WO2006061081A2 - Electrochemical deposition of tantalum and/or copper in ionic liquids - Google Patents
Electrochemical deposition of tantalum and/or copper in ionic liquids Download PDFInfo
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- WO2006061081A2 WO2006061081A2 PCT/EP2005/012180 EP2005012180W WO2006061081A2 WO 2006061081 A2 WO2006061081 A2 WO 2006061081A2 EP 2005012180 W EP2005012180 W EP 2005012180W WO 2006061081 A2 WO2006061081 A2 WO 2006061081A2
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- Prior art keywords
- pyrrolidinium
- tantalum
- imidazolium
- methyl
- hydroxyethyl
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/615—Microstructure of the layers, e.g. mixed structure
- C25D5/617—Crystalline layers
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
Definitions
- the invention relates to a method for the electrochemical deposition of tantalum and / or copper on a substrate in an ionic
- Tantalum is a platinum-gray, hard, very tough, elastic, malleable polishable metal that you can roll and forge. It covers the air with a protective oxide layer or is spontaneously oxidized by water. Thin layers of tantalum can be used in a variety of applications, such as barrier, protective or sealing layers, which can also be an intermediate layer, for container liners, (micro) electronic components or devices such as tantalum electrolytic capacitors the production of glow wires or gold bond wires, magnetic recording media or thermal printheads for inkjet printers. In surgery, tantalum is used as a material for bone nails, bone substitutes, joint implants, staples, pine screws, and other instruments because this high atomic number metal is well biocompatible and has good blood compatibility similar to titanium.
- Implants are often made of implant materials, which are then coated with a thin layer of tantalum (Dresdner Transferbrief, issue 04/2001, Volume 9, ed. TU Dresden, BTI - consulting firm for technology transfer and innovation promotion mbH, TECHZentrumDresden: Lone treatment of vascular stents increase blood compatibility and X-ray contrast or ⁇ cht-Zeitung from 17.04.2002, One prosthesis type for all - that's yesterday's snow).
- Copper is a corrosion-resistant precious metal, which has excellent electrical conductivity and thermal conductivity, and exhibits very low electromigration behavior.
- thin layers of copper have been used instead of the previously used aluminum as contact material for the semiconductor structures.
- the person skilled in some physical and chemical vapor deposition methods are known, for example, the sputtering method or Vakuumbedampfungsmethode.
- the electrochemical deposition of copper from an aqueous medium is also known (A. Thies, Galvanotechnik, 11 (2002) 2837-2843).
- a silicon chip is covered by vapor deposition with a thin 20-70 nm thick tantalum layer and then the copper contact is applied in the aqueous medium , the problem arises that tantalum is spontaneously oxidized by water before the copper deposition occurs. This results in not inconsiderable contact resistance between copper and the surface oxidized tantalum.
- tantalum Because of its reactive nature, unlike copper, tantalum can not be deposited in aqueous media. Organic solvents are excluded due to the risk of explosion and the problem of producing them anhydrous.
- Electrochemical methods are known for the deposition of tantalum in high-temperature molten salts such as LiF / NaF / CaF 2 melts, at 500 0 C. (Mehmood et al., Materials Transactions, 44 (2003), 1659-1662) or from the mixture of K 2 TaF 7 in, for example, the eutectic mixture LiF / NaF / KF (50/30/20) at temperatures of 600-900 0 C on iron (JP H06-57479).
- the extremely high temperatures and the corrosive behavior of the high-temperature molten salts cause these
- Method is unsuitable for some applications, for example for the application in the chip technology, or is not economical due to the safety aspect in the implementation of the deposition and the high cost.
- JP 2001279486 now describes an electrochemical process for the deposition of tantalum wherein the deposition takes place in a molten salt consisting of tantalum pentachloride, alkylimidazolium chloride and fluorides of an alkali metal or alkaline earth metal.
- a molten salt consisting of tantalum pentachloride, alkylimidazolium chloride and fluorides of an alkali metal or alkaline earth metal.
- TaCI 5 LiF and 1-ethyl-3-methyl-imidazolium chloride in a ratio of 30 mol: 10 mol deposited at temperatures around 100 0 C: 60mol.
- the object of the invention was to find an alternative method for the electrochemical deposition of tantalum and / or copper under anhydrous conditions.
- the object is achieved by the method according to the invention.
