CH656401A5 - METHOD FOR ELECTRICALLY DEPOSITING METALS. - Google Patents
METHOD FOR ELECTRICALLY DEPOSITING METALS. Download PDFInfo
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- CH656401A5 CH656401A5 CH3992/83A CH399283A CH656401A5 CH 656401 A5 CH656401 A5 CH 656401A5 CH 3992/83 A CH3992/83 A CH 3992/83A CH 399283 A CH399283 A CH 399283A CH 656401 A5 CH656401 A5 CH 656401A5
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- solution
- hydrocarbon
- anion radical
- dissolved
- metals
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- 229910052751 metal Inorganic materials 0.000 title claims description 24
- 239000002184 metal Substances 0.000 title claims description 24
- 238000000034 method Methods 0.000 title claims description 21
- 150000002739 metals Chemical class 0.000 title claims description 12
- 238000000151 deposition Methods 0.000 title description 4
- 239000000758 substrate Substances 0.000 claims description 16
- 150000002430 hydrocarbons Chemical class 0.000 claims description 12
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 11
- 229930195733 hydrocarbon Natural products 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 10
- 239000003125 aqueous solvent Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000003638 chemical reducing agent Substances 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910020968 MoSi2 Inorganic materials 0.000 description 2
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 229910003822 SiHCl3 Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- -1 tetraalkylammonium halide Chemical class 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 101100277038 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) dbp-5 gene Proteins 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012457 nonaqueous media Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- DPKBAXPHAYBPRL-UHFFFAOYSA-M tetrabutylazanium;iodide Chemical compound [I-].CCCC[N+](CCCC)(CCCC)CCCC DPKBAXPHAYBPRL-UHFFFAOYSA-M 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Electrodes Of Semiconductors (AREA)
Description
Die vorliegende Erfindung bezieht sich auf die Abscheidung von Metallen oder Halbleitern durch chemische Reduktion in nichtwässrigen Lösungsmitteln in Pulverform oder als bevorzugte Alternative, in Form von festhaftenden Schichten auf geeigneten Unterlagen. The present invention relates to the deposition of metals or semiconductors by chemical reduction in non-aqueous solvents in powder form or as a preferred alternative, in the form of firmly adhering layers on suitable substrates.
Zur Abscheidung von Metallen, besonders in Form von auf Unterlagen festhaftenden Schichten, gibt es heute elektrolytische und rein chemische Verfahren in wässrigen Lösungen, die zu genügend guten Resultaten für Metalle, die diesen Lösungen gegenüber beständig sind, wie z.B. Au, Ni, Cr und andere, führen. Diese Verfahren sind jedoch prinzipiell für Metalle, die unedler als Wasser sind, nicht anwendbar. Es ist jedoch von höchstem technischem und wirtschaftlichem Interesse, Metalle oder Halbleiter wie z.B. Silizium für photo-voltaische Zellen zur Sonnenenergiegewinnung, Molybdän, Aluminium oder Tantal und ähnliche als korrosionsfeste Überzüge, oder intermetallische Verbindungen wie z.B. For the deposition of metals, particularly in the form of layers adhering to substrates, there are now electrolytic and purely chemical processes in aqueous solutions that give sufficiently good results for metals that are resistant to these solutions, e.g. Au, Ni, Cr and others. In principle, however, these processes cannot be used for metals that are less noble than water. However, it is of the highest technical and economic interest to use metals or semiconductors such as e.g. Silicon for photovoltaic cells for solar energy generation, molybdenum, aluminum or tantalum and the like as corrosion-resistant coatings, or intermetallic compounds such as e.g.
MoSi2 als harte, verschleissfeste Überzüge in Form festhaftender Schichten auf geeigneten Unterlagen abzuschneiden. Cut off MoSi2 as hard, wear-resistant coatings in the form of firmly adhering layers on suitable underlays.
