JP2017538040A - 金属及び金属アロイの無電解めっきのためのめっき浴組成物 - Google Patents
金属及び金属アロイの無電解めっきのためのめっき浴組成物 Download PDFInfo
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- JP2017538040A JP2017538040A JP2017532092A JP2017532092A JP2017538040A JP 2017538040 A JP2017538040 A JP 2017538040A JP 2017532092 A JP2017532092 A JP 2017532092A JP 2017532092 A JP2017532092 A JP 2017532092A JP 2017538040 A JP2017538040 A JP 2017538040A
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- Prior art keywords
- plating bath
- metal
- electroless
- plating
- acid
- Prior art date
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- BSXVKCJAIJZTAV-UHFFFAOYSA-L copper;methanesulfonate Chemical compound [Cu+2].CS([O-])(=O)=O.CS([O-])(=O)=O BSXVKCJAIJZTAV-UHFFFAOYSA-L 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
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- 150000002169 ethanolamines Chemical class 0.000 description 1
- HCPOCMMGKBZWSJ-UHFFFAOYSA-N ethyl 3-hydrazinyl-3-oxopropanoate Chemical compound CCOC(=O)CC(=O)NN HCPOCMMGKBZWSJ-UHFFFAOYSA-N 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
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- 239000011737 fluorine Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 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 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- NMUOATVLLQEYHI-UHFFFAOYSA-N iminoaspartic acid Chemical compound OC(=O)CC(=N)C(O)=O NMUOATVLLQEYHI-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 description 1
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- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- XKPJKVVZOOEMPK-UHFFFAOYSA-M lithium;formate Chemical compound [Li+].[O-]C=O XKPJKVVZOOEMPK-UHFFFAOYSA-M 0.000 description 1
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- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 238000001579 optical reflectometry Methods 0.000 description 1
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- 229960003104 ornithine Drugs 0.000 description 1
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
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- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
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- NBOMNTLFRHMDEZ-UHFFFAOYSA-N thiosalicylic acid Chemical compound OC(=O)C1=CC=CC=C1S NBOMNTLFRHMDEZ-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/02—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton
- C07C229/04—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
- C07C229/06—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton
- C07C229/10—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton the nitrogen atom of the amino group being further bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
