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
  • C23C18/02—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 thermal decomposition
  • C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
  • C23C18/1204—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
  • C23C18/1208—Oxides, e.g. ceramics
  • C23C18/1216—Metal oxides
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/02104—Forming layers
  • H01L21/02365—Forming inorganic semiconducting materials on a substrate
  • H01L21/02518—Deposited layers
  • H01L21/02521—Materials
  • H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
  • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
  • C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
• • 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
  • C23C18/02—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 thermal decomposition
  • C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
  • C23C18/125—Process of deposition of the inorganic material
  • C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
• • 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
  • C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
• • 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
  • C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
  • C23C18/143—Radiation by light, e.g. photolysis or pyrolysis
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/02104—Forming layers
  • H01L21/02365—Forming inorganic semiconducting materials on a substrate
  • H01L21/02612—Formation types
  • H01L21/02617—Deposition types
  • H01L21/02623—Liquid deposition
  • H01L21/02628—Liquid deposition using solutions
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
  • H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/18, H10D48/04 and H10D48/07, with or without impurities, e.g. doping materials
  • H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
  • H01L21/477—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
  • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
  • H10D62/80—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
  • H10F71/00—Manufacture or treatment of devices covered by this subclass
  • H10F71/138—Manufacture of transparