TW201922768A - 釕化合物、薄膜形成用原料及薄膜之製造方法 - Google Patents
釕化合物、薄膜形成用原料及薄膜之製造方法 Download PDFInfo
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- TW201922768A TW201922768A TW107126821A TW107126821A TW201922768A TW 201922768 A TW201922768 A TW 201922768A TW 107126821 A TW107126821 A TW 107126821A TW 107126821 A TW107126821 A TW 107126821A TW 201922768 A TW201922768 A TW 201922768A
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- Prior art keywords
- thin film
- raw material
- compound
- ruthenium
- film
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- 239000010409 thin film Substances 0.000 title claims abstract description 92
- 239000002994 raw material Substances 0.000 title claims abstract description 79
- 150000003304 ruthenium compounds Chemical class 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 55
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 30
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 29
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 12
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008016 vaporization Effects 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 14
- 230000008018 melting Effects 0.000 abstract description 14
- 238000000034 method Methods 0.000 description 70
- 239000010408 film Substances 0.000 description 69
- 239000002243 precursor Substances 0.000 description 41
- 239000007789 gas Substances 0.000 description 39
- 238000006243 chemical reaction Methods 0.000 description 29
- 229910052751 metal Inorganic materials 0.000 description 29
- 239000002184 metal Substances 0.000 description 29
- 238000000231 atomic layer deposition Methods 0.000 description 28
- 230000015572 biosynthetic process Effects 0.000 description 25
- 238000005755 formation reaction Methods 0.000 description 21
- -1 tert-amyl Chemical group 0.000 description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 17
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- 239000000243 solution Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
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- 238000005229 chemical vapour deposition Methods 0.000 description 10
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 10
- 238000002309 gasification Methods 0.000 description 10
- 229910044991 metal oxide Inorganic materials 0.000 description 10
- 150000004706 metal oxides Chemical class 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 10
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- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
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- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000012434 nucleophilic reagent Substances 0.000 description 8
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- 239000010703 silicon Substances 0.000 description 8
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- DHCWLIOIJZJFJE-UHFFFAOYSA-L dichlororuthenium Chemical compound Cl[Ru]Cl DHCWLIOIJZJFJE-UHFFFAOYSA-L 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000005160 1H NMR spectroscopy Methods 0.000 description 5
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 5
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- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
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- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
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- WFRBDWRZVBPBDO-UHFFFAOYSA-N 2-methyl-2-pentanol Chemical compound CCCC(C)(C)O WFRBDWRZVBPBDO-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
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- 238000000354 decomposition reaction Methods 0.000 description 2
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- 229910017053 inorganic salt Inorganic materials 0.000 description 2
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- 238000005259 measurement Methods 0.000 description 2
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- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
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- 150000004658 ketimines Chemical group 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- RYEXTBOQKFUPOE-UHFFFAOYSA-M magnesium;propane;chloride Chemical compound [Mg+2].[Cl-].CC[CH2-] RYEXTBOQKFUPOE-UHFFFAOYSA-M 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- 150000003282 rhenium compounds Chemical class 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
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- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/0006—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table compounds of the platinum group
- C07F15/0046—Ruthenium 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
- C23C16/06—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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- 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
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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
- 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]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- 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
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- 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 Table
