tert−ブトキシジアセトキシシラン、ジメチルジメトキシシラン、およびメチルトリエトキシシランからなる群から選択される少なくとも1種である、態様28の方法。
(態様30)
該ケイ素含有流体が、アセトキシトリメチルシラン、メチルトリアセトキシシラン、またはジメチルジアセトキシシランの少なくとも1種を含む、態様29の方法。
(態様31)
ケイ素含有誘電体材料の該層が、多孔性である、態様23の方法。
(態様32)
該第1の誘電率が、約1.5〜約3.5であり、該第2の誘電率が、該第1の誘電率より約5%〜約150%高く、そして該第3の誘電率が該第2の誘電率に比較して約10%〜約150%回復する、態様23の方法。
(態様33)
該第1の誘電率が、約1.5〜約2.8である、態様32の方法。
(態様34)
該第1の誘電率が、約1.8〜約2.7である、態様33の方法。
(態様35)
少なくとも400℃の温度に曝した後のケイ素含有誘電体材料の該層が、該第3の誘電率の10%以内である誘電率を有する、態様23の方法。
(態様36)
該ケイ素含有流体が、直鎖シラザン、環状シラザン、環状有機シロキサン、有機シロキサン、アルキルアルコキシシラン、アルキルアセトキシシラン、アルキルクロロシラン、カルボシラン、アミノアルキルシラン、アルキルアミノアルキルシラン、およびアミノアルキルアルコキシシランからなる群から選択される少なくとも1種を含む、態様23の方法。
(態様37)
該ケイ素含有流体が、アルキルアセトキシシランを含む、態様36の方法。
(態様38)
第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率の回復方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面と、アルキルアルコキシシランを含むケイ素含有流体とを接触させるステップ、
該ケイ素含有流体の第2の部分が、該ケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、該ケイ素含有流体の第1の部分を除去するステップ、そして、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を紫外線照射および熱エネルギーに曝すステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有する、方法。
(態様39)
該アルキルアルコキシシランが、メチルトリエトキシシラン、メチルトリメトキシシラン、メチルトリプロポキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジメチルジプロポキシシラン、トリメチルメトキシシラン、トリメチルエトキシシラン、およびトリメチルプロポキシシランからなる群から選択された少なくとも1種である、態様38の方法。
(態様40)
該アルキルアルコキシシランが、メチルトリエトキシシランである、態様39の方法。
(態様41)
該アルキルアルコキシシランが、ジメチルジメトキシシランである、態様39の方法。
(態様42)
ケイ素含有誘電体材料の該層が、多孔性である、態様38の方法。
(態様43)
該第1の誘電率が、約1.5〜約3.5であり、該第2の誘電率が、該第1の誘電率より約5%〜約150%高く、そして該第3の誘電率が、該第2の誘電率に比べて約10%〜約150%回復する、態様42の方法。
(態様44)
該第1の誘電率が、約1.5〜約2.8である、態様43の方法。
(態様45)
該第1の誘電率が、約1.8〜約2.7である、態様44の方法。
(態様46)
少なくとも400℃の温度に曝した後で、ケイ素含有誘電体材料の該層が、該第3の誘電率の10%以内である誘電率を有する、態様38の方法。
Claims (29)
- 第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率を回復させる方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面と、ケイ素含有流体とを接触させるステップ、
洗浄溶媒を用いた洗浄により、ある量の該ケイ素含有流体が、ケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、そして該ケイ素含有流体が、孔を塞がず、埋めず、充填せず、または密封せず、かつ該ケイ素含有誘電体材料の上にさらなる層を形成しないように、大部分の該ケイ素含有流体を、除去するステップであって、該除去ステップが、該接触ステップと、曝すステップとの間で起こるステップ、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を、不活性雰囲気中で紫外線照射のエネルギー源およびプラズマエネルギー源に曝すステップ、そして、
該ケイ素含有誘電体材料を、50℃から450℃への温度に少なくとも一回ヒートサイクルするステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有し、
ここでケイ素含有誘電体材料の該層が、該プラズマエネルギー源および該紫外線照射に同時に曝される、方法。 - 該紫外線照射が、単色紫外線照射である、請求項1の方法。
- 該接触ステップが、化学気相堆積工程によって行われる、請求項1の方法。
