WO2016110409A1 - Procédé de production de nanofils de zinc - Google Patents

Procédé de production de nanofils de zinc Download PDF

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Publication number
WO2016110409A1
WO2016110409A1 PCT/EP2015/080914 EP2015080914W WO2016110409A1 WO 2016110409 A1 WO2016110409 A1 WO 2016110409A1 EP 2015080914 W EP2015080914 W EP 2015080914W WO 2016110409 A1 WO2016110409 A1 WO 2016110409A1
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WIPO (PCT)
Prior art keywords
zinc
range
solution
nanowires
concentration
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PCT/EP2015/080914
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English (en)
Inventor
Heino Sommer
Rihab AL-SALMAN
Torsten Brezesinski
Original Assignee
Basf Se
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Filing date
Publication date
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Publication of WO2016110409A1 publication Critical patent/WO2016110409A1/fr

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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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/006—Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • 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
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc
    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc

Definitions

  • Zn nanostructures are mainly synthesized by high temperature techniques such as thermal evaporation of zinc metal at temperatures of 550 °C - 900 °C [D. Yuvaraj, K.N. Rao, K. Barai, Solid State Commun., 149 (2009) 349; Y. Tong, M. Shao, G. Qian, Y. Ni, Nanotechnology 16 (2005) 2512], thermal decomposition of ZnS powders at 1000 °C [Y. Wang, L. Zhang, G. Meng, C. Liang, G. Wang, S. Sun, Chem. Commun., (2001 ) 2632] and chemical reduction of ZnO by e.g. boron at 1050 °C [Y.J. Chen, B.
  • the obtained nanowires can have a diameter of 10 to 100 nm and a length of few hundred micrometers.
  • the method is limited to HOPG substrate and includes multi steps.
  • it needs an accurate control of the deposition conditions to have the suitable density of nuclei and suitable size of the particles.
  • the nanowires can be hardly harvested from the HOPG substrate without destroying them.
  • a process for producing zinc nanowires comprising at least the process step of (a) electrochemically depositing zinc directly onto at least one surface of an electrode from a solution comprising (A) at least one zinc compound,
  • the zinc nanowires obtainable or obtained by the inventive process are preferably crystalline.
  • the thickness of zinc nanowires obtainable or obtained by the inventive process is usually in the range from 1 nm to 100 nm, preferably in the range from 5 nm to 50 nm, in particular in the range from 10 nm to 30 nm.
  • the zinc nanowires obtainable or obtained by the inventive process can be covered by a surface layer comprising the elements silicon, oxygen and carbon.
  • the thickness of the surface layer can vary in a wide range. Preferably the thickness of the surface layer is in range of a 1/50 to 1/3, more preferably 1/20 to 1/5 of the total thickness of the nan- owire.
  • the zinc nanowires, disregarding an existing surface layer consist essentially of zinc, that means that the zinc-content of the zinc nanowires is preferably at least 80 %, more preferably in the range of from 90 % to 100 %, in particular from 97 % to 100 % by weight based on the total weight of the zinc nanowires disregarding the total weight of an existing surface layer.
  • the length of the zinc nanowires can be varied in a wide range, depending on the reaction conditions.
  • Zinc is electrochemically deposited onto at least one surface of an electrode.
  • the zinc nanowires show an aspect ratio of at least 100, more preferably an aspect ratio in the range from 500 to 3000, in particular in the range from 1000 to 2000.
  • the definition of the aspect ratio as used herein is for example given in WO 2013/052456, page 8, paragraph [0050].
  • the zinc nanowires obtainable or obtained by the inventive process can show different morphological arrangements, like porous structure of nanowires or closely-stacked zinc nanowires having a high-aspect-ratio.
  • the length, the thickness, the aspect ratio or the morphological arrangement of the zinc nan- owires obtained by the inventive process can be determined from the SEM images of the corresponding samples.
  • process step (a) of the inventive process zinc nanowires are directly electrochemically deposited onto at least one surface of an electrode from a solution comprising at least one zinc compound (A), at least one silicon compound (B) and at least one ionic liquid (C).
  • the method of electrochemical deposition is well known as mentioned in WO 2013/052456, page 17, paragraph [0074] and referring the literature cited therein.
  • the solution from which zinc nanowires are electrochemically deposited comprises at least one zinc compound (A), also referred to hereinafter as component (A) for short.
  • the zinc of compo- nent (A) is usually in the oxidation state +2.
  • Component (A) is preferably at least partly, preferably completely soluble in the formed solution.