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Abstract
本發明係以提供蒸氣壓為高、比以往所知之化合物之熔點為低的釕化合物、含有該化合物之薄膜形成用原料及使用該原料而形成含有釕之薄膜的薄膜之製造方法為目的。 為達成上述目的,提供下述一般式所表示之釕化合物、含有該釕化合物之薄膜形成用原料及使用該薄膜形成用原料之薄膜之製造方法。(式中,R1
~R3
係各自獨立表示碳原子數1~5之烷基,但是,當R1
為甲基之時,R2
與R3
係相異之基)。
Description
本發明係關於一種具有特定之構造之新穎的釕化合物、含有該化合物之薄膜形成用原料及使用該原料而形成含有釕之薄膜的薄膜之製造方法。
包含釕元素之薄膜形成用材料係表示特異的電特性,應用於各種之用途。例如,DRAM元件所代表之記憶體元件之電極材料、阻抗膜、可使用於硬碟之記錄層之反磁性膜及使用作為固體高分子形燃料電池(polymer electrolyte fuel cell)用之觸媒材料等。
作為上述薄膜之製造法,舉例為濺鍍法、離子鍍敷法、塗佈熱分解法或溶凝膠法等之MOD法、化學氣相成長法等。此等之中,包含ALD(Atomic Layer Deposition,原子層成長)法之化學氣相成長(以下有時僅記載為「CVD」)法,由於具有組成控制性、階差被覆性優異,適於量產化,且可混合積體(Hybrid integration)等之多種優點,故為最佳之製造製程。
從以往,已知各種釕化合物可使用作為CVD法用原料之釕化合物。例如,在專利文獻1中,揭示於釕鍵結具有2個羰基及2個之特定之構造之酮亞胺基之釕化合物,但並對於於本發明之釕化合物之記載。因此,在專利文獻1所揭示之釕化合物之熔點為100℃以上,故不可充份滿足作為化學氣相成長原料之化合物。 [先前技術文獻] [專利文獻]
[專利文獻1] 國際公開第2010/071364號
[發明欲解決之課題]
使CVD法等之化合物氣化來形成薄膜之方法中,可使用作為原料之化合物(前驅物)所需要之性質係熔點為低且可於液體之狀態下輸送者、液體之黏度為低者、蒸氣壓為大且易於使其氣化者、熱安定性為高者。其中,在可使用於ALD法之情形時,具有稱為ALD窗口之可適用於ALD法的溫度區域被期待著。特別是,對於可使用於ALD法之釕化合物,具有ALD窗口,蒸氣壓為高,且熔點為低的化合物被期待著,但對於以往之釕化合物,於該等之點並無可充分滿足之化合物。
因此,本發明之目的為提供蒸氣壓高,比過去已知的化合物具有更低熔點的釕化合物、含有該化合物的薄膜形成用原料,及使用該原料而形成含有釕之薄膜的薄膜之製造方法。 [用以解決課題之手段]
本發明人等重複檢討之結果,發現具有特定之構造的釕化合物可解決上述課題,因而完成本發明。 即,本發明係關於下述一般式(1)所表示之釕化合物:
(式中,R1
~R3
係各自獨立表示碳原子數1~5之烷基,但是,當R1
為甲基之時,R2
與R3
係相異之基)。
又,本發明係提供含有上述一般式(1)所表示之釕化合物之薄膜形成用原料。
進而,本發明係提供一種製造於基體之表面含有釕原子的薄膜之方法,其特徵包含下述步驟:使如請求項2之薄膜形成用原料氣化,得到含有前述釕化合物的蒸氣之步驟、 將前述蒸氣導入於處理氛圍之步驟, 及藉由使該化合物分解、藉由使其化學反應,或藉由其兩者使該化合物堆積於基體之步驟。 [發明之效果]
依據本發明,可得到蒸氣壓為高,且熔點為低的釕化合物,而該化合物係適合作為CVD法用之薄膜形成用原料,其中,由於具有ALD窗口,較佳可使用作為ALD法用之薄膜形成用原料。
[用以實施本發明之最佳形態]
本發明之釕化合物為上述一般式(1)所表示者,且為一氧化碳加成到釕原子之化合物。本發明之釕化合物可適合作為具有CVD法等氣化步驟的薄膜製造方法之先驅物(Precursor)者,由於為可適用於ALD法之先驅物,特別適合作為使用於ALD法之先驅物者。
上述一般式(1)中,R1
~R3
係各自獨立表示碳原子數1~5之烷基。但是,當R1
為甲基之情形時,R2
與R3
係相異之基。
上述一般式(1)中,作為R1
~R3
所表示之碳原子數1~5之烷基係可舉出例如甲基、乙基、正丙基、異丙基、正丁基、仲丁基、叔丁基、異丁基、正戊基、仲戊基、叔戊基、異戊基、新戊基。
上述一般式(1)中,R1
、R2
及R3
係依據適用之薄膜之製造方法來適當選擇。使用於具有使化合物氣化之步驟之薄膜之製造方法之情形時,R1
、R2
及R3
之組合以於常溫常壓下成為液體狀態,且蒸氣壓為大者為較佳。
具體而言,R1
為甲基、乙基、正丙基者由於蒸氣壓為高,故為較佳,其中,以甲基或乙基為特別佳。又,R3
為叔丁基者由於熔點為低,故較佳,R3
為叔丁基,R2
為甲基、乙基、正丙基、異丙基、正丁基、仲丁基者為又較佳,R3
為叔丁基,R2
為乙基者由於熔點特別低,故為較佳。
又,R1
為甲基或乙基,R3
為叔丁基,R2
為乙基者係蒸氣壓為高,熔點亦低者,故為較佳,R1
為甲基、R3
為叔丁基,R2
為乙基者係熔點為特別低,於25℃下之液體狀態之黏度為低,故為較佳。另一方面,利用不伴隨氣化步驟之MOD法之薄膜之製造方法之情形時,R1
、R2
及R3
係依據對於所使用之溶劑之溶解性、薄膜形成反應等,可任意地選擇。
作為本發明之釕化合物的較佳的具體例係可舉例如下述化合物No.1~No.217。 尚,下述化學式中之「Me」係表示甲基,「Et」係表示乙基,「nPr」係表示正丙基,「iPr」係表示異丙基,「sBu」係表示仲丁基、「tBu」係表示叔丁基,「tAm」係表示叔戊基。
於上述化合物中,就熔點為低而言,以化合物No.10、31、46,74、214為佳,以化合物No.10、31及214為又較佳。且,就蒸氣壓之觀點而言,以化合物No.10及No.31為較佳。
本發明之釕化合物係依據其製造方法並不特別地限制,可於公知之二氯化釕三羰基或十二碳三釕所代表之碳釕化合物中,藉由使對應之構造之脒化合物或對應之構造之脒化合物之鹼金屬鹽反應來獲得。
