JP2017007952A - 新規な化合物、薄膜形成用原料及び薄膜の製造方法 - Google Patents
新規な化合物、薄膜形成用原料及び薄膜の製造方法 Download PDFInfo
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- JP2017007952A JP2017007952A JP2015121840A JP2015121840A JP2017007952A JP 2017007952 A JP2017007952 A JP 2017007952A JP 2015121840 A JP2015121840 A JP 2015121840A JP 2015121840 A JP2015121840 A JP 2015121840A JP 2017007952 A JP2017007952 A JP 2017007952A
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- thin film
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- forming
- metal
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- 239000002994 raw material Substances 0.000 title claims abstract description 99
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 48
- 239000002184 metal Substances 0.000 claims abstract description 46
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 29
- 229910017052 cobalt Inorganic materials 0.000 claims description 28
- 239000010941 cobalt Chemical group 0.000 claims description 28
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 25
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
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- 125000004429 atom Chemical group 0.000 claims description 10
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- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 7
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- DTJSYSWZBHHPJA-UHFFFAOYSA-N n,n'-di(propan-2-yl)ethane-1,2-diimine Chemical compound CC(C)N=CC=NC(C)C DTJSYSWZBHHPJA-UHFFFAOYSA-N 0.000 description 6
- 230000001590 oxidative effect Effects 0.000 description 6
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- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 5
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- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 5
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 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 5
- 238000005259 measurement Methods 0.000 description 5
- HACCVLBYBQLWMC-UHFFFAOYSA-N n,n'-ditert-butylethane-1,2-diimine Chemical compound CC(C)(C)N=CC=NC(C)(C)C HACCVLBYBQLWMC-UHFFFAOYSA-N 0.000 description 5
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 4
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- 229910052707 ruthenium Inorganic materials 0.000 description 1
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- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-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
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 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
- 150000003609 titanium compounds Chemical class 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
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- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
【解決手段】本発明の新規化合物は、特定のジアザジエン系金属化合物からなることを特徴とする。
【選択図】図1
Description
即ち、本発明は、下記一般式(I)または下記一般式(II)で表される新規な化合物、これを含有してなる薄膜形成用原料及び該原料を用いた薄膜の製造方法を提供するものである:
気化工程を伴わないMOD法による薄膜の製造方法の場合は、R1及びR2は、使用される溶媒に対する溶解性、薄膜形成反応等によって任意に選択することができる。
例えば、本発明の一般式(I)で表される化合物のうち、コバルトの化合物を製造する場合には、コバルトのハロゲン化物、硝酸塩等の無機塩又はその水和物と、該当するジアザジエン化合物とを反応させる方法;コバルトのハロゲン化物、硝酸塩等の無機塩又はその水和物と、該当するジアザジエン化合物を反応させる方法などを利用することができる。
また、本発明の一般式(II)で表される化合物のうち、コバルトのジアザジエニル化合物を製造する場合には、例えば、コバルトのハロゲン化物、硝酸塩等の無機塩又はその水和物と、該当するジアザジエン化合物とを、ナトリウム、リチウム、水素化ナトリウム、ナトリウムアミド、水酸化ナトリウム、ナトリウムメチラート、アンモニア、アミン等の塩基の存在下で反応させる方法;コバルトのハロゲン化物、硝酸塩等の無機塩又はその水和物と、該当するジアザジエン化合物のナトリウム錯体、リチウム錯体、カリウム錯体等を反応させる方法;本発明の一般式(I)で表される化合物の不均化などを利用することができる。
[実施例1:化合物No.2の製造]
200mlの4つ口フラスコに、塩化コバルト(II)5.02g(0.039mol)、テトラヒドロフラン19.5gを仕込み、室温下で撹拌した。その中に、N,N’−ジイソプロプル−1,4−ジアザ−1,3−ブタジエン5.47g(0.039mol)、テトラヒドロフラン40.5gにより調製した溶液を氷冷下で滴下した。次いで、N,N’−ジ−sec−ブチル−1,4−ジアザ−1,3−ブタジエン7.50g(0.044mol)、テトラヒドロフラン39.1g、Li0.59g(0.085mol)により調製した溶液を滴下し、滴下後室温に戻し17時間攪拌し、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度140℃、圧力96Pa、塔頂温度120℃で蒸留を行い、暗褐色液体を得た。収量は8.20g、収率は58%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:226℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:9.766mg)
(2)減圧TG−DTA
質量50%減少温度:145℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:9.821mg)
(3)元素分析(金属分析:ICP−AES)
コバルト含有量:16.5質量%(理論値 16.04質量%)
CHN分析:C59.6%(理論値58.9%)、H10.0%(理論値9.9%)、N15.1%(理論値15.3%)
300mlの4つ口フラスコに、塩化コバルト(II)10.0g(0.077mol)、テトラヒドロフラン54.2gを仕込み、室温下で撹拌した。その中に、N,N’−ジイソプロピル−1,4−ジアザ−1,3−ブタジエン10.9g(0.078mol)、テトラヒドロフラン67.7gにより調製した溶液を氷冷下で滴下した。次いでN,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン14.3g(0.085mol)、テトラヒドロフラン82.9g、Li1.19g(0.17mol)により調製した溶液を滴下し、滴下後室温に戻し15時間攪拌した。バス温度100℃、微減圧下で溶媒を留去した後、n−ヘプタンにより溶媒交換を行い、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度140℃、圧力54Pa、塔頂温度114℃で蒸留を行い、濃褐色固体を得た。収量は23.2g、収率は82%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:231℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:10.21mg)
(2)減圧TG−DTA
質量50%減少温度:146℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:9.324mg)
(3)元素分析(金属分析:ICP−AES)
コバルト含有量:16.0質量%(理論値 16.04質量%)
CHN分析:C59.0%(理論値58.9%)、H10.0%(理論値9.9%)、N15.1%(理論値15.3%)
200mlの4つ口フラスコに、塩化コバルト(II)5.09g(0.039mol)、テトラヒドロフラン44.6gを仕込み、室温下で撹拌した。その中に、N,N’−ジ−sec−ブチル−1,4−ジアザ−1,3−ブタジエン6.65g(0.039mol)を氷冷下で滴下した。次いでN,N’−ジイソプロピル−1,4−ジアザ−1,3−ブタジエン5.97g(0.042mol)、テトラヒドロフラン38.0g、Li0.59g(0.085mol)により調製した溶液を滴下し、滴下後室温に戻し21時間攪拌し、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度145℃、圧力90Pa、塔頂温度129℃で蒸留を行い、暗褐色液体を得た。収量は7.28g、収率は51%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:230℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:9.737mg)
(2)減圧TG−DTA
質量50%減少温度:149℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:9.802mg)
(3)元素分析(金属分析:ICP−AES)
コバルト含有量:16.2質量%(理論値 16.04質量%)
CHN分析:C58.1%(理論値58.9%)、H9.3%(理論値9.9%)、N15.1%(理論値15.7%)
500mlの4つ口フラスコに、塩化コバルト(II)15.0g(0.12mol)、テトラヒドロフラン45.6gを仕込み、室温下で撹拌した。その中に、N,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン19.7g(0.12mol)、テトラヒドロフラン81.9gにより調製した溶液を氷冷下で滴下した。次いでN,N’−ジイソプロピル−1,4−ジアザ−1,3−ブタジエン17.8g(0.12mol)、テトラヒドロフラン121g、Li1.76g(0.25mol)により調製した溶液を滴下し、滴下後室温に戻し18時間攪拌した。バス温度95℃、微減圧下で溶媒を留去した後、n−ヘプタンにより溶媒交換を行い、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度140℃、圧力110Pa、塔頂温度133℃で蒸留を行い、濃褐色固体を得た。収量は25.4g、収率は60%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:227℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:10.00mg)