- C07C229/12—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton the nitrogen atom of the amino group being further bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings to carbon atoms of acyclic carbon skeletons
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C237/00—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups
- C07C237/02—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atoms of the carboxamide groups bound to acyclic carbon atoms of the carbon skeleton
- C07C237/04—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atoms of the carboxamide groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being acyclic and saturated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
- C23C18/1641—Organic substrates, e.g. resin, plastic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
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- Inorganic Chemistry (AREA)
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
- R1は、-O-R3及び-NH-R4からなる群から選択され、ここで、R3は、水素、リチウム、ナトリウム、カリウム、ルビジウム、セシウム、アンモニウム、アルキル、アリールから選択され、R4は、水素、アルキル、及びアリールから選択され;
- R2は、水素、アルキル、アルキルアリール、及びアリールからなる群から選択され;
- Yは、
- Zは、
- nは、1から2の範囲の整数である)
に従うめっき速度調整剤(plating rate modifier)を更に含むことを特徴とする、無電解めっき浴によって解決される。
(i)基材を用意する工程;
(ii)前記基材を、少なくとも1つの金属イオン源、少なくとも1つの還元剤、及び少なくとも1つの式(I)に従うめっき速度調整剤を含む無電解めっき浴と接触させ、それによって、前記基材の少なくとも一部分上に金属又は金属アロイの層を堆積させる工程
を含む、金属又は金属アロイを堆積させるための本発明の方法によっても解決される。
(i)基材を用意する工程;
(ii)前記基材を、少なくとも1つの金属イオン源、少なくとも1つの還元剤、及び少なくとも1つのめっき速度調整剤を含む無電解めっき浴と接触させ、それによって、前記基材の少なくとも一部分上に金属又は金属アロイの層を堆積させる工程
を含む。
(i.a)基材を前処理する工程
を更に含んでよい。
金属又は金属アロイをその上に堆積するために用いた基材は、この順で二酸化ケイ素(5から500nm)、窒化タンタル(3から30nm)、タンタル(3から30nm)、及び最終ルテニウムライナー層(2から10nm)からなる層接合体(layer assembly)を有するシリコンから作製されたウエハ基材であった。前記最終ルテニウムライナー層を、適切な還元剤(ジエチレングリコール中の還元剤としての2g/lのジメチルアミノボラン(DMAB)からなる溶液(t=5分、T=70℃))で還元する。
リン含有量及び堆積物厚さを、XRF装置Fischerscope XDV-SDD(Helmut Fischer GmbH社、ドイツ)を用いたXRFにより、各基材の5点で測定した。堆積物の層状構造を仮定することにより、そのようなXRFデータから層厚さを算出することができる。めっき速度は、得られた層厚さを、前記層厚さを得るために必要な時間で除することによって算出した。
金属及び金属アロイ堆積物の光沢は、目視検査によって特定した。
金属又は金属アロイ層の外側表面の平滑性を、走査型原子間力顕微鏡(先端半径7nm未満のNanosensors社製PointProbe(登録商標)を備えたDigital Instruments社、Nano-Scope)を用い、スキャンサイズ:5×5μm、タッピングモードでのスキャンによって特定した。SQ値(二乗平均平方根粗さ)がこれらの測定から得られ、対応する以下の例に示す。
質量スペクトルは、LC-MS装置Bruker MicroTOF II(溶離液A:5mmolギ酸アンモニウム水溶液、溶離液B:アセトニトリル、勾配系 溶離液A:溶離液B=95:5(体積/体積)、検出器:ESI-TOF MS、ギ酸リチウム及び/又はギ酸ナトリウムで較正(質量依存))を用いて得た。
ガラス反応器中、10.55g(117mmol)のβ-アラニンを、72.74gの水に溶解し、その後、4.74g(118.5mmol)の水酸化ナトリウムをこの溶液に添加した。両化合物を完全に溶解した後、この均一な無色溶液を60℃に加熱した。11分間以内で、11.97g(58.6mmol)のグリセロールジグリシジルエーテルをこの溶液に滴下した。その後、この反応混合物を、更に39時間にわたって60℃に加熱し、その後25℃に冷却した。水を補給して100gの合計質量とした後、めっき速度調整剤の25質量パーセント水溶液を得た。
ガラス反応器に、8.16mLの水を投入した。23.47g(78mmol)の50質量パーセント水酸化セシウム水溶液を、この溶媒にゆっくり溶解させた。更に7分以内に、10.37g(78mmol)のロイシンを添加し、それによって、無色透明の溶液を得た。この反応混合物を60℃に加熱し、19分以内に、78g(39.1mmol、50質量パーセント水溶液、Mn=1000Da)のポリエチレンジグリシジルエーテルを滴下した。この反応混合物を、所与の温度で更に5.5時間撹拌し、その後室温に冷却した。めっき速度調整剤の透明な明るい黄色の溶液120gを得た(40質量パーセント水溶液)。