接著,所謂本發明之薄膜形成用原料係將以上述說明之本發明之釕化合物作為薄膜之前驅物者,且其形態可依據該薄膜形成用原料所適用之製造製程而相異。例如,製造僅包含釕作為金屬的薄膜之情形時,本發明之薄膜形成用原料不含本發明之釕化合物以外之金屬化合物及半金屬化合物。另一方面,製造包含2種類以上之金屬及/或半金屬之薄膜之情形時,除了本發明之釕化合物以外,本發明之薄膜形成用原料亦含有包含所期望之金屬的化合物及/或包含半金屬之化合物(以下亦稱為「其他前驅物」)。本發明之薄膜形成用原料如後述,亦可進一步含有有機溶劑及/或親核性試藥。本發明之薄膜形成用原料如上述說明,由於前驅物之本發明之釕化合物的物性為適用於CVD法、ALD法,故特別適合作為化學氣相成長用原料(以下有時稱為「CVD用原料」)。
本發明之薄膜形成用原料為化學氣相成長用原料之情形時,其形態可依據所使用的CVD法之輸送供給方法等方法而適當選擇。
作為上述之輸送供給方法,藉由將CVD用原料於儲存該原料之容器(以下有時亦記載為「原料容器」)中加熱及/或減壓而氣化成為蒸氣,將該蒸氣與視必要所使用之氬、氮、氦等之載氣一起導入設置有基體之成膜腔室內(以下有時亦記載為「堆積反應部」)之氣體輸送法、將CVD用原料於液體或溶液狀態下輸送至氣化室,於氣化室藉由加熱及/或減壓而氣化成為蒸氣,將該蒸氣導入成膜腔室內之液體輸送法。氣體輸送法之情形時,以上述一般式(I)表示之釕化合物本身可作為CVD原料。液體輸送法之情況時,可將上述一般式(I)表示之釕化合物本身或該化合物溶於有機溶劑中之溶液作為CVD用原料。該等之CVD用原料亦可進一部包含其他前驅物或親核性試藥。
又,於多成分系之CVD法中,有使CVD用原料各成分獨立氣化、供給之方法(以下有時亦記載為「單一源法」)與使多成分原料預先以期望組成混合之混合原料氣化、供給之方法(以下有時亦記載為「混合源法」)。混合源法之情形時,可將本發明之釕化合物與其他前驅物之混合物或者將該混合物溶於有機溶劑之混合溶液作為CVD用原料。該混合物或混合溶液亦可進一步包含親核性試藥等。
作為上述有機溶劑並未特別限制,可使用公知之一般有機溶劑。作為該有機溶劑可舉出例如乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等之乙酸酯類;四氫呋喃、四氫吡喃、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、二丁醚、二噁烷等之醚類;甲基丁基酮、甲基異丁基酮、乙基丁基酮、二丙基酮、二異丁基酮、甲基戊基酮、環己酮、甲基環己酮等之酮類;己烷、環己烷、甲基環己烷、二甲基環己烷、乙基環己烷、庚烷、辛烷、甲苯、二甲苯等之烴類;1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基環己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基環己烷、1,4-二氰基苯等之具有氰基之烴類;吡啶、二甲基吡啶(lutidine)等。該等係可根據溶質之溶解性、使用溫度與沸點、引火點之關係等而單獨或作為2種以上的混合溶劑使用。
使用該等之有機溶劑之情形時,將前驅物溶於有機溶劑之溶液的CVD用原料中之前驅物全體量0.01~ 2.0莫耳/升為佳,特別佳為0.05~1.0莫耳/升。所謂前驅物全體量,於本發明之薄膜形成用原料不含本發明之釕化合物以外之金屬化合物及半金屬化合物之情形時,為本發明之釕化合物的量,於本發明之薄膜形成用原料含有除了包含該釕化合物以外之其他之金屬的化合物及/或包含半金屬的化合物之情形時,為本發明之釕化合物及其他前驅物之合計量。
且,於多成分系之CVD法之情形時,作為與本發明之釕化合物一起使用之其他前驅物並未特別限制,可使用於CVD原料中所使用之公知一般前驅物。
作為上述其他先驅物,可舉出選自由醇化合物、甘醇化合物、β-二酮化合物、環戊二烯化合物、有機胺化合物等作為有機配位子使用的化合物所成群的1種或2種以上與矽素或金屬的化合物。又,作為先驅物之金屬種類,可舉出鋰、鈉、鉀、鎂、鈣、鍶、鋇、鈦、鋯、鉿、釩、鈮、鉭、鉻、鉬、鎢、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鋁、鎵、銦、鍺、錫、鉛、銻、鉍、鈧、釔、鑭、鈰、鐠、釹、鉅、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿或鎦。
作為上述其他先驅物的有機配位子所使用的醇化合物,可舉出甲醇、乙醇、丙醇、異丙醇、丁醇、仲丁基醇、異丁基醇、叔丁基醇、戊基醇、異戊基醇、叔戊基醇等烷基醇類;2-甲氧基乙醇、2-乙氧基乙醇、2-丁氧基乙醇、2-(2-甲氧基乙氧基)乙醇、2-甲氧基-1-甲基乙醇、2-甲氧基-1,1-二甲基乙醇、2-乙氧基-1,1-二甲基乙醇、2-異丙氧基-1,1-二甲基乙醇、2-丁氧基-1,1-二甲基乙醇、2-(2-甲氧基乙氧基)-1,1-二甲基乙醇、2-丙氧基-1,1-二乙基乙醇、2-s-丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等醚醇類;二甲基胺基乙醇、乙基甲基胺基乙醇、二乙基胺基乙醇、二甲基胺基-2-戊醇、乙基甲基胺基-2-戊醇、二甲基胺基-2-甲基-2-戊醇、乙基甲基胺基-2-甲基-2-戊醇、二乙基胺基-2-甲基-2-戊醇等二烷基胺基醇類等。
作為上述其他先驅物的有機配位子所使用的甘醇化合物,可舉出1,2-乙烷二醇、1,2-丙烷二醇、1,3-丙烷二醇、2,4-己二醇、2,2-二甲基-1,3-丙烷二醇、2,2-二乙基-1,3-丙烷二醇、1,3-丁二醇、2,4-丁二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙烷二醇、2,4-戊烷二醇、2-甲基-1,3-丙烷二醇、2-甲基-2,4-戊烷二醇、2,4-己二醇、2,4-二甲基-2,4-戊烷二醇等。
又,作為上述其他先驅物的有機配位子所使用的β-二酮化合物,可舉出乙醯丙酮、己烷-2,4-二酮、5-甲基己烷-2,4-二酮、庚烷-2,4-二酮、2-甲基庚烷-3,5-二酮、5-甲基庚烷-2,4-二酮、6-甲基庚烷-2,4-二酮、2,2-二甲基庚烷-3,5-二酮、2,6-二甲基庚烷-3,5-二酮、2,2,6-三甲基庚烷-3,5-二酮、2,2,6,6-四甲基庚烷-3,5-二酮、辛烷-2,4-二酮、2,2,6-三甲基辛烷-3,5-二酮、2,6-二甲基辛烷-3,5-二酮、2,9-二甲基壬烷-4,6-二酮、2-甲基-6-乙基癸烷-3,5-二酮、2,2-二甲基-6-乙基癸烷-3,5-二酮等的烷基取代β-二酮類;1,1,1-三氟戊烷-2,4-二酮、1,1,1-三氟-5,5-二甲基己烷-2,4-二酮、1,1,1,5,5,5-六氟戊烷-2,4-二酮、1,3-二全氟己基丙烷-1,3-二酮等氟取代烷基β-二酮類;1,1,5,5-四甲基-1-甲氧基己烷-2,4-二酮、2,2,6,6-四甲基-1-甲氧基庚烷-3,5-二酮、2,2,6,6-四甲基-1-(2-甲氧基乙氧基)庚烷-3,5-二酮等醚取代β-二酮類等。
又,作為上述其他先驅物的有機配位子所使用的環戊二烯化合物,可舉出環戊二烯、甲基環戊二烯、乙基環戊二烯、丙基環戊二烯、異丙基環戊二烯、丁基環戊二烯、仲丁基環戊二烯、異丁基環戊二烯、叔丁基環戊二烯、二甲基環戊二烯、四甲基環戊二烯等。
作為上述有機配位子所使用的有機胺化合物,可舉出甲基胺、乙基胺、丙基胺、異丙基胺、丁基胺、仲丁基胺、叔丁基胺、異丁基胺、二甲基胺、二乙基胺、二丙基胺、二異丙基胺、乙基甲基胺、丙基甲基胺、異丙基甲基胺等。
上述其他先驅物在該技術領域中為公知者,其製造方法亦為公知。若要舉出製造方法之一例子,例如作為有機配位子使用醇化合物之情形時,藉由將先前所述的金屬的無機鹽或其水合物與該醇化合物之鹼金屬烷氧化物進行反應而可製造出先驅物。於此,作為金屬的無機鹽或其水合物,可舉出金屬的鹵素化物、硝酸鹽等,作為鹼金屬烷氧化物,可舉出鈉烷氧化物、鋰烷氧化物、鉀烷氧化物等。
上述其他先驅物在單源方法之情形時,以與本發明之釕化合物在熱及/或氧化分解之舉動上類似的化合物為佳,在混合源法之情形時,以在熱及/或氧化分解的舉動為類似以外,於混合時不會因化學反應等而引起變質者為佳。
又,於本發明之薄膜形成用原料中,視必要欲對於本發明之釕化合物及其他先驅物賦予安定性,可含有親核性試藥。作為該親核性試藥,可舉出乙二醇二甲醚(Glyme)、二甘醇二甲醚、三甘醇、四甘醇二甲醚等乙二醇醚類、18-冠-6、二環己基-18-冠-6、24-冠-8、二環己基-24-冠-8、二苯并-24-冠-8等冠醚類、乙二胺、N,N’-四甲基乙二胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、1,1,4,7,7-五甲基二乙烯三胺、1,1,4,7,10,10-六甲基三乙烯四胺、三乙氧基三乙烯胺等聚胺類、Cyclam、環烯等環狀聚胺類、吡啶、吡咯烷、哌啶、嗎啉、N-甲基吡咯烷、N-甲基哌啶、N-甲基嗎啉、四氫呋喃、四氫吡喃、1,4-二噁烷、噁唑、噻唑、氧雜硫戊環等雜環化合物類、乙醯乙酸甲酯、乙醯乙酸乙酯、乙醯乙酸-2-甲氧基乙基等β-酮酯類或乙醯丙酮、2,4-己烷二酮、2,4-庚烷二酮、3,5-庚烷二酮、二新戊醯基甲烷等β-二酮類,該等親核性試藥之使用量對於先驅物全體的量1莫耳而言,以0.1莫耳~10莫耳的範圍為佳,又較佳為1~4莫耳。
本發明之薄膜形成用原料中,極力不包含構成此的成分以外之雜質金屬元素成分、雜質氯等雜質鹵素成分,及雜質有機成分。雜質金屬元素成分在元素單位下以100ppb以下為佳,以10ppb以下為又較佳。總量以1ppm以下為佳,以100ppb以下為又較佳。特別作為LSI的閘極絕緣膜、閘極膜、障礙層使用之情形時,必須將對所得的薄膜之電氣特性有影響的鹼金屬元素及鹼土類金屬元素之含有量減少。雜質鹵素成分以100ppm以下為佳,以10ppm以下為較佳,以1ppm以下為最佳。雜質有機成分的總量以500ppm以下為佳,以50ppm以下為又較佳,以10ppm以下為最佳。又,水分因為成為在化學氣相成長用原料中之顆粒產生或薄膜形成中之顆粒產生的原因,故對於前驅物、有機溶劑及親核性試藥,欲減低各水分,在使用之時預先盡可能除去水分為佳。前驅物、有機溶劑及親核性試藥的各水分量以10ppm以下為佳,以1ppm以下為又較佳。
又,本發明之薄膜形成用原料欲減低或防止所形成的薄膜之顆粒污染,極力地不包含顆粒為較佳。具體而言,在液相之光散射式液中粒子檢測器進行顆粒測定中,比0.3μm大的粒子數在液相1ml中以100個以下為較佳,比0.2μm大的粒子數在液相1ml中以1000個以下為又較佳,比0.2μm大的粒子數在液相1ml中以100個以下為最佳。
作為本發明之使用薄膜形成用原料製造薄膜的本發明之薄膜的製造方法,其為將氣化本發明之薄膜形成用原料的蒸氣,及視必要使用的反應性氣體,導入於設置有基體的成膜室內(處理氛圍),其次將先驅物在基體上進行分解、藉由使其化學反應、或藉由其兩者而將含有金屬的薄膜於基體表面使其成長、堆積的CVD法所得者。對於原料的輸送供給方法、堆積方法、製造條件、製造裝置等,並無特別限制,可使用一般公知的條件及方法。
作為上述視必要使用的反應性氣體,例如作為氧化性者,可舉出氧、臭氧、二氧化氮、一氧化氮、水蒸氣、過氧化氫、甲酸、乙酸、乙酸酐等,作為還原性者,可舉出氫,又作為製造氮化物者,可舉出單烷基胺、二烷基胺、三烷基胺、伸烷基二胺等有機胺化合物、肼、氨等,該等可使用1種或2種以上。此等中,亦就本發明之薄膜形成用原料與臭氧的反應性良好而言,作為反應性氣體使用1種之情形時,以使用臭氧為較佳,作為反應性氣體使用2種以上的混合氣體之情形時,至少包含臭氧為佳。
又,作為上述輸送供給方法,可舉出前述氣體輸送法、液體輸送法、單源方法、混合源法等。
又,作為上述堆積方法,可舉出將原料氣體或原料氣體與反應性氣體僅藉由熱進行反應而堆積薄膜的熱CVD、使用熱與電漿的電漿CVD、使用熱與光的光CVD、使用熱、光及電漿的光電漿CVD、將CVD的堆積反應分為基本過程,在分子水準下進行階段式堆積的ALD。
作為上述基體的材質,例如可舉出矽;氮化矽、氮化鈦、氮化鉭、氧化鈦、氮化鈦、氧化釕、氧化鋯、氧化鉿、氧化鑭等陶瓷;玻璃;金屬鈷等金屬。作為基體的形狀,可舉出板狀、球狀、纖維狀、鱗片狀。基體表面可為平面,亦可為成溝槽結構等三次元結構。