- the invention relates to a process for the electrochemical deposition of tantalum and / or copper on a substrate in an ionic liquid containing at least one tetraalkylammonium, tetraalkylphosphonium, 1, 1-dialkylpyrrolidinium, 1-hydroxyalkyl-1-alkyl-pyrrolidinium-, 1 -Hydroxyalkyl-3-alkylimidazolium or 1,3-bis (hydroxyalkyl) imidazolium cation, wherein the alkyl groups or the Alkyl chain of the hydroxyalkyl group may each independently have 1 to 10 carbon atoms.
- tantalum or copper takes place independently of each other on a wide variety of substrates in different ways
- tantalum and copper may also take place sequentially as desired in the particular application of chip technology, i.
- tantalum is deposited on silicon, for example a silicon wafer, electrochemically with the method according to the invention and then in the same medium, the deposition of copper on the tantalum-coated silicon.
- the ionic liquids which are suitable for the process according to the invention and comprise at least one tetraalkylammonium, tetraalkylphosphonium, 1,1-dialkylpyrrolidinium, 1-hydroxyalkyl-1-alkylpyrrolidinium, 1-hydroxyalkyl-3-alkylimidazolium or 1, 3
- Bis (hydroxyalkyl) imidazolium cation wherein the alkyl groups or the alkylene chain of the hydroxyalkyl group may each independently have 1 to 10 carbon atoms, are highly conductive and generally up to 400 0 C thermally stable. They have, for example, a wide electrochemical window in the cathodic branch, which ranges from -2000 mV to -3500 mV against ferrocene / ferrocinium, preferably from -2700 mV to -3000 mV against ferrocene / ferrocinium.
- alkyl group having 1 to 10 carbon atoms is meant, for example, methyl, ethyl, isopropyl, propyl, butyl, sec-butyl or tert-butyl, and also pentyl, 1-, 2- or 3-methylbutyl, 1, 1 -, 1, 2- or 2,2-dimethylpropyl, 1-ethylpropyl, hexyl, heptyl, octyl, nonyl or decyl.
- the alkyl groups may also be partially or completely substituted by fluorine.
- Fluorinated alkyl groups are, for example, difluoromethyl, trifluoromethyl, pentafluoroethyl, pentafluoropropyl, heptafluoropropyl, heptafluorobutyl or nonafluorobutyl.
- a hydroxyalkyl group having 1 to 10 carbon atoms is understood as meaning, for example, 1-hydroxymethyl, 2-hydroxyethyl, 3-hydroxypropyl, 4-hydroxybutyl, and also 5-hydroxypentyl, 6-hydroxyhexyl, 7-hydroxyheptyl, 8-hydroxyoctyl, 9-hydroxynonyl or 10-hydroxydecyl.
- the alkylene chain of the hydroxy group can also be partially or completely substituted by fluorine.
- Fluorinated hydroxyalkyl groups can be described, for example, by the subformula - (CHF) n -OH or - (CF 2 ) n -OH, where n can denote 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10.
- Suitable anions which, in combination with the cations according to the invention, satisfy the abovementioned condition can be selected from the group perfluoroalkylsulfonate, perfluoroacetate, bis (fluorosulfonyl) imide, bis (perfluoroalkylsulfonyl) imide, tris (perfluoroalkyl) trifluorophosphate, bis (perfluoroalkyl) tetrafluorophosphate, Tris (Perfluoroalkylsulfonyl) methide or perfluoroalkyl borate.
- perfluoroalkyl group means that all H atoms of the corresponding alkyl group are replaced by F atoms.
- the perfluoroalkyl groups in the indicated anions in each case independently of one another have 1 to 10 C atoms, more preferably 1, 2, 3 or 4 C atoms.
- Anions which are suitable according to the invention can be selected, for example, from the group trifluoromethylsulfonate, pentafluoroethylsulfonate,
- perfluoroalkyl groups may independently of one another denote different perfluoroalkyl groups.
- mixed anions such as trifluoromethylsulfonylpentafluoroethylsulfonylimide, bis (trifluoromethyl) sulfonylpentafluoroethylsulfonylmethide also fall under the above definition.