ガラス反応器に、65.58mLの水を投入した。23.47g(78mmol)の50質量パーセント水酸化セシウム水溶液を、この溶媒にゆっくり溶解させた。更に7分以内に、10.37g(78mmol)のロイシンを添加し、それによって、無色透明の溶液を得た。この反応混合物を60℃に加熱し、14分以内に、20.58g(39.1mmol、Mn=526Da)のポリエチレンジグリシジルエーテルを滴下した。この反応混合物を、所与の温度で更に5.5時間撹拌し、その後室温に冷却した。めっき速度調整剤の透明な僅かに黄色の溶液120gを得た(40質量パーセント水溶液)。
ガラス反応器に、30.37mLの水を投入した。33.0g(110mmol)の50質量パーセント水酸化セシウム水溶液を、この溶媒にゆっくり溶解させた。更に5分以内に、14.6g(110mmol)のロイシンを添加し、それによって、無色透明の溶液を得た。この反応混合物を60℃に加熱し、20分以内に、22.03g(55.1mmol、Mn=200Da)のポリエチレンジグリシジルエーテルを滴下した。この反応混合物を、所与の温度で更に1時間撹拌し、その後室温に冷却した。水を充分な量で添加して、めっき速度調整剤の透明な黄色溶液100gを得た(34.7質量パーセント水溶液)。
ガラス反応器に、30.76mLの水を投入した。34.2g(114mmol)の50質量パーセント水酸化セシウム水溶液を、この溶媒にゆっくり溶解させた。更に5分以内に、15.14g(114mmol)のロイシンを添加し、それによって、無色透明の溶液を得た。この反応混合物を60℃に加熱し、20分以内に、19.90g(57.1mmol)のエチレンジグリシジルエーテルを滴下した。この反応混合物を、所与の温度で更に1時間撹拌し、その後室温に冷却した。この反応混合物を、300mLの水で希釈し、めっき速度調整剤の無色透明溶液を得た(9.7質量パーセント水溶液)。
ガラス反応器に、26.69mLの水を投入した。33.0g(110mmol)の50質量パーセント水酸化セシウム水溶液を、この溶媒にゆっくり溶解させた。5分以内に、9.41g(71mmol)のロイシンを添加し、それによって、無色透明の溶液を得た。この反応混合物を60℃に加熱し、16分以内に、42.6g(35.5mmol、Mn=600Da)のポリプロピレンジグリシジルエーテルを滴下した。この反応混合物を、所与の温度で更に1時間撹拌し、その後室温に冷却した。水を充分な量で添加して、めっき速度調整剤の透明な黄色溶液100gを得た(42.1質量パーセント水溶液)。
ニッケルめっき(比較例)
ニッケル塩、様々な濃度cのβ-アラニン、及び以下に挙げるさらなる添加剤を水に溶解することにより、無電解ニッケルめっき浴を調製した。
ニッケルリン層の堆積(発明例)
合成例1のめっき速度調整剤を用いて、適用例1に記載した実験を繰り返した。めっき速度調整剤の濃度と関連した得られためっき速度を特定し、これは、以下の表2に見出すことができる。
無電解銅めっき浴のめっき速度
銅塩、様々な濃度cのめっき速度調整剤、及び塩基(水酸化ナトリウム及び水酸化セシウム)、及び典型的な錯化剤を水に溶解することにより、無電解銅めっき浴を調製した。前記無電解銅めっき浴中の銅イオンの濃度は、3.25g/lであった。グリオキシル酸を、還元剤として用い、ギ酸を、増強剤として添加した。めっき浴のpHは、表3に示す塩基により、12から13の間であり、これらを、基材上への銅の堆積のために、35℃に加熱した。基材を、めっき浴中に20分間浸漬した。堆積の間、めっき浴に窒素をパージした。添加剤及び塩基の濃度と関連しためっき速度は、表3に見出すことができる。
無電解コバルトタングステンめっき浴のめっき速度
以下の成分を水に溶解することにより、コバルトタングステンめっき浴を調製した。
無電解コバルトタングステンめっき浴のめっき速度
100mg/lの合成例1を、適用例4で述べたように無電解コバルトタングステンめっき浴に添加した。同様に、上記で説明した例で用いたものと同じ基材を用いて、その上にめっきを行った。無電解コバルトタングステンめっき浴の相対的めっき速度は、20.2%低下した(添加剤を含まない無電解コバルトタングステンめっき浴と比較して)。したがって、めっき速度は、めっき速度調整剤によって明確に低下した。
PEG及びめっき速度調整剤を含有する無電解めっき浴のめっき速度の比較
適用例3で述べた無電解銅めっき浴(水酸化物源を含有)を用いて、めっき速度及びめっき浴安定性に対するポリエチレングリコール及びめっき速度調整剤の効果を比較した。したがって、合成例2のめっき速度調整剤(発明例)及びポリエチレングリコールPEG600(比較例)を、めっき浴に溶解した。次に、基材をめっき浴中に浸漬した(T=35℃、t=20分)。添加剤と関連して得られためっき速度は、表5に見出すことができる。
無電解銅めっき浴の安定性
適用例3で述べたようにして無電解銅めっき浴(水酸化物源を含有)を調製した。異なるめっき速度調整剤を含有する無電解めっき浴を、24時間放置し、次に、何らかの析出物について目視で検査した。更に、2つの例示のめっき浴の残留銅濃度を調べた。
Claims (15)
- 銅、ニッケル、コバルト、又はこれらのアロイを堆積させるための無電解めっき浴であって、少なくとも1つの金属イオン源及び少なくとも1つの還元剤を含み、式(I)
- R1は、-O-R3及び-NH-R4からなる群から選択され、ここで、R3は、水素、リチウム、ナトリウム、カリウム、ルビジウム、セシウム、アンモニウム、アルキル、アリールから選択され、R4は、水素、アルキル、及びアリールから選択され;
- R2は、水素、アルキル、アルキルアリール、及びアリールからなる群から選択され;
- Yは、
- Zは、
- nは、1から2の範囲の整数である)
に従うめっき速度調整剤を更に含むことを特徴とする、無電解めっき浴。 - 前記めっき速度調整剤の残基R5からR8が、非分岐鎖状飽和C1-からC6-アルキレン残基であり、ここで、前記非分岐鎖状飽和アルキレン残基に結合した個々の水素はそれぞれ、アルキル、アリール、及びヒドロキシルから選択される官能基によって任意選択で置換されていることを特徴とする、請求項1又は2に記載の無電解めっき浴。