又,作為上述製造條件,可舉出反應溫度(基體溫度)、反應壓力、堆積速度等。對於反應溫度,可使本發明之化合物充分地反應的溫度之100℃以上為較佳,以150℃~400℃為又較佳,以200℃~350℃為特佳。又,反應壓力在熱CVD或光CVD之情形時,以10Pa~大氣壓為較佳,使用電漿之情形時,以10Pa~2000Pa為較佳。 又,堆積速度可藉由原料的供給條件(氣化溫度、氣化壓力)、反應溫度、反應壓力進行控制。堆積速度若過大時,所得之薄膜的特性會有惡化的情形產生,過小時,在生產性上會產生問題,故以0.01nm/分~100nm/分為較佳,以1nm/分~50nm/分為又較佳。又,ALD法的情形時為,欲得到所期望膜厚而控制循環次數。
作為上述製造條件,進一步可舉出使薄膜形成用原料進行氣化而成為蒸氣時的溫度或壓力。使薄膜形成用原料氣化來獲得蒸氣的步驟可在原料容器內進行,亦可在氣化室內進行。在任一情形中,本發明之薄膜形成用原料在0℃~150℃下使其蒸發為較佳。又,在原料容器內或氣化室內使薄膜形成用原料氣化來獲得蒸氣之情形時,原料容器內的壓力及氣化室內之壓力皆為1Pa~10000Pa者為較佳。
本發明之薄膜之製造方法除了採用ALD法,藉由上述之輸送供給方法使薄膜形成用原料氣化成為蒸氣,將該蒸氣導入成膜腔室內之原料導入步驟以外,亦可具有藉由該蒸氣中之上述化合物於上述基體之表面形成前驅物薄膜之前驅物薄膜成膜步驟、將未反應排氣之排氣步驟及使該前驅物薄膜與反應性氣體化學反應,於該基體之表面形成含有金屬之薄膜之含金屬之薄膜形成步驟。
以下對於上述ALD法的各步驟,將形成金屬氧化物薄膜的情形作為例子進行詳細說明。首先,進行上述原料導入步驟。將薄膜形成用原料成為蒸氣時的較佳溫度或壓力與藉由CVD法的薄膜之製造方法所說明者相同。其次,藉由將導入於成膜室的蒸氣與基體的表面進行接觸,於基體表面形成前驅物薄膜(前驅物薄膜形成步驟)。此時,可加熱基體,或加熱成膜室而進行加熱。在該步驟所成膜的前驅物薄膜為由本發明之化合物所生成的薄膜,或本發明之化合物的一部分分解及/或反應所生成的薄膜,具有與目的的金屬氧化物薄膜相異的組成。進行本步驟時的基體溫度以室溫~500℃為較佳,以150℃~350℃為又較佳。進行本步驟時的系統(成膜室內)之壓力以1Pa~ 10000Pa為較佳,以10Pa~1000Pa為又較佳。
其次,將未反應的化合物氣體或副產物的氣體由成膜室排氣(排氣步驟)。未反應的化合物氣體或副產物的氣體由成膜室完全排氣者為理想,但完全排氣非必須。作為排氣方法,可舉出藉由氮、氦、氬等惰性氣體沖洗系統內的方法、將系統內經減壓而排氣的方法、組合此等之方法等。減壓之情形時的減壓度以0.01Pa~300Pa為佳,以0.01Pa~100Pa為較佳。
其次,於成膜室導入氧化性氣體作為反應性氣體,藉由該氧化性氣體之作用或氧化性氣體及熱之作用,由在先前前驅物薄膜形成步驟所得之前驅物薄膜形成金屬氧化物薄膜(含有金屬氧化物的薄膜形成步驟)。對於本步驟,使熱產生作用之情形時的溫度以室溫~500℃為較佳,150~350℃為又較佳。進行本步驟時的系統(成膜室內)之壓力以1Pa~10000Pa為較佳,10Pa~1000Pa為又較佳。本發明之化合物因與氧化性氣體的反應性為良好,故可得到殘留碳含有量較少的高品質金屬氧化物薄膜。
於本發明之薄膜的製造方法中,採用如上述ALD法之情形時,將藉由上述原料導入步驟、前驅物薄膜形成步驟、排氣步驟及含有金屬氧化物的薄膜形成步驟所成的一連操作之薄膜堆積作為1循環,將該循環重複進行數次至得到必要膜厚之薄膜。該情形時,進行1循環後,與上述排氣步驟同樣地,自堆積反應部排氣出未反應的化合物氣體及反應性氣體(形成金屬氧化物薄膜之情形時的氧化性氣體), 進一步排出副產物的氣體後,再進行1循環者為佳。
又,於藉由金屬氧化物薄膜的ALD法之形成中,可施加電漿、光、電壓等能量,亦可使用觸媒。施加該能量的時期及使用觸媒的時期並無特別限定。例如,在原料導入步驟中之化合物氣體導入時、於前驅物薄膜成膜步驟或含有金屬氧化物的薄膜形成步驟中之加溫時、於排氣步驟中之系統內排氣時、可於含有金屬氧化物的薄膜形成步驟中之氧化性氣體導入時,亦可在上述各步驟之間。
又,於本發明之薄膜的製造方法中,於薄膜堆積之後,欲得到更良好的電氣特性,可在惰性氛圍下、氧化性氛圍下或還原性氛圍下進行退火處理,若階差埋入為必要時,可設有迴流步驟。此情形時的溫度為200℃~1000℃,以250℃~500℃為佳。
使用本發明之薄膜形成用原料製造薄膜的裝置,可使用公知的化學氣相成長法用裝置。作為具體裝置之例子,可舉出如圖1所示可將先驅物進行起泡供給的裝置,或如、圖2所示具有氣化室之裝置。又,可舉出如圖3及圖4所示對於反應性氣體可進行電漿處理的裝置。不僅為如圖1~圖4所示葉片式裝置,亦可使用利用批式爐可同時處理多數片之裝置。
使用本發明之薄膜形成用原料所製造的薄膜,可藉由適宜地選擇其他先驅物、反應性氣體及製造條件,可製成金屬、氧化物陶瓷、氮化物陶瓷、玻璃等所期望種類的薄膜。已知該薄膜顯示電氣特性及光學特性等,應用於各種用途上。例如,可舉出金屬釕薄膜、氧化釕薄膜、釕合金及含有釕之複合氧化物薄膜等。作為釕合金系可舉出Pt-Ru合金。作為含有釕之複合氧化物薄膜係可舉出SrRuO3
。該等之薄膜,例如,DRAM元件所代表之記憶體元件之電極材料、阻抗膜、可使用於硬碟之記錄層之反磁性膜及可廣泛使用於聚合物電解質燃料電池(polymer electrolyte fuel cell)用之觸媒材料等之製造。 [實施例]
以下依據實施例、製造例、比較例及評估例對本發明進行更詳細地說明。然而,本發明並未受到以下實施例等任何限制。 [實施例1]化合物No.10之合成 於反應燒瓶中,加入N’-(叔丁基)-N-乙基乙醯亞胺醯胺16g與去水THF 225mL,並充分混合。於冰冷下,於所得到之溶液中,滴入72.6mL之正丁基鋰之己烷溶液(1.55M),並攪拌1小時。於特別準備之反應燒瓶中,加入二氯化釕三羰基13.1g與去水THF 511mL,並充分混合後,以於冰冷下,滴入前述之反應溶液。反應溶液係於15小時之室溫攪拌後,以80℃實施4小時加熱迴流。攪拌後,回到室溫並過濾。所得到之濾液於減壓下、以油浴75℃下實施去溶劑。將所得到之釕錯合物以油浴135℃、13Pa進行蒸餾,得到6.41g之淡黃色黏狀液體。