  • Examples of zinc compounds (A) in the oxidation state +2 are zinc(ll) halides like ZnC , Zn(ll) triflate, zinc(ll) oxalate, zinc(ll) acetate, zinc(ll) acetylacetonate or zinc(ll) stearate.
  • Preferred zinc compounds (A) are zinc(ll) halides like zinc dichloride, zinc dibromide or zinc diiodide, in particular zinc dichloride.
  • the inventive process is characterized in that the zinc compound (A) is a zinc dihalide, in particular zinc dichloride.
  • the concentration of component (A) in the solution can be varied in a wide range depending on the solubility of component (A) in the solution.
  • the concentration of component (A) in the solution is in the range from 0.01 M to 0.5 M, more preferably in the range from 0.01 M to 0.3 M, in particular in the range from 0.02 M to 0.2 M.
  • the solution from which zinc nanowires are electrochemically deposited comprises further at least one silicon compound (B), also referred to hereinafter as component (B) for short.
  • the silicon of component (B) is usually in the oxidation state +4.
  • Component (B) is preferably at least partly, more preferably completely soluble in the formed solution.
  • silicon compounds (B) are silicon tetrahalides like SiCU or SiBr 4 , organo halo silanes like dimethyldichlorosilane, trichloro(phenyl)silane or trimethylchlorosilane.
  • Preferred silicon compounds (B) are silicon tetrahalides like silicon tetrachloride or silicon tetra- bromide, in particular silicon tetrachloride.
  • the inventive process is characterized in that the silicon compound (B) is a silicon tetrahalide, in particular silicon tetrachloride.
  • the electrochemical deposition of zinc from a solution comprising only one zinc compound (A) and an ionic liquid (C) and no silicon compound (B) results in the formation of large agglomerates of 100-200 nm hexagonal platelets of metallic zinc, while zinc nanowires are formed by the electrochemical deposition of zinc from a solution comprising component (A), component (B) and at least one ionic liquid (C), wherein the concentration of the silicon compound (B) in the solution is in the range from 0.01 M to 1 M, preferably in the range from 0.05 M to 1 M, more preferably the range from 0.1 M to 0.9 M, in particular in the range from 0.4 M to 0.8 M.
  • the inventive process is characterized in that the concentration of the silicon compound (B) in the solution is in the range from 0.4 M to 0.8 M.
  • the solution, from which zinc nanowires are electrochemically deposited comprises further at least one ionic liquid (C), also referred to hereinafter as component (C) for short.
  • Ionic liquids (C) are known to the person skilled in the art. Several ionic liquids, which are liquid salts with a melting point below 100 °C, in particular below room temperature, are commercially available or can be pre- pared according to known protocols.
  • the ionic liquid (C) can be varied in a wide range as long as component (C) is liquid at the temperature of the deposition and dissolves the components (A) and (B) sufficiently and does not chemically react with them.
  • the ions of the ionic liquid (C) preferably do not react under the conditions of the electrochemical deposition.
  • Preferred example of ionic liquids (C) is 1 -ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide.
  • the inventive process is characterized in that the ionic liquid (C) is selected from the group consisting of 1 -butyl-1 -methylpyrrolidinium bis(trifluoromethylsulfonyl) imide (BMP-TFSI) and 1 -ethyl-3-methylimidazolium
  • EMIm-TFSI bis(trifluoromethylsulfonyl) imide
  • EMIm-TFSI bis(trifluoromethylsulfonyl) imide
  • the solution might comprise further components, which are inert under the conditions of the electrochemical deposition reaction like polar aprotic solvents which are usually used in electrolytes of electrochemical cell.
  • the solution is essentially free of water, i.e. the water content in the solution is below 0.1 % by weight, preferably below 500 ppm, in particular in the range from 0.1 ppm to 10 ppm.
  • component C for example as technical grade, comprises more water than desired
  • the water can be removed by known methods, like stripping the water from component A by heating it under reduced pressure, or by adding drying reagents like molecular sieves or by adding scavengers like aluminum alkyls, magnesium alkyls or lithium alkyls. It is also possible to remove excess water by adding additional amount of silicon tetrachloride, which form insoluble compounds by reacting with water.
  • the sum of the weight of all components (A), (B) and (C) is at least 90% by weight, preferably in the range from 95% to 100% by weight, in particular in the range from 98% to 100% by weight based on the total weight of the solution.
  • a solution comprising at least one zinc compound (A), at least one silicon compound (B), wherein the concentration of the silicon compound (B) in the solution is in the range from 0.01 M to 1 M, preferably in the range from 0.1 M to 1 M, more preferably the range from 0.2 M to 0.9 M, in particular in the range from 0.4 M to 0.8 M and at least one ionic liquid (C) is also possible in the presence of at least one organic solvent (D).
  • the organic solvent (D) is a polar aprotic solvent, more preferably a polar aprotic solvent selected from the group consisting of cyclic carbonates, in particular propylene carbonate, ethylene carbonate and fluoroethylene carbonate, acetonitrile, dimethylformamide, tetrahydrofurane, acetone and dimethyl sulfoxide.
  • a polar aprotic solvent selected from the group consisting of cyclic carbonates, in particular propylene carbonate, ethylene carbonate and fluoroethylene carbonate, acetonitrile, dimethylformamide, tetrahydrofurane, acetone and dimethyl sulfoxide.
  • the inventive process is characterized in that the solution comprises at least one organic solvent (D), preferably at least one polar aprotic solvent (D), more preferably a polar aprotic solvent selected from the group consisting of cyclic car- bonates, in particular propylene carbonate, ethylene carbonate and fluoroethylene carbonate, acetonitrile, dimethylformamide, tetrahydrofurane, acetone and dimethyl sulfoxide.
  • D organic solvent
  • D preferably at least one polar aprotic solvent (D)
  • the concentration of component (C) in the solution which comprises beside component (A) and component (B) also component (D), can be varied in a wide range.
  • the concentration of all ionic liquids (C) in the solution is at least 0.05 M, more preferably at least 0.1 M, in particular at least 0.2 M up to the maximal concentration of the sum of all ionic liquids (C) in a solution comprising no organic solvent (D).
  • the inventive process is characterized in that the concentration of all ionic liquids (C) in the solution is at least 0.05 M, more preferably at least 0.1 M, in particular at least 0.2 M up to the maximal concentration of the sum of all ionic liquids
  • the inventive process is characterized in that the solution comprises at least one organic solvent (D), preferably at least one polar aprotic solvent
  • a polar aprotic solvent selected from the group consisting of cyclic carbonates, in particular propylene carbonate, ethylene carbonate and fluoroethylene carbonate, acetonitrile, dimethylformamide, tetrahydrofurane, acetone and dimethyl sulfoxide, and wherein the concentration of all ionic liquids (C) in the solution is at least 0.05 M, more preferably at least 0.1 M, in particular at least 0.2 M up to the maximal concentration of the sum of all ionic liquids (C) in a solution comprising no organic solvent (D).
  • the solution used in process step a) is usually prepared by simply mixing the components (A), (B) and (C) preferably under inert and dry, i.e. water-free, conditions, using Schlenk technique or working in a glove-box.
  • the electrochemical deposition can be take place in a wide temperature range.
  • process step (a) takes place at a temperature in the range from 0 °C to 100 °C, more preferably in the range from 15 °C to 50 °C, in particular in the range from 20 °C to 35 °C.
  • the inventive process is characterized in that process step (a) takes place at a temperature in the range from 15 °C to 50 °C, in particular in the range from 20 °C to 35 °C.
  • the time of electrochemically depositing zinc can be varied in a broad range and is preferably adjusted to the desired length of the zinc nanowires deposited.
  • the electrochemical deposition can be take place in a wide range of deposition potentials which are given by reference to a Pt quasi-reference electrode.
  • process step (a) takes place at a deposition potential in the range from -1.9 V to - 2.5 V vs. Pt quasi-reference electrode.
  • the inventive process is characterized in that process step (a) takes place at a deposition potential in the range from -1.9 V to - 2.5 V vs. Pt qua- si-reference electrode.
  • process step (a) takes place at a deposition potential in the range from -1.9 V to - 2.5 V vs. Pt qua- si-reference electrode.
  • the surface of the electrode and the solution can be static to each other or the solution is in motion relative to the surface of the electrode, e.g. by simply stirring the solution or by continuously supplying the surface of the electrode with new solution using a pump around system.
  • the surface of the electrode, where the zinc nanowires are deposited during the electrochemical deposition can be selected from a large number of electrically conductive materials like metals and conductive carbons.
  • the electrochemical deposition of the zinc nanowire takes place on the surface of an electrode, wherein the surface is composed of a material se- lected from the group consisting of copper, zinc and glassy carbon.
  • the inventive process is characterized in that the surface of the electrode, where the zinc nanowires are deposited, is composed of a material selected from the group consisting of copper, zinc, and glassy carbon.
  • Zinc nanowires with a high aspect ratio in the range from 500 to 2000 and a high number of nanowires per electrode area are preferably obtained in process step a) of the inventive process under conditions wherein the zinc compound (A) is zinc dichloride, wherein the concentration of zinc dichloride in the solution is in the range from 0.01 M to 0.3 M, in particular in the range from 0.05 to 0.2 M, and the silicon compound (B) is silicon tetrachloride, wherein the concentration of silicon tetrachloride in the solution is in the range from 0.4 M to 0.8 M, and wherein process step (a) takes place at a temperature in the range from 15 °C to 50 °C, preferably 20 °C to 35 °C, and at a deposition potential in the range from -1.9 V to - 2.5 V vs.
  • the zinc compound (A) is zinc dichloride, wherein the concentration of zinc dichloride in the solution is in the range from 0.01 M to 0.3 M, in particular in the range from
  • the inventive process is characterized in that the zinc compound (A) is zinc dichloride, wherein the concentration of zinc dichloride in the solution is in the range from 0.02 to 0.2 M, and the silicon compound (B) is silicon tetrachloride, wherein the concentration of silicon tetrachloride in the solution is in the range from 0.4 M to 0.8 M, and wherein process step (a) takes place at a temperature in the range from 15 °C to 50 °C and at a deposition potential in the range from -1.9 V to - 2.5 V vs. Pt quasi-reference electrode.
  • the zinc nanowires obtained in process step a) of the inventive process are usually isolated by separation them mechanically from the surface of the electrode, for example by cutting.
  • the isolated zinc nanowires can be used in different applications e.g. in electronics, catalysis and for the preparation of nanowires comprising zinc oxide, which can be used in sensors and solar cells.
  • the present invention also provides zinc nanowires, preferably zinc nanowires having an aspect ratio in the range from 500 to3000, in particular in the range from 1000 to 2000 obtainable by a process for producing zinc nanowires as described above.
  • This process comprises the above- described process step (a) especially also with regard to preferred embodiments thereof.
  • the present invention likewise also provides zinc nanowires, preferably zinc nanowires having an aspect ratio in the range from 500 to3000, in particular in the range from 1000 to 2000, wherein the zinc nanowires are prepared by a process comprising at least the process steps of (a) electrochemically depositing zinc directly onto at least one surface of an electrode from a solution comprising
  • the process step a) has been described above. In particular, preferred embodiments of the process step have been described above.
  • the zinc nanowires preferably zinc nanowires having an aspect ratio in the range from 500 to 3000, in particular in the range from 1000 to 2000, which are obtainable or obtained by the inventive process, are preferably crystalline.
  • the thickness of zinc nanowires obtainable or obtained by the inventive process is usually in the range from 1 nm to 100 nm, preferably in the range from 5 nm to 50 nm, in particular in the range from 10 nm to 30 nm.
  • the zinc nanowires obtainable or obtained by the inventive process can be covered by a surface layer comprising the elements silicon, oxygen and carbon. The thickness of the surface layer can vary in a wide range.
  • the thickness of the surface layer is in range of a 1/50 to 1/3, more preferably 1/20 to 1/5 of the total thickness of the nanowire.
  • the zinc nanowires, disregarding an existing surface layer consist essentially of zinc, that means that the zinc-content of the zinc nanowires is preferably at least 80 %, more preferably in the range of from 90 % to 100 %, in particular from 97 % to 100 % by weight based on the total weight of the zinc nanowires disregarding the total weight of an existing surface layer.
  • ionic liquid (IL) 1 -ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide EMIm-TFSI, lo-Li-Tec
  • SiCU (99.998%, Alfa Aesar) was used as received.
  • the electrochemical cell was made of Teflon and clamped over a Teflon-covered O-ring yielding a geometric surface area of 0.5 cm 2 of the used substrate.
  • a Pt wire was coiled into three rings with a diameter of ⁇ 1 .5 cm and was embedded into the Teflon cavity (0.6 cm deep and 0.5 cm thick) which surrounds the reaction area of the working electrode.
  • the Teflon cell looks like a small cylinder (8 mm in diameter, where the working electrode is underneath) surrounded by a bigger cylinder (18 mm in diameter, where the coiled Pt wire is placed on its Teflon ground).
  • This coiled wire was serv- ing as a counter electrode.
  • a Pt wire was immersed into the reaction solution near from the working electrode (about 2 mm away from it) to serve as a quasi-reference electrode.
  • the Teflon cell was filled with about 2 ml of 0.05 M ZnCI 2 and 0.5 M SiCI 4 in EMIm-TFSI IL solution and the substrate was a Cu foil with a geometric surface area of 0.5 cm 2 .
  • the deposition was performed by applying a constant potential of - 2.0 V vs. Pt quasi-reference electrode for 75 minutes which corresponds to a total charge flow of 0.42 C/cm 2 .
  • Figure 2 shows SEM images of the obtained Zn nanowires.
  • the Teflon cell was filled with about 2 ml solution of (0.5 M SiCI 4 + 0.1 M ZnCI 2 ) in EMIm-TFSI IL.
  • the Zn deposition on Cu foil was then performed by a constant potential of - 2.0 V vs. Pt quasi-reference electrode for 1 hour which corresponds to a total charge flow of 0.94 C/cm 2 .
  • Figure 3 shows SEM images of the obtained Zn nanowires.
  • Figure 1 SEM images of Zn deposit obtained from a solution of 0.05 M ZnC in EMIm-TFSI