- 前記めっき速度調整剤の残基R5からR8が、エタン-1,2-ジイル(-CH2-CH2-)、プロパン-1,2-ジイル(-CH(CH3)-CH2-)、ブタン-1,2-ジイル(-CH(CH2-CH3)-CH2-)、及び2-ヒドロキシプロパン-1,3-ジイル(-CH2-CH(OH)-CH2-)からなる群から選択される、請求項1から3のいずれか一項に記載の無電解めっき浴。
- 式(I)に従う前記めっき速度調整剤が、無電解めっき浴中に、0.1から1500μmol/lの濃度で含有されることを特徴とする、請求項1から4のいずれか一項に記載の無電解めっき浴。
- 前記金属イオン源が、水溶性の銅塩、ニッケル塩、及びコバルト塩、並びに水溶性の銅化合物、ニッケル化合物、及びコバルト化合物から選択される、請求項1から5のいずれか一項に記載の無電解めっき浴。
- 安定化剤を更に含む、請求項1から6のいずれか一項に記載の無電解めっき浴。
- 前記金属イオン源が、水溶性ニッケル塩、及び水溶性ニッケル化合物から選択され、前記還元剤が、次亜リン酸塩化合物、ホウ素系還元剤、ホルムアルデヒド、ヒドラジン、及びこれらの混合物から選択される、請求項6又は7に記載の無電解めっき浴。
- 前記金属イオン源が、水溶性コバルト塩、及び水溶性コバルト化合物から選択され、前記還元剤が、次亜リン酸塩化合物、ホウ素系還元剤、ホルムアルデヒド、ヒドラジン、及びこれらの混合物から選択される、請求項6又は7に記載の無電解めっき浴。
- 前記金属イオン源が、水溶性銅塩、及び水溶性銅化合物から選択され、少なくとも1つの前記還元剤が、ホルムアルデヒド、パラホルムアルデヒド、グリオキシル酸、グリオキシル酸源、アミノボラン、水素化ホウ素アルカリ金属塩、ヒドラジン、ポリサッカリド、糖、次亜リン酸、グリコール酸、ギ酸、前述の酸の塩、及びこれらの混合物からなる群から選択される、請求項6又は7に記載の無電解めっき浴。
- (i)基材を用意する工程、
(ii)前記基材を、請求項1から10のいずれか一項に記載の無電解めっき浴と接触させ、それによって、前記基材の少なくとも一部分上に金属又は金属アロイを堆積させる工程
を含む、金属又は金属アロイを堆積させるための方法。 - (i.a)前記基材を前処理する工程
を更に含む、請求項11に記載の金属又は金属アロイを堆積させるための方法。 - 前記基材が、ガラス、プラスチック、シリコン、絶縁体、及び金属基材からなる群から選択される、請求項11又は12に記載の金属又は金属アロイを堆積させるための方法。
- 前記基材が、プリント回路板、チップキャリア、半導体ウエハ、回路キャリア、及び相互接続デバイスから選択される、請求項13に記載の金属又は金属アロイを堆積させるための方法。
- 前記基材が、ポリイミド(PI)及びポリエチレンテレフタレート(PET)ホイルから選択される、請求項13に記載の金属又は金属アロイを堆積させるための方法。
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PCT/EP2015/078679 WO2016096480A1 (en) | 2014-12-16 | 2015-12-04 | Plating bath compositions for electroless plating of metals and metal alloys |
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EP3271500B1 (en) | 2015-03-20 | 2018-06-20 | ATOTECH Deutschland GmbH | Activation method for silicon substrates |
TWI707061B (zh) * | 2015-11-27 | 2020-10-11 | 德商德國艾托特克公司 | 鈀之電鍍浴組合物及無電電鍍方法 |
TWI713737B (zh) | 2016-05-04 | 2020-12-21 | 德商德國艾托特克公司 | 沉積金屬或金屬合金至基板表面及包含基板表面活化之方法 |
ES2826441T3 (es) | 2017-06-02 | 2021-05-18 | Atotech Deutschland Gmbh | Baños de metalizado no electrolítico de aleación de níquel, un método de deposición de aleaciones de níquel, depósitos de aleación de níquel y usos de dichos depósitos de aleación de níquel formados |
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JP7441056B2 (ja) | 2019-08-07 | 2024-02-29 | イビデン株式会社 | 銅めっき廃液からの銅析出法およびそれを用いた銅分離回収装置 |
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US9909216B2 (en) | 2018-03-06 |
KR20170093870A (ko) | 2017-08-16 |
ES2639300T3 (es) | 2017-10-26 |
US20170327954A1 (en) | 2017-11-16 |
TWI667371B (zh) | 2019-08-01 |
EP3034650B1 (en) | 2017-06-21 |
TW201625814A (zh) | 2016-07-16 |
CN107002241B (zh) | 2019-07-30 |
CN107002241A (zh) | 2017-08-01 |
KR101943246B1 (ko) | 2019-01-28 |
WO2016096480A1 (en) | 2016-06-23 |
CA2970560A1 (en) | 2016-06-23 |
JP6726186B2 (ja) | 2020-07-22 |
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