(分析值) (1)常壓TG-DTA 質量50%減少溫度:216℃(760Torr、Ar流量:100ml/分、昇溫10℃/分) (2)減壓TG-DTA 質量50%減少溫度:138℃(10Torr、Ar流量:50ml/分、昇溫10℃/分) (3)1H-NMR(重苯) 1.01-1.08ppm (6H,multiplet)、1.18-1.26ppm (18H,multiplet)、1.48-1.53ppm (6H,multiplet)、2.86-3.10ppm (4H,multiplet) (4)元素分析(理論值) C:49.4%(49.18%)、H:7.8%(7.80%)、N:12.7% (12.75%)
[實施例2]化合物No.31之合成 於反應燒瓶中,加入N’-(叔丁基)-N-丙醯亞胺醯胺10.35g與去水THF120mL,並充分混合。於所得到之溶液中,於冰冷下,滴入36.7ml之正丁基鋰之己烷溶液(1.55M),並攪拌1小時。於特別準備之反應燒瓶中,加入二氯化釕三羰基7.0g與去水THF 273mL,並充分混合後,以於冰冷下,滴入前述之反應溶液。反應溶液係於2小時之室溫攪拌後,以80℃實施10小時加熱迴流。攪拌後,回到室溫並過濾。將所得之濾液於減壓下,以油浴75℃實施去溶劑。將所得到之釕錯合物以油浴145℃、15Pa進行蒸餾,得到0.95g之淡黃色黏狀液體。
(分析值) (1)常壓TG-DTA 質量50%減少溫度:224℃(760Torr、Ar流量:100ml/分、昇溫10℃/分) (2)減壓TG-DTA 質量50%減少溫度:151℃(10Torr、Ar流量:50ml/分、昇溫10℃/分) (3)1H-NMR(重苯) 0.86-0.97ppm (6H,multiplet)、1.06-1.09ppm (6H,multiplet)、1.21-1.30ppm (18H.multiplet)、1.89-1.98ppm (4H,multiplet)、2.83-3.11ppm (4H.multiplet) (4)元素分析(理論值) C:51.3%(51.37%)、H:8.0%(8.19%)、N:12.0% (11.98%)
[實施例3]化合物No.46之合成 於反應燒瓶中,加入二氯化釕三羰基5.5g與去水THF 80mL,並充分混合。於冰冷下,滴入藉由N,N’-二異丙基碳二亞胺5.7g與乙基鋰1.58g調製之N,N’-二異丙基-丙脒鋰之THF溶液於所得到之懸濁液中。以室溫攪拌19小時後,以減壓下油浴75℃實施去溶劑。將生成之釕錯合物放入於燒瓶中,連接於連續蒸餾精製裝置,以加熱溫度125℃、27Pa進行蒸餾,得到0.5之黃色黏性固體。
(分析值) (1)常壓TG-DTA 質量50%減少溫度:222℃(760Torr、Ar流量:100ml/分、昇溫10℃/分) (2)減壓TG-DTA 質量50%減少溫度:153℃(10Torr、Ar流量:50ml/分、昇溫10℃/分) (3)1H-NMR(重苯) 0.82-0.86ppm (3H、triplet)、1.00-1.01 (3H、doublet)、1.15-1.16ppm (6H,doublet)、1.22-1.24 (3H、doublet)、1.75-1.90ppm (2H,multiplet)、3.29-3.38ppm (1H,septet)、3.59-3.69ppm (1H,septet) (4)元素分析(理論值) C:51.5%(51.37%)、H:8.2%(8.19%)、N:11.8% (11.98%)
[實施例4]化合物No.74之合成 於反應燒瓶中,加入二氯化釕三羰基5.2g與去水THF 80mL,並充分混合。於所得到之懸濁液中,於冰冷下,滴入藉由N,N’-二異丙基碳二亞胺5.4g與丙基氯化鎂4.3g調製之N,N’-二異丙基-丁基脒之THF溶液。以室溫攪拌19小時後,以減壓下油浴75℃實施去溶劑。將生成之釕錯合物放入燒杯中,連接於連續蒸餾精製裝置,以加熱溫度145℃、42Pa進行蒸餾,得到0.6g之棕色黏性液體(以室溫結晶化)。
(分析值) (1)常壓TG-DTA 質量50%減少溫度:222℃(760Torr、Ar流量:100ml/分、昇溫10℃/分) (2)減壓TG-DTA 質量50%減少溫度:157℃(10Torr、Ar流量:50ml/分、昇溫10℃/分) (3)1H-NMR(重苯) 0.75-0.79ppm (3H、triplet)、1.02-1.04 (3H、doublet)、1.17-1.19ppm (6H,doublet-doublet)、1.24-1.26 (3H、doublet)、1.31-1.41ppm (2H,sextet)、1.79-1.93ppm (2H,multiplet)、3.34-3.43ppm (1H,septet)、3.64-3.73ppm (1H,septet) (4)元素分析(理論值) C:53.4(53.31%)、H:8.5%(8.54%)、N:11.2 (11.30%)
[實施例5]化合物No.214之合成 於反應燒瓶中,加入二氯化釕三羰基4.9g與去水THF 80mL,並充分混合。於所得到之懸濁液中,於冰冷下,滴入藉由N,N’-二異丙基碳二亞胺5.1g與正丁基鋰2.5g調製之N,N’-二異丙基-戊基脒鋰之THF溶液。以室溫攪拌19小時後,以減壓下油浴75℃實施去溶劑。將生成之釕錯合物放入燒瓶中,連接於連續蒸餾精製裝置,以加熱溫度150℃、55Pa進行蒸餾,得到0.5g棕色黏性液體。
(分析值) (1)常壓TG-DTA 質量50%減少溫度:230℃(760Torr、Ar流量:100ml/分、昇溫10℃/分) (2)減壓TG-DTA 質量50%減少溫度:162℃(10Torr、Ar流量:50ml/分、昇溫10℃/分) (3)1H-NMR(重苯) 0.79-0.83ppm (3H、triplet)、1.04-1.06 (3H、doublet)、1.19-1.22ppm (8H,multiplet)、1.26-1.28 (3H、doublet)、1.32-1.41ppm (2H,sextet)、1.86-2.00ppm (2H,multiplet)、3.39-3.48ppm (1H,septet)、3.69-3.78ppm (1H,eptet) (4)元素分析(理論值) C:54.9(55.04%)、H:8.8%(8.85%)、N:10.8 (10.70%)
[評估例1]釕化合物之物性評估 對於在實施例1~5所得到的本發明之化合物No.10、31、46、74及214以及下述比較化合物1及2,使用TG-DTA測定裝置,確認藉由在常壓氛圍下(760torr)的加熱使試樣質量減少50質量%的時間點之溫度(L)。L為低者因蒸氣壓為高,故判斷為較佳者。且,將25℃中之狀態以目視觀測。對於25℃中作為固體者進行熔點測定。該等之結果表示於表1。尚,下述比較化合物1及比較化合物2之化學式中「Me」係表示甲基,「Et」係表示乙基,「tBu」係表示叔丁基。
由表1的結果得知,化合物No.10、31、46、74及214任一者比比較化合物1及比較化合物2之蒸氣壓為高、熔點為低。其中,化合物No.10、31及214係與具有類似結構之比較化合物相比得知,大幅地具有低熔點。此外,可得知化合物No.10及31之蒸氣壓為特別高。
[實施例6]金屬釕薄膜之製造 將化合物No.10作為原子層堆積法用原料,使用圖1所示裝置,藉由以下條件的ALD法,於矽晶圓上製造出金屬釕薄膜。 將所得之薄膜藉由X線光電子分光法進行薄膜組成的確認後,所得的薄膜為金屬釕,且殘留碳含量少於1.0 atom%。又,藉由X線反射率法進行膜厚測定,算出該平均值時,膜厚為平均26.4nmnm,每1循環所得之膜厚平均為0.05nm。
(條件) 基板:矽晶圓 反應溫度(矽晶圓溫度);325℃ 反應性氣體:氧 將由下述(1)~(4)所成的一連串步驟作為1循環,重複500次循環; (1)將在原料容器溫度:140℃,原料容器內壓力:100Pa的條件下使其氣化的原子層堆積法用原料導入於成膜室中,在系統壓力:100Pa下進行30秒堆積; (2)藉由15秒的氬氣沖洗,除去未堆積的原料; (3)將反應性氣體導入於成膜室,在系統壓力:100Pa下進行5秒反應; (4)藉由15秒的氬氣沖洗,除去未反應的反應性氣體及副產物氣體。
[實施例7]金屬釕薄膜之製造 除了使用將化合物No.31作為原子層堆積法用原料之外,以與實施例6相同之條件製造金屬釕薄膜。將所得之薄膜藉由X線光電子分光法進行薄膜組成的確認後,所得的薄膜為金屬釕,且殘留碳含量少於1.0atom%。又,藉由X線反射率法進行膜厚測定,算出該平均值時,膜厚為平均25.7nmnm,每1循環所得之膜厚平均為0.05nm。
[實施例8] 除了使用將化合物No.46作為原子層堆積法用原料之外,以與實施例6相同之條件製造金屬釕薄膜。將所得之薄膜藉由X線光電子分光法進行薄膜組成的確認後,所得的薄膜為金屬釕,且殘留碳含量少於1.0atom%。又,藉由X線反射率法進行膜厚測定,算出該平均值時,膜厚為平均26.3nm,每1循環所得之膜厚平均為0.05nm。
[實施例9]金屬釕薄膜之製造 將化合物No.10作為原子層堆積法用原料,使用圖1所示裝置,藉由以下條件的ALD法,於矽晶圓上製造出金屬釕薄膜。 將所得之薄膜藉由X線光電子分光法進行薄膜組成的確認後,所得的薄膜為金屬釕,且殘留碳含量少於1.0 atom%。又,藉由X線反射率法進行膜厚測定,算出該平均值時,膜厚為平均15nm,每1循環所得之膜厚平均為0.03nm。
(條件) 基板:矽晶圓 反應溫度(矽晶圓溫度);350℃ 反應性氣體:氫 將由下述(1)~(4)所成的一連串步驟作為1循環,重複500次循環; (1)將在原料容器溫度:140℃,原料容器內壓力:100Pa的條件下使其氣化的原子層堆積法用原料導入於成膜室中,在系統壓力:100Pa下進行30秒堆積; (2)藉由15秒的氬氣沖洗,除去未堆積的原料; (3)將反應性氣體導入於成膜室,在系統壓力:100Pa下進行60秒反應; (4)藉由15秒的氬氣沖洗,除去未反應的反應性氣體及副產物氣體。
[比較例3] 除了使用將比較化合物2作為原子層堆積法用原料之外,以與實施例6相同之條件製造金屬釕薄膜。將所得之薄膜藉由X線光電子分光法進行薄膜組成的確認後,所得的薄膜為金屬釕,且殘留碳含量少於6.0atom%。又,藉由X線反射率法進行膜厚測定,算出該平均值時,膜厚為平均10nm,每1循環所得之膜厚平均為0.02nm。
由實施例6~9的結果得知,皆可製造殘留碳含量為低、品質佳的金屬釕薄膜。另一方面,可得知比較例3所得到之薄膜係可獲得殘留碳含量為非常地高、品質不佳的金屬釕薄膜。又,當比較實施例6~8及比較例3之每1循環所得之膜厚時,可得知實施例6~8係可以生產性優於比較例3之2倍以上,來製造金屬釕薄膜。 由以上之結果可知,依據本發明,可利用ALD法生產性佳地製造高品質的金屬釕薄膜。
[圖1] 表示有關本發明之薄膜之製造方法所使用之化學氣相成長用裝置之一例子之概要圖。 [圖2] 表示有關本發明之薄膜之製造方法所使用之化學氣相成長用裝置之另一例子之概要圖。 [圖3] 表示有關本發明之薄膜之製造方法所使用之化學氣相成長用裝置之又另一例子之概要圖。 [圖4] 表示有關本發明之薄膜之製造方法所使用之化學氣相成長用裝置之又另一例子之概要圖。
Claims (3)
- 一種釕化合物,其特徵為以下述一般式(1)表示:(式中,R1 ~R3 係各自獨立表示碳原子數1~5之烷基,但是,當R1 為甲基之時,R2 與R3 係相異之基)。
- 一種薄膜形成用原料,其含有如請求項1之釕化合物。
- 一種製造於基體之表面含有釕原子的薄膜之方法,其特徵包含下述步驟:使如請求項2之薄膜形成用原料氣化,得到含有前述釕化合物的蒸氣之步驟、 將前述蒸氣導入於處理氛圍之步驟, 及藉由使該化合物分解、藉由使其化學反應,或藉由其兩者使該化合物堆積於基體之步驟。
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