(2)減圧TG−DTA
質量50%減少温度:144℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:10.07mg)
(3)元素分析(金属分析:ICP−AES)
コバルト含有量:16.1質量%(理論値 16.04質量%)
CHN分析:C58.7%(理論値58.9%)、H9.2%(理論値9.9%)、N15.9%(理論値15.3%)
200mlの4つ口フラスコに、塩化コバルト(II)5.05g(0.039mol)、テトラヒドロフラン43.3gを仕込み、室温下で撹拌した。その中に、N,N’−ジ−nプロピル−1,4−ジアザ−1,3−ブタジエン5.60g(0.040mol)を氷冷下で滴下した。次いでN,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン7.36g(0.044mol)、テトラヒドロフラン40.8g、Li0.59g(0.085mol)により調製した溶液を滴下し、滴下後室温に戻し17時間攪拌した。バス温度90℃、微減圧下で溶媒を留去した後、n−ヘプタンにより溶媒交換を行い、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度145℃、圧力56Pa、塔頂温度110℃で蒸留を行い、濃緑色液体を得た。収量は6.97g、収率は49%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:227℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:9.688mg)
(2)減圧TG−DTA
質量50%減少温度:146℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:10.31mg)
(3)元素分析(金属分析:ICP−AES)
コバルト含有量:16.2質量%(理論値 16.04質量%)
CHN分析:C58.2%(理論値58.9%)、H9.3%(理論値9.9%)、N15.7%(理論値15.3%)
200mlの4つ口フラスコに、塩化ニッケル(II)4.0g(0.031mol)、テトラヒドロフラン23.8gを仕込み、室温下で撹拌した。その中に、N,N’−ジイソプロピル−1,4−ジアザ−1,3−ブタジエン4.33g(0.031mol)、テトラヒドロフラン19.7gにより調製した溶液を氷冷下で滴下した。次いでN,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン5.19g(0.031mol)、テトラヒドロフラン37.4g、Li0.42g(0.062mol)により調製した溶液を滴下し、滴下後室温に戻し20時間攪拌した。バス温度70℃、微減圧下で溶媒を留去した後、n−ヘキサンにより溶媒交換を行い、濾過を行った。得られた濾液から溶媒を除去し、クーゲルロールを用いて残渣を105℃、30Paの条件下で精製して暗赤色固体を得た。収量は1.81g、収率は16%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:210℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:9.980mg)
(2)減圧TG−DTA
質量50%減少温度:142℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:9.698mg)
(3)1H−NMR(溶媒:重ベンゼン)(ケミカルシフト:多重度:H数)
(8.934−8.948:d:2)(8.733−8.738:d:2)(2.785−2.834:m:1)(2.603−2.667:m:1)(1.941:s:9)(1.908−1.925:d:6)(1.899:s:9)(1.839−1.856:d:6)
(4)元素分析(金属分析:ICP−AES)
ニッケル含有量:質量16.2%(理論値質量16.0%)
CHN分析:C59.3%(理論値58.9%)、H10.2%(理論値9.9%)、N15.9%(理論値15.3%)
500mlの4つ口フラスコに、塩化マンガン(II)10.0g(0.080mol)、テトラヒドロフラン49.5gを仕込み、室温下で撹拌した。その中に、N,N’−ジイソプロピル−1,4−ジアザ−1,3−ブタジエン11.1g(0.080mol)、テトラヒドロフラン54.6gにより調製した溶液を氷冷下で滴下した。次いでN,N’−ジ−tert−ブチル−1,4−ジアザ−1,3−ブタジエン13.4g(0.080mol)、テトラヒドロフラン79.2g、Li1.10g(0.16mol)により調製した溶液を滴下し、滴下後室温に戻し15時間攪拌した。バス温度90℃、微減圧下で溶媒を留去した後、n−ヘキサンにより溶媒交換を行い、濾過を行った。得られた濾液から溶媒を除去し、残渣をバス温度128℃、圧力60Pa、塔頂温度118℃で蒸留を行い、黒色固体である目的物を得た。収量は12.8g、収率は44%であった。
(分析値)
(1)常圧TG−DTA
質量50%減少温度:219℃(Ar流量:100ml/分、昇温10℃/分、サンプル量:9.805mg)
(2)減圧TG−DTA
質量50%減少温度:140℃(10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量:9.847mg)
(3)元素分析(金属分析:ICP−AES)
マンガン含有量:15.5質量%(理論値15.1質量%)
CHN分析:C60.3%(理論値59.5%)、H10.2%(理論値10.0%)、N15.2%(理論値15.4%)
化合物No.2、3、5、6および9並びに下記に示す比較化合物1について、目視によって常圧30℃における各化合物の状態を観察し、固体化合物については微小融点測定装置を用いて融点を測定した。化合物No.2、3、5、6および9並びに下記に示す比較化合物1について、示差操作熱量測定(DSC)を用いて熱分解が開始する温度を測定した。化合物No.2、3、5、6および9並びに下記に示す比較化合物1について、TG−DTAを用いて重量が50%減少した際の温度を測定した。結果を表1に示す。
TD−GTA測定条件:10Torr、Ar流量:50ml/分、昇温10℃/分、サンプル量約10mg
化合物No.30及び下記に示す比較化合物2について、目視によって常圧30℃における各化合物の状態を観察し、固体化合物については微小融点測定装置を用いて融点を測定した。化合物No.30及び下記に示す比較化合物2について、DSCを用いて熱分解が開始する温度を測定した。結果を表2に示す。