Es ist möglich, solche Metalle oder Halbleiter durch elektrolytische Reduktion in geschmolzenen Salzen oder in nichtwässrigen Lösungsmitteln abzuscheiden. Solche Verfahren sind z.B. für Silizium im Journal of the Electrochemical Society 128, Seite 1708-1711 (1981), oder im U.S. Patent 3 990 953 beschrieben worden. Elektrolytischen Verfahren haftet jedoch allgemein der Nachteil an, dass die Unterlagen, auf denen das Metall abgeschieden werden soll, elektrisch leitend sein und mit einer Stromquelle verbunden werden müssen. Bei Elementen wie z.B. Silizium kommt als Nachteil hinzu, dass deren geringe Leitfähigkeit die Geschwindigkeit der elektrolytischen Abscheidung herabsetzt. Wenn die elektrolytische Abscheidung in geschmolzenen Salzen durchgeführt wird, kommen alle Nachteile und Schwierigkeiten des Arbeitens bei höheren Temperaturen hinzu. Die rein chemische Abscheidung eines Metalles aus einer Lösung einer seiner Verbindungen, wie z.B. das bekannte Vernickeln, umgeht diese Nachteile. It is possible to deposit such metals or semiconductors by electrolytic reduction in molten salts or in non-aqueous solvents. Such methods are e.g. for silicon in Journal of the Electrochemical Society 128, pages 1708-1711 (1981), or in U.S. 3,990,953. However, electrolytic processes generally have the disadvantage that the supports on which the metal is to be deposited are electrically conductive and have to be connected to a power source. For elements such as Another disadvantage of silicon is that its low conductivity reduces the speed of electrodeposition. When electrodeposition is carried out in molten salts, there are all the disadvantages and difficulties of working at higher temperatures. The purely chemical deposition of a metal from a solution of one of its compounds, e.g. the well-known nickel plating avoids these disadvantages.
Bei diesem Verfahren wird einer Lösung einer geeigneten Metallverbindung ein Reduktionsmittel hinzugefügt, wodurch das Metall reduziert wird und entweder in Pulverform ausfallt oder aber auf einer Unterlage als festhaftende Schicht abgeschieden wird. Zur Gewinnung von reinem Silizium ist ein solches Verfahren z.B. im Deutschen Patent No DBP 5 1 071 680 beschrieben worden: als Lösungsmittel wird eines der bekannten nichtwässrigen Lösungsmittel verwendet, indem eine Siliziumverbindung, wie z.B. SiCl4 gelöst wird. Als Reduktionsmittel wird eine Dispersion von Natrium verwendet. Es gelingt so, Silizium in Pulverform zu gewinnen, das 10 von der Natriumdispersion getrennt werden muss. Die Verwendung eines unlöslichen Reduktionsmittels hat also den Nachteil eines zusätzlichen Verfahrensschrittes bei der Gewinnung von Metallen in Pulverform. Eine Abscheidung des Metalles in Form einer festhaftenden Schicht auf einer Unter-i5 läge ist mit einem unlöslichen Reduktionsmittel überhaupt kaum möglich. In this method, a reducing agent is added to a solution of a suitable metal compound, as a result of which the metal is reduced and either precipitates in powder form or is deposited on a base as a firmly adhering layer. To obtain pure silicon, such a process is e.g. in German Patent No DBP 5 1 071 680: one of the known non-aqueous solvents is used as the solvent by adding a silicon compound, e.g. SiCl4 is dissolved. A dispersion of sodium is used as the reducing agent. It is thus possible to obtain silicon in powder form, which 10 has to be separated from the sodium dispersion. The use of an insoluble reducing agent therefore has the disadvantage of an additional process step in the extraction of metals in powder form. It is hardly possible to deposit the metal in the form of a firmly adhering layer on an underlay with an insoluble reducing agent.
Die vorliegende Erfindung umgeht alle diese beschriebenen Nachteile. Es wurde nämlich gefunden, dass es gelingt Halbleiter wie Silizium, oder Metalle wie Molybdän, Tantal, 20 Chrom, Kobalt, und viele andere, sowie auch intermetallische Verbindungen, aus nichtwässrigen Lösungen ihrer Verbindungen in einer gewünschten Form abzuscheiden, indem man als Reduktionsmittel in nichtwässrigen Lösungsmitteln lösliche Anionenradikale von Kohlenwasserstoffverbindungen, 25 im besonderen von aromatischen, bzw. mehrkernigen aromatischen Verbindungen wie Naphtalin, Biphenyl oder Phenanthren, verwendet. Um eine solche Lösung von Anionenradi-kalen zu erhalten, wird einer nichtwässrigen Lösung des entsprechenden Kohlenwasserstoffes Natrium, oder ein anderes 30 Reduktionsmittel hinzugefügt, öderes wird die nichtwässrige Lösung des Kohlenwasserstoffes, dem noch ein Leitsalz, wie z.B. ein Tetraalkylammoniumhalogenid beigegeben wurde, elektrolysiert. The present invention overcomes all of the disadvantages described. It has been found that semiconductors such as silicon, or metals such as molybdenum, tantalum, 20 chromium, cobalt, and many others, as well as intermetallic compounds, can be separated from non-aqueous solutions of their compounds in a desired form by using as reducing agents in non-aqueous ones Solvent-soluble anion radicals from hydrocarbon compounds, in particular from aromatic or polynuclear aromatic compounds such as naphthalene, biphenyl or phenanthrene, are used. In order to obtain such a solution of anion radicals, sodium or another reducing agent is added to a non-aqueous solution of the corresponding hydrocarbon, or the non-aqueous solution of the hydrocarbon to which a conducting salt, e.g. a tetraalkylammonium halide was added, electrolyzed.
Das erfindungsgemässe Verfahren zur stromlosen Ab-35 Scheidung von Metallen oder Halbleitern in Pulverform oder in Form von auf Substraten festhaftenden Schichten ist dadurch gekennzeichnet, dass die in einem nichtwässrigen Lösungsmittel gelösten Verbindungen der abzuscheidenden Stoffe mit Hilfe eines ebenfalls im selben Lösungsmittel gelö-40 sten Anionenradikals eines Kohlenwasserstoffes reduziert werden. The method according to the invention for the electroless deposition of metals or semiconductors in powder form or in the form of layers adhering to substrates is characterized in that the compounds of the substances to be deposited dissolved in a non-aqueous solvent with the aid of an anion radical likewise dissolved in the same solvent of a hydrocarbon can be reduced.
Das Substrat kann dabei eine beliebige Substanz, wie z.B. ein Metall, Glas, Porzellan, Saphir, Plastik, Teflon, Kunstharz, usw. sein. The substrate can be any substance, e.g. a metal, glass, porcelain, sapphire, plastic, teflon, synthetic resin, etc.
45 Eine andere erfindungsgemässe Form des Verfahrens besteht darin, dass man wie oben die Lösungen der Metallverbindung und des Anionenradikals vereinigt, ohne dass Substrate in die Lösung tauchen, wobei das Metall direkt in Pulverform aus der Lösung abgeschieden wird. 45 Another form of the method according to the invention is that the solutions of the metal compound and the anion radical are combined as described above without substrates being immersed in the solution, the metal being deposited directly from the solution in powder form.
so Folgende Beispiele beschreiben mögliche Ausführungsformen des erfindungsgemässen Verfahrens. The following examples describe possible embodiments of the method according to the invention.
Beispiele Examples
Beispiel 1 example 1
55 In einem mit trockenem Argon gespülten, geschlossenen Reaktionsgefäss befindet sich eine 0,5 molare Lösung von SiHCl3 in Propylenkarbonat, in die die zu beschichtenden Kupfersubstrate eingetaucht sind. Dieser Lösung wird eine 0,05 molare Lösung von Naphtalin in Propylenkarbonat, die 60 als Bodensatz Natrium enthielt, zugesetzt. Auf den Substraten scheidet sich darauf eine Siliziumschicht von ungefähr 5 (im Dicke ab. 55 A 0.5 molar solution of SiHCl3 in propylene carbonate, in which the copper substrates to be coated are immersed, is located in a closed reaction vessel flushed with dry argon. A 0.05 molar solution of naphthalene in propylene carbonate, which contained 60 as the sediment sodium, is added to this solution. A silicon layer of approximately 5 (in thickness) is deposited on the substrates.
Beispiel 2 Example 2
65 In einem mit trockenem Stickstoff gespülten Reaktionsgefäss befindet sich eine 0,1 molare Lösung von Biphenyl in Di-methylformamid, die während einer Stunde mit einer Dispersion aus Natrium in Kontakt war und darauf filtriert wurde. 65 In a reaction vessel flushed with dry nitrogen there is a 0.1 molar solution of biphenyl in dimethylformamide, which was in contact with a dispersion of sodium for one hour and was then filtered.
3 3rd
656 401 656 401
In diese Lösung tauchen Substrate aus Stahl. Dieser Lösung wird eine 0,1 molare Lösung von MoC15 in Dimethylform-amid zugegeben. Auf dem Stahlsubstrat scheidet sich darauf eine festhaftende Schicht aus Molybdän ab. Steel substrates are immersed in this solution. A 0.1 molar solution of MoC15 in dimethylformamide is added to this solution. A firmly adhering layer of molybdenum is deposited on the steel substrate.
Beispiel 3 Example 3
In einem wie oben beschriebenen Reaktionsgefäss befindet sich eine Lösung von CoJ2 (0,05 molar) und Naphtalin (0,1 molar) in Acetonitril, in die Substrate aus Cu, Ni, Aluminium oder Aluminiumlegierungen, oder ähnlichen Werkstoffen, eintauchen. Nachdem dieser Lösung Lithium oder ein anderes reduzierendes Metall zugegeben und die Lösung gerührt wurde, scheidet sich auf den Substraten eine Schicht aus Kobalt ab. Diese Form des Verfahrens ist nicht immer vorteilhaft, da sich das abzuscheidende Metall auch auf dem reduzierenden Metall direkt niederschlagen kann. In a reaction vessel as described above there is a solution of CoJ2 (0.05 molar) and naphthalene (0.1 molar) in acetonitrile, into which substrates made of Cu, Ni, aluminum or aluminum alloys or similar materials are immersed. After lithium or another reducing metal has been added to this solution and the solution has been stirred, a layer of cobalt is deposited on the substrates. This form of the method is not always advantageous since the metal to be deposited can also be deposited directly on the reducing metal.
Beispiel 4 Example 4
Man verfährt wie in den Beispielen 1 bis 3, ausser dass sich anstelle der in diesen Beispielen erwähnten Metallsalze MoC15 und SiCl4 in je 0, l molarer Lösung befinden. Auf den Substraten scheidet sich darauf eine Schicht aus MoSi2 ab. The procedure is as in Examples 1 to 3, except that instead of the metal salts MoC15 and SiCl4 mentioned in these examples are in 0.1 molar solution. A layer of MoSi2 is deposited on the substrates.
Beispiel 5 Example 5
Das Reaktionsgefäss besteht aus einem rechteckiggeformten, flachen Kanal, an dessen beiden gegenüberliegenden Wandungen die einseitig zu beschichtenden Substrate angeordnet sind. Durch diesen Kanal strömt eine Lösung von SÌHCI3 (0,1 molar) und Naphtalin (0,1 molar), wobei letztere, bevor sie in das Reaktionsgefäss eingespeist wird, über Natrium gehalten wird. Die Strömungsgeschwindigkeit wird so eingestellt, dass der Verbrauch von SiHCl3 und Naphtalin-anionenradikals nicht mehr als 20-30% der Konzentration am Eingang der Zelle beträgt. Man erhält so Schichten gleich-mässiger Qualität aus Silizium auf den Substraten. The reaction vessel consists of a rectangular, flat channel, on the two opposite walls of which the substrates to be coated on one side are arranged. A solution of SÌHCI3 (0.1 molar) and naphthalene (0.1 molar) flows through this channel, the latter being held over sodium before it is fed into the reaction vessel. The flow rate is adjusted so that the consumption of SiHCl3 and naphthalene anion radicals is not more than 20-30% of the concentration at the entrance to the cell. This gives layers of uniform quality made of silicon on the substrates.