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention concerne un procédé de production de nanofils de zinc comprenant au moins l'étape de procédé de dépôt électrochimique de zinc directement sur au moins une surface d'une électrode à partir d'une solution comprenant au moins un composé de zinc (A), au moins un composé de silicium (B) et au moins un liquide ionique (C).
PCT/EP2015/080914 2015-01-09 2015-12-22 Procédé de production de nanofils de zinc WO2016110409A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP15150626.8 2015-01-09
EP15150626 2015-01-09

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WO2016110409A1 true WO2016110409A1 (fr) 2016-07-14

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Citations (3)

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WO2012170311A2 (fr) 2011-06-06 2012-12-13 Washington State University Research Foundation Batteries comportant des électrodes nanostructurées et procédés associés
WO2013052456A1 (fr) 2011-10-05 2013-04-11 Nanosys, Inc. Matériaux actifs à nanostructure de silicium pour batteries au lithium-ion et procédés, compositions, composants et dispositifs s'y rapportant

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US20100258443A1 (en) * 2004-11-19 2010-10-14 The Trustees Of Boston College Methods of fabricating nanowires and electrodes having nanogaps
WO2012170311A2 (fr) 2011-06-06 2012-12-13 Washington State University Research Foundation Batteries comportant des électrodes nanostructurées et procédés associés
WO2013052456A1 (fr) 2011-10-05 2013-04-11 Nanosys, Inc. Matériaux actifs à nanostructure de silicium pour batteries au lithium-ion et procédés, compositions, composants et dispositifs s'y rapportant
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