- Suitable cations are, optionally linear or branched, tetramethylammonium, tetraethylammonium, tetrapropylammonium,
- Particularly suitable cations are tetramethylammonium, trimethylalkylammonium, where the alkyl group has 1 to 10 carbon atoms Trihexyltetradecylphosphonium, triisobutyl (methyl) phosphonium, tributyl (ethyl) phosphonium, tributyl (methyl) phosphonium, 1-butyl-1-methylpyrrolidinone, 1-butyl-1-ethylpyrrolidinium, 1-hexyl-1-methylpyrrolidinium, 1-methyl-1-octylpyrrolidinium or 1- (2-hydroxyethyl) -3-methylimidazolium, very particularly suitable cations are 1-butyl-1-methylpyrrolidinium, 1-hexyl-1-methylpyrrolidiniunn, 1-methyl-1-octylpyrrolidinium or 1- (2-hydroxyethyl) -3-methylimidazolium.
- Tris (pentafluoroethyl) trifluorophosphate Tris (pentafluoroethyl) trifluorophosphate.
- tantalum or copper ions are dissolved in a suitable ionic liquid as described above. This can be done on the one hand by anodic dissolution of the metal or a suitable metal salt, for example TaH 4 or TaH 5 , in the ionic liquid, on the other hand by dissolving a tantalum or copper salt in the ionic liquid.
- a suitable ionic liquid as described above. This can be done on the one hand by anodic dissolution of the metal or a suitable metal salt, for example TaH 4 or TaH 5 , in the ionic liquid, on the other hand by dissolving a tantalum or copper salt in the ionic liquid.
- suitable copper or tantalum salts are copper (II), copper (I), tantalum (IV) or tantalum (V) halides, for example chlorides, bromides, iodides or fluorides, imides, for example copper (II), Copper (I), tantalum (IV) or tantalum (V) bis (perfluoroalkylsulfonyl) imides, amides, for example Ta (NR 2 ) 4 or Ta (NR 2 ) S , where R is an alkyl group having 1 to
- alkoxides such as copper (II) -, copper (L) -, tantalum (IV) - or tantalum (V) -methoxide, buyer (II) -, copper (L) -, tantalum (IV ) - or tantalum (V) ethoxide or buyer (II), copper (I), tantalum (IV) or tantalum (V) tartrate.
- tantalum salt is also suitable as the tantalum salt.
- TaX y bis (trifluoromethylsulfonyl) imide
- X F, Cl, Br or I
- y 1, 2, 3 or 4
- z 1, 2, 3 or 4
- the sum y + z 4 or 5 means.
- the salts are used anhydrous.
- the salts may also contain crown ethers.
- the ionic liquid containing the copper salt may also be dried.
- Particularly suitable copper or tantalum salts are salts whose anions are identical or chemically very similar to the anion of the ionic liquid.
- the first tantalum deposition is carried out according to the invention by dissolving a tantalum salt in the ionic liquid and carrying out the second copper deposition according to the invention by passing the copper ions into the ionic liquid by anodic oxidation to guarantee freedom from water.
- the presence of an alkali or alkaline earth metal fluoride in the electrochemical deposition of tantalum according to the present invention has been found to be advantageous.
- the fluoride should preferably be in a ratio of 2: 1 (fluoride / tantalum salt) to 1: 1 (fluoride / tantalum salt) are added, preferably in the ratio 1: 1.
- Preferred alkali metal or alkaline earth metal fluorides are, for example, lithium fluoride, sodium fluoride, potassium fluoride, magnesium fluoride or calcium fluoride. Particular preference is given to adding lithium fluoride.
- tantalum salts are tantalum tetrafluoride, tantalum pentafluoride, tantalum tetrachloride, tantalum tetrabromide, tantalum tetraiodide, tantalum pentabromide or tantalum pentaiodide. Very particular preference is given to tantalum pentafluoride.
- the ion concentration in the ionic liquid to the metal deposition is preferably 10 -5 to 10 mol / l. Preference is given to working with an ion concentration of 10 -3 to 10 -1 mol / l.
- an ion concentration of in each case 0.25 mol / l to 1 mol / l has proven to be the preferred range.
- the metal deposition according to the invention takes place in one
- Inert gas atmosphere for example, under argon, wherein the oxygen and water content should be less than 1 ppm.
- the deposition is carried out in a 3-electrode cell as known to those skilled in the art (for example, AJ Bard, LR Faulkner, Electrochemical Methods, Wiley). Copper deposition on a suitable substrate uses copper wires as counter and reference electrodes. In tantalum deposition, platinum wires are used as a quasi-reference and counter electrode. In general, however, any electrode material is suitable if it is ensured by the construction of the experiment that the products formed at the counter electrode do not disturb the processes at the working electrode.