- 該ケイ素含有流体が、メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリ−n−プロポキシシラン、メチルトリイソプロポキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジメトキシシラン、ジエチルジエトキシシラン、ジエトキシメチルシラン、1、1、3、3−テトラメトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラエトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラメトキシ−1、3−ジフェニルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラフェニルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラフェニルジシロキサン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシラン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、ビス(エトキシジフェニルシリル)メタン、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、メチルトリアセトキシシラン、メチルエトキシシラシクロプロパン、ヘキサメチルシラブタン、ジメチルジアセトキシシラン、ヘキサメチルシクロトリシロキサン、デカメチルシクロペンタシラン、ドデカメチルシクロヘキサシランおよびジ−tert−ブトキシジアセトキシシランからなる群から選択される少なくとも1種である、請求項3の方法。
- 該接触ステップがスピンオン堆積工程によって行われる、請求項1の方法。
- ケイ素含有誘電体材料の該層が、多孔性である、請求項1の方法。
- 該第1の誘電率が、1.5〜3.5であり、該第2の誘電率が該第1の誘電率より5%〜200%高く、そして該第3の誘電率が該第2の誘電率に比較して、10%〜150%回復する、請求項1の方法。
- 該第1の誘電率が、1.5〜2.8である、請求項7の方法。
- 該第1の誘電率が、1.8〜2.7である、請求項8の方法。
- ケイ素含有誘電体材料の該層が、少なくとも400℃の温度に曝した後で、該第3の誘電率の10%以内である誘電率を有する、請求項1の方法。
- 該ケイ素含有流体が、直鎖シラザン、環状シラザン、環状有機シロキサン、有機シロキサン、アルキルアルコキシシラン、アルキルアセトキシシラン、アルキルクロロシラン、カルボシラン、アミノアルキルシラン、アルキルアミノアルキルシラン、およびアミノアルキルアルコキシシランからなる群から選択される少なくとも1種を含む、請求項1の方法。
- 第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率を回復させる方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面とケイ素含有流体とを接触させるステップ、
洗浄溶媒を用いた洗浄により、ある量の該ケイ素含有流体が、ケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、そして該ケイ素含有流体が、孔を塞がず、埋めず、充填せず、または密封せず、かつ該ケイ素含有誘電体材料の上にさらなる層を形成しないように、大部分の該ケイ素含有流体を、除去するステップ、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を、不活性雰囲気中で紫外線照射および熱エネルギーおよびプラズマエネルギー源に曝すステップ、そして、
ケイ素含有誘電体材料の該層を50℃から450℃への温度に少なくとも一回ヒートサイクルするステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有し、
ここでケイ素含有誘電体材料の該層が、該プラズマエネルギー源および該紫外線照射に同時に曝される、方法。 - 該紫外線照射が、単色紫外線照射である、請求項12の方法。
- 該接触ステップを化学気相堆積工程によって行う、請求項12の方法。
- 該ケイ素含有流体が、メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリ−n−プロポキシシラン、メチルトリイソプロポキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジメトキシシラン、ジエチルジエトキシシラン、ジエトキシメチルシラン、1、1、3、3−テトラメトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラエトキシ−1、3−ジメチルジシロキサン、1、1、3、3−テトラメトキシ−1、3−ジフェニルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラメチルジシロキサン、1、3−ジメトキシ−1、1、3、3−テトラフェニルジシロキサン、1、3−ジエトキシ−1、1、3、3−テトラフェニルジシロキサン、2、2、4、6、6−ペンタメチル−2、4、6−トリシラ−ヘプタン、1−メチル−1−エトキシシラシクロペンタン、1、1、3、3−テトラメチル−1、3−ジシラシクロブタン、1、3−ジメチル−1、3−ジエトキシ−1、3−ジシラシクロブタン、ビス(トリメチルシリルメチル)ベンゼン、(トリデカフルオロ−1、1、2、2−テトラヒドロオクチル)トリエトキシシラン、ビス(ジメトキシメチルシリル)メタン、ビス(ジエトキシメチルシリル)メタン、ビス(ジメトキシフェニルシリル)メタン、ビス(ジエトキシフェニルシリル)メタン、ビス(メトキシジメチルシリル)メタン、ビス(エトキシジメチルシリル)メタン、ビス(メトキシジフェニルシリル)メタン、ビス(エトキシジフェニルシリル)メタン、ヘキサメチルジシラザン、ヘキサメチルシクロトリシラザン、ヘプタメチルジシラザン、オクタメチルシクロテトラシラザン、ノナメチルトリシラザン、ジメチルシクロシラザン、アセトキシトリメチルシラン、メトキシトリメチルシラン、エトキシトリメチルシラン、3−アミノプロピルジメチルエトキシシラン、3−アミノプロピルメチルジエトキシシラン、ビス(ジメチルアミノ)ジメチルシラン、ジメチルアミノトリメチルシラン、アミノメチルトリメチルシラン、オクタメチルシクロテトラシロキサン、テトラメチルシクロテトラシロキサン、メチルトリアセトキシシラン、メチルエトキシシラシクロプロパン、ヘキサメチルシラブタン、ジメチルジアセトキシシラン、ヘキサメチルシクロトリシロキサン、デカメチルシクロペンタシラン、ドデカメチルシクロヘキサシランおよびジ−tert−ブトキシジアセトキシシランからなる群から選択される少なくとも1種である、請求項14の方法。
- ケイ素含有誘電体材料の該層が、多孔性である、請求項14の方法。
- 該第1の誘電率が、1.5〜3.5であり、該第2の誘電率が、該第1の誘電率より5%〜150%高く、そして該第3の誘電率が該第2の誘電率に比較して10%〜150%回復する、請求項14の方法。
- 該第1の誘電率が、1.5〜2.8である、請求項17の方法。
- 該第1の誘電率が、1.8〜2.7である、請求項18の方法。
- 少なくとも400℃の温度に曝した後のケイ素含有誘電体材料の該層が、該第3の誘電率の10%以内である誘電率を有する、請求項14の方法。
- 該ケイ素含有流体が、直鎖シラザン、環状シラザン、環状有機シロキサン、有機シロキサン、アルキルアルコキシシラン、アルキルアセトキシシラン、アルキルクロロシラン、カルボシラン、アミノアルキルシラン、アルキルアミノアルキルシラン、およびアミノアルキルアルコキシシランからなる群から選択される少なくとも1種を含む、請求項12の方法。
- 該ケイ素含有流体が、アルキルアセトキシシランを含む、請求項21の方法。
- 第1の誘電率および少なくとも1つの表面を有するケイ素含有誘電体材料の層の誘電率の回復方法であって、ケイ素含有誘電体材料の該層の該第1の誘電率が第2の誘電率に増加しており、該方法は、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面と、アルキルアルコキシシランを含むケイ素含有流体とを接触させるステップ、
洗浄溶媒を用いた洗浄により、ある量の該ケイ素含有流体が、ケイ素含有誘電体材料の該層の該少なくとも1つの表面と接触を続けるように、そして該ケイ素含有流体が、孔を塞がず、埋めず、充填せず、または密封せず、かつ該ケイ素含有誘電体材料の上にさらなる層を形成しないように、大部分の該ケイ素含有流体を、除去するステップ、
ケイ素含有誘電体材料の該層の該少なくとも1つの表面を、不活性雰囲気中で紫外線照射および熱エネルギーに曝すステップ、そして、
ケイ素含有誘電体材料の該層を50℃から450℃への温度に少なくとも一回ヒートサイクルするステップ、の各ステップを含み、
ケイ素含有誘電体材料の該層を該エネルギー源に曝した後で、ケイ素含有誘電体材料の該層が、該第2の誘電率より低い第3の誘電率を有し、
ここでケイ素含有誘電体材料の該層が、該プラズマエネルギー源および該紫外線照射に同時に曝される、方法。 - 該アルキルアルコキシシランが、メチルトリエトキシシラン、メチルトリメトキシシラン、メチルトリプロポキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジメチルジプロポキシシラン、トリメチルメトキシシラン、トリメチルエトキシシラン、およびトリメチルプロポキシシランからなる群から選択された少なくとも1種である、請求項23の方法。
- ケイ素含有誘電体材料の該層が、多孔性である、請求項23の方法。
- 該第1の誘電率が、1.5〜3.5であり、該第2の誘電率が、該第1の誘電率より5%〜150%高く、そして該第3の誘電率が、該第2の誘電率に比べて10%〜150%回復する、請求項25の方法。
- 該第1の誘電率が、1.5〜2.8である、請求項26の方法。
- 該第1の誘電率が、1.8〜2.7である、請求項27の方法。
- 少なくとも400℃の温度に曝した後で、ケイ素含有誘電体材料の該層が、該第3の誘電率の10%以内である誘電率を有する、請求項23の方法。
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- 2008-02-12 TW TW097104758A patent/TWI347637B/zh active
- 2008-02-14 JP JP2008032948A patent/JP2008199028A/ja not_active Withdrawn
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KR100984195B1 (ko) | 2010-09-28 |
KR20080076847A (ko) | 2008-08-20 |
TW200845212A (en) | 2008-11-16 |
JP2012009899A (ja) | 2012-01-12 |
JP2008199028A (ja) | 2008-08-28 |
TWI347637B (en) | 2011-08-21 |
US7500397B2 (en) | 2009-03-10 |
US20080199977A1 (en) | 2008-08-21 |
EP1959485A2 (en) | 2008-08-20 |
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