5 5
Beispiel 6 Example 6
Man verfahrt wie in den Beispielen 1 bis 5, ausser dass das Substrat aus Glas, Keramik wie A1203 oder einem Kunststoff wie Polypropylen besteht. The procedure is as in Examples 1 to 5, except that the substrate consists of glass, ceramic such as A1203 or a plastic such as polypropylene.
10 10th
Beispiel 7 Example 7
Man verfährt wie in den Beispielen 1 bis 6, ausser dass der Lösung, die den Kohlenwasserstoff enthält, Tetrabutylam-moniumiodid (Konzentration 0,1 molar) zugesetzt wird und 15 dass die Lösung, bevor sie mit der Lösung des Metallsalzes vereinigt wird, zwischen zwei Platinelektroden elektrolysiert wird, wobei durch geeignete bekannte Mittel (Diaphragmen) verhindert wird, dass das an der Anode entstehende Jod in die reduzierende Lösung gelangt. The procedure is as in Examples 1 to 6, except that tetrabutylam monium iodide (concentration 0.1 molar) is added to the solution containing the hydrocarbon and 15 that the solution, before it is combined with the solution of the metal salt, between two Platinum electrodes is electrolyzed, with suitable known means (diaphragms) preventing the iodine formed at the anode from reaching the reducing solution.
20 Es versteht sich, dass diese angeführten Beispiele nicht erschöpfend sind. Es ist sogar ein Vorteil der vorliegenden Erfindung, dass die verschiedenen Parameter des Verfahrens dem jeweiligen gewünschten Zweck angepasst werden können. Das betrifft im besonderen die Natur und die Konzentra-25 tion der Kohlenwasserstoffe, die die reduzierenden Anionen-radikale bilden, die Natur der Lösungsmittel, die Natur und Konzentration der Metallverbindungen, sowie ihrer Mischungen, um gleichzeitig verschiedene Metalle abzuscheiden oder deren Legierungen oder intermetallische Phasen zu 30 bilden. 20 It is understood that these examples are not exhaustive. It is even an advantage of the present invention that the various parameters of the method can be adapted to the desired purpose. This applies in particular to the nature and concentration of the hydrocarbons that form the reducing anion radicals, the nature of the solvents, the nature and concentration of the metal compounds and their mixtures, in order to simultaneously deposit different metals or their alloys or intermetallic phases to form 30.
C C.
Claims (6)
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH3992/83A CH656401A5 (en) | 1983-07-21 | 1983-07-21 | METHOD FOR ELECTRICALLY DEPOSITING METALS. |
| AT841796A ATA179684A (en) | 1983-07-21 | 1984-05-30 | METHOD FOR ELECTRICALLY DEPOSITING METALS |
| DE19843422731 DE3422731A1 (en) | 1983-07-21 | 1984-06-19 | METHOD FOR ELECTRICALLY DEPOSITING METALS |
| IT48429/84A IT1177814B (en) | 1983-07-21 | 1984-06-20 | METHOD OR SEMI-CONDUCTOR DEPOSITION WITHOUT CURRENT |
| JP59134039A JPS6026668A (en) | 1983-07-21 | 1984-06-28 | Process for non-electrolytically depositing metal or semiconductor |
| FR8411047A FR2549497A1 (en) | 1983-07-21 | 1984-07-11 | PROCESS FOR DEPOSITING METALS OR SEMICONDUCTORS WITHOUT CURRENT |
| GB08418549A GB2143853A (en) | 1983-07-21 | 1984-07-20 | Deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH3992/83A CH656401A5 (en) | 1983-07-21 | 1983-07-21 | METHOD FOR ELECTRICALLY DEPOSITING METALS. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH656401A5 true CH656401A5 (en) | 1986-06-30 |
Family
ID=4267786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH3992/83A CH656401A5 (en) | 1983-07-21 | 1983-07-21 | METHOD FOR ELECTRICALLY DEPOSITING METALS. |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS6026668A (en) |
| AT (1) | ATA179684A (en) |
| CH (1) | CH656401A5 (en) |
| DE (1) | DE3422731A1 (en) |
| FR (1) | FR2549497A1 (en) |
| GB (1) | GB2143853A (en) |
| IT (1) | IT1177814B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242713A (en) * | 1988-12-23 | 1993-09-07 | International Business Machines Corporation | Method for conditioning an organic polymeric material |
| US5318803A (en) * | 1990-11-13 | 1994-06-07 | International Business Machines Corporation | Conditioning of a substrate for electroless plating thereon |
| JP4636236B2 (en) * | 2003-10-16 | 2011-02-23 | Ｊｓｒ株式会社 | Composition for forming silicon / cobalt film and method for forming silicon / cobalt film |
| US7718228B2 (en) * | 2003-10-16 | 2010-05-18 | Jsr Corporation | Composition for forming silicon-cobalt film, silicon-cobalt film and method for forming same |
| AT500782B8 (en) * | 2004-11-19 | 2007-02-15 | Plansee Se | METHOD FOR SEPARATING LAYERS FROM IONIC LIQUIDS |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3635761A (en) * | 1970-05-05 | 1972-01-18 | Mobil Oil Corp | Electroless deposition of metals |
| FR2264892B2 (en) * | 1972-04-24 | 1976-12-17 | Rhone Poulenc Textile | |
| FR2196394A1 (en) * | 1972-08-19 | 1974-03-15 | Metallgesellschaft Ag | Plating inner walls of chemical appts - by chemical reduction or organo-metal cpds dissolved in hydrocarbons |
| AT322940B (en) * | 1972-10-31 | 1975-06-10 | Siemens Ag | BATHROOMS FOR ELECTRICALLY NICKEL-PLATING METAL, PLASTIC AND CERAMICS |
| FR2239539B1 (en) * | 1973-08-01 | 1976-04-30 | Rhone Poulenc Textile | |
| US3993491A (en) * | 1973-12-07 | 1976-11-23 | Surface Technology, Inc. | Electroless plating |
| DE2409251C3 (en) * | 1974-02-22 | 1979-03-15 | Kollmorgen Corp., Hartford, Conn. (V.St.A.) | Process for the catalytic seeding of non-metallic surfaces for a subsequent, electroless metallization and bath solutions for carrying out the process |
| US3993799A (en) * | 1974-10-04 | 1976-11-23 | Surface Technology, Inc. | Electroless plating process employing non-noble metal hydrous oxide catalyst |
| GB1468973A (en) * | 1975-07-18 | 1977-03-30 | Atomic Energy Authority Uk | Microcircuit packages |
| GB1473223A (en) * | 1975-09-04 | 1977-05-11 | Welwyn Electric Ltd | Circuit board blanks |
| US4265943A (en) * | 1978-11-27 | 1981-05-05 | Macdermid Incorporated | Method and composition for continuous electroless copper deposition using a hypophosphite reducing agent in the presence of cobalt or nickel ions |
| US4337091A (en) * | 1981-03-23 | 1982-06-29 | Hooker Chemicals & Plastics Corp. | Electroless gold plating |
-
1983
- 1983-07-21 CH CH3992/83A patent/CH656401A5/en not_active IP Right Cessation
-
1984
- 1984-05-30 AT AT841796A patent/ATA179684A/en not_active IP Right Cessation
- 1984-06-19 DE DE19843422731 patent/DE3422731A1/en not_active Withdrawn
- 1984-06-20 IT IT48429/84A patent/IT1177814B/en active
- 1984-06-28 JP JP59134039A patent/JPS6026668A/en active Pending
- 1984-07-11 FR FR8411047A patent/FR2549497A1/en active Pending
- 1984-07-20 GB GB08418549A patent/GB2143853A/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| GB8418549D0 (en) | 1984-08-22 |
| DE3422731A1 (en) | 1985-01-31 |
| IT1177814B (en) | 1987-08-26 |
| GB2143853A (en) | 1985-02-20 |
| FR2549497A1 (en) | 1985-01-25 |
| JPS6026668A (en) | 1985-02-09 |
| IT8448429A0 (en) | 1984-06-20 |
| ATA179684A (en) | 1986-12-15 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PLI | Licence |
Free format text: PROF. DR. OSKAR FRIEDRICH OLAJ |
|
| PL | Patent ceased |