- the inventive method is preferably carried out potentiostatically, at electrode potentials between 0 and -2000 mV vs.. Tantalum deposition and at temperatures between 10 0 C and 35O 0 C, preferably between 100 0 C to 300 ° C.
- the method according to the invention can also be carried out by means of pulsed techniques, as known to the person skilled in the art, for example as described in J.-C. Puippe, F. Leaman, Pulse-Plating: Electrolytic Metal Deposition with Pulsed Current, Eugen G. Leuze Verlag, 1990.
- the metals tantalum or copper can be deposited in layer thicknesses between 200 .mu.m and 200 .mu.m, namely in microcrystalline or nano-crystalline covering layers.
- the desired layer thickness is controlled via the electrode potential and the flowed charge as well as the electrochemical parameters.
- F Faraday constant
- A area
- p density of the metal
- I current
- t time
- M molar mass of the metal
- Figure 1 shows a cyclic voltammogram of an approximately 1 molar solution of TaF 5 in 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide (BMP Tf 2 N) at room temperature on Au (111).
- BMP Tf 2 N 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide
- tantalum pentafluoride is apparently reduced in several reduction steps during the process of the invention.
- LiF is added to TaFs / i-butyl-i-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide, a new reduction peak is formed, see Figure 2, to give tantalum, as shown in Figure 3.
- Figure 2 shows a cyclic voltammogram of a 0.25 molar solution of TAFs and 0.25 molar solution of LiF in 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide at 200 0 C on Au (111).
- XRD X-ray diffraction, Tantalum cobalt K alpha
- Figure 4 shows a cyclic voltammogram of 1-butyl-1-methylpyrrolidinium trifluoromethanesulfonate in which copper was previously anodically dissolved on Au (111).
- concentration of the copper ions in the ionic liquid is 10 -1 mol / l.
- Figure 4 in which two successive scans are shown, shows two or three reduction processes on Au (111), whereby the process can be assigned to copper deposition at -1000 mV and -1700 mV. Copper is deposited in the process according to the invention in very high quality and is particularly nanoscale.
- Suitable substrates are for example selectable from all categories, for example non-metals, semi-metals, metals, metal alloys, conductive or metallized ceramics or conductive or metallized
- a preferred nonmetal is, for example, graphite.
- a preferred semi-metal is, for example, silicon.
- Preferred metals are, for example, gold, platinum, copper, iron, cobalt, nickel or molybdenum.
- Preferred metal alloys are, for example, the most diverse
- suitable substrates may already already consist of several layers to which a further layer as an intermediate layer or final layer of tantalum or copper is applied by the process according to the invention.
- a further layer as an intermediate layer or final layer of tantalum or copper is applied by the process according to the invention.
- the ionic liquid can be washed out with organic solvents or, in the case of copper, with water.
- Suitable organic solvents are, for example, toluene, benzene, methylene chloride, acetonitrile, acetone, methanol, ethanol or isopropanol.
- the invention also relates to a particular embodiment of the process, wherein tantalum in an ionic liquid containing at least one tetraalkylammonium, tetraalkylphosphonium, 1,1-dialkylpyrrolidinium, 1-hydroxyalkyl-1-alkyl-pyrrolidinium, 1-hydroxyalkyl-3-alkyl-imidazolium or 1, 3-bis (hydroxyalkyl) imidazolium cation, wherein the alkyl groups or the alkylene chain of the hydroxyalkyl group can each independently have 1 to 10 carbon atoms, is deposited, under electrochemical potential control the tantalum ion-containing ionic liquid is replaced by pure ionic liquid, then under potential control the ionic copper ion-containing
- Example 1 Deposition of Tantalum from TaF 5
- a saturated solution of TaF 5 and LiF in the ionic liquid 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide is prepared and transferred under protective gas atmosphere at room temperature into the 3-electrode measuring cell.
- a typical 3-electrode measuring cell was used, as described, for example, in AJ. Bard and LR Faulkner, Electrochemical Methods, Wiley.
- the 3-electrode measuring cell has a gold electrode as working electrode (cathode) and platinum wires serve as quasi-reference and counter electrode.