化合物No.39及び下記に示す比較化合物3について、目視によって常圧30℃における各化合物の状態を観察し、固体化合物については微小融点測定装置を用いて融点を測定した。化合物No.39及び下記に示す比較化合物3について、DSCを用いて熱分解が開始する温度を測定した。結果を表3に示す。
化合物No.2、3、5、6および9を化学気相成長用原料とし、図1に示すALD装置を用いて以下の条件のALD法により、Cu基板上に各々金属コバルト薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法(XPS分析)による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は3〜6nmであり、膜組成は金属コバルト(XPS分析によるCo2pピークで確認)であり、炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。
(条件)
反応温度(基板温度):270℃、反応性ガス:水素ガス
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、150サイクル繰り返した:
(1)原料容器加熱温度:100℃、原料容器内圧力100Paの条件で気化させた化学気相成長用原料の蒸気を導入し、系圧100Paで30秒間堆積させる;
(2)5秒間のアルゴンパージにより、未反応原料を除去する;
(3)反応性ガスを導入し、系圧力100Paで30秒間反応させる;
(4)5秒間のアルゴンパージにより、未反応原料を除去する。
比較化合物1を化学気相成長用原料とし、実施例8と同様の方法でCu基板上に金属コバルト薄膜の製造を試みたが、平滑な薄膜を得ることはできなかった。Cu基板上に形成されたCo含有物中の炭素含有量は10%以上であった。
(条件)
反応温度(基板温度):270℃、反応性ガス:水素ガス
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、150サイクル繰り返した:
(1)原料容器加熱温度:100℃、原料容器内圧力100Paの条件で気化させた化学気相成長用原料の蒸気を導入し、系圧100Paで30秒間堆積させる;
(2)5秒間のアルゴンパージにより、未反応原料を除去する;
(3)反応性ガスを導入し、系圧力100Paで30秒間反応させる;
(4)5秒間のアルゴンパージにより、未反応原料を除去する。
化合物No.30を化学気相成長用原料とし、図1に示すALD装置を用いて以下の条件のALD法により、Cu基板上に金属ニッケル薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は3〜6nmであり、膜組成は金属ニッケル(XPS分析によるNi2pピークで確認)であり、炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。
(条件)
反応温度(基板温度):220℃、反応性ガス:水素ガス
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、150サイクル繰り返した:
(1)原料容器加熱温度:100℃、原料容器内圧力100Paの条件で気化させた化学気相成長用原料の蒸気を導入し、系圧100Paで30秒間堆積させる;
(2)5秒間のアルゴンパージにより、未反応原料を除去する;
(3)反応性ガスを導入し、系圧力100Paで30秒間反応させる;
(4)5秒間のアルゴンパージにより、未反応原料を除去する。
化合物No.39を化学気相成長用原料とし、図1に示すALD装置を用いて以下の条件のALD法により、Cu基板上に金属マンガン薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は3〜6nmであり、膜組成は金属マンガン(XPS分析によるMn2pピークで確認)であり、炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。
(条件)
反応温度(基板温度):240℃、反応性ガス:水素ガス
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、150サイクル繰り返した:
(1)原料容器加熱温度:100℃、原料容器内圧力100Paの条件で気化させた化学気相成長用原料の蒸気を導入し、系圧100Paで30秒間堆積させる;
(2)5秒間のアルゴンパージにより、未反応原料を除去する;
(3)反応性ガスを導入し、系圧力100Paで30秒間反応させる;
(4)5秒間のアルゴンパージにより、未反応原料を除去する。
Claims (5)
- 一般式(I)または一般式(II)において、Mが銅、鉄、ニッケル、コバルト又はマンガンである、請求項1に記載の化合物。
- 一般式(I)または一般式(II)において、nが1である、請求項1または2に記載の化合物。
- 請求項1ないし3のいずれか一項に記載の化合物を含有してなる薄膜形成用原料。
- 請求項4に記載の薄膜形成用原料を気化させて得られる化合物を含有する蒸気を、基体が設置された成膜チャンバー内に導入し、該化合物を分解及び/又は化学反応させて該基体の表面に金属原子及びケイ素原子から選ばれる少なくとも1種の原子を含有する薄膜を形成する薄膜の製造方法。
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EP16811362.9A EP3312187A4 (en) | 2015-06-17 | 2016-05-17 | METHOD FOR PRODUCING A NOVEL COMPOUND, RAW MATERIAL FOR THIN LAYERING AND THIN LAYER |
CN201680025896.6A CN107531734A (zh) | 2015-06-17 | 2016-05-17 | 新型的化合物、薄膜形成用原料和薄膜的制造方法 |
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JP2022512154A (ja) * | 2018-12-19 | 2022-02-02 | ハンソル ケミカル カンパニー リミテッド | コバルト前駆体、その製造方法およびこれを用いた薄膜の製造方法 |
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CN110128373B (zh) * | 2019-06-12 | 2023-03-24 | 鸿翌科技有限公司 | 哌嗪基锡配合物及其制备方法、薄膜、太阳能电池 |
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US20180051372A1 (en) | 2018-02-22 |
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