- the electrode potential is at -1300 mV vs. Platinum quasi-reference set.
- tantalum begins at -1250 mV.
- An in situ STM image at -1200 mV on Au (111) clearly shows ( Figure 5) that small crystallites with a height of a few nanometers are deposited. These form a layer about 100 nm thick.
- the metallic character can be detected by current / voltage tunneling spectra ( Figure 6).
- Example 2 Deposition of tantalum from TaF 5 on platinum
- Example 2 Analogously to Example 1, a 0.25 molar solution of TaF 5 and LiF in the ionic liquid 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide prepared and transferred under protective gas atmosphere at room temperature in the 3-Elektrodenmeßzelle.
- a typical 3-electrode measuring cell was used, as described, for example, in AJ. Bard and LR Faulkner, Electrochemical Methods, Wiley.
- the 3-electrode measuring cell has as a working electrode (cathode) a platinum electrode and platinum wires serve as a quasi-reference and counter electrode.
- the electrode potential is at -1300 mV vs. Platinum quasi-reference set.
- the 3-Elektrodenmeßzelle here consists of Cu as a working electrode, for
- the electrode potential of the copper working electrode is set to +500 mV versus Cu / Cu +.
- the dissolved amount of copper ions is over the
- the platinum counter electrode is spatially separated to avoid redeposition of copper there.
- the SEM image ( Figure 7) shows that copper is deposited nanoscale. In this case, a layer thickness of 10 ⁇ m was produced. In principle, the layer thickness is not limited, i. it can be produced in the desired thickness, depending on the application.
- the 3-electrode measuring cell has a working electrode (cathode)
- Gold electrode and copper wires serve as reference and counter electrode.
- the electrode potential is at -500 mV vs. Cu / Cu + set.
- Example 3 copper was deposited nanoscale ( ⁇ 59 nm) in this ionic liquid, it being possible to adjust the layer thickness variably. Typically, a layer thickness of 10 microns was deposited.
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EP05813986A EP1831433A2 (en) | 2004-12-10 | 2005-11-15 | Electrochemical deposition of tantalum and/or copper in ionic liquids |
CA002590080A CA2590080A1 (en) | 2004-12-10 | 2005-11-15 | Electrochemical deposition of tantalum and/or copper in ionic liquids |
JP2007544757A JP2008523242A (en) | 2004-12-10 | 2005-11-15 | Electrochemical deposition of tantalum and / or copper in ionic liquids |
US11/721,277 US20090242414A1 (en) | 2004-12-10 | 2005-11-15 | Electronchemical deposition of tantalum and/or copper in ionic liquids |
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DE102004059520.8 | 2004-12-10 | ||
DE102004059520A DE102004059520A1 (en) | 2004-12-10 | 2004-12-10 | Electrochemical deposition of tantalum and / or copper in ionic liquids |
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CN (1) | CN101076617A (en) |
CA (1) | CA2590080A1 (en) |
DE (1) | DE102004059520A1 (en) |
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- 2005-11-15 WO PCT/EP2005/012180 patent/WO2006061081A2/en active Application Filing
- 2005-11-15 EP EP05813986A patent/EP1831433A2/en not_active Withdrawn
- 2005-11-15 JP JP2007544757A patent/JP2008523242A/en active Pending
- 2005-11-15 US US11/721,277 patent/US20090242414A1/en not_active Abandoned
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JP2010525161A (en) * | 2007-04-17 | 2010-07-22 | ネーデルランドセ オルガニサティエ フォール トエゲパストナトールヴェテンシャッペリク オンデルゾエク ティエヌオー | Barrier layer and manufacturing method thereof |
WO2009019147A2 (en) * | 2007-08-06 | 2009-02-12 | Katholieke Universiteit Leuven | Deposition from ionic liquids |
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Also Published As
Publication number | Publication date |
---|---|
EP1831433A2 (en) | 2007-09-12 |
RU2007125776A (en) | 2009-01-20 |
US20090242414A1 (en) | 2009-10-01 |
DE102004059520A1 (en) | 2006-06-14 |
WO2006061081A3 (en) | 2007-08-02 |
KR20070085936A (en) | 2007-08-27 |
CN101076617A (en) | 2007-11-21 |
CA2590080A1 (en) | 2006-06-15 |
JP2008523242A (en) | 2008-07-03 |
TW200626755A (en) | 2006-08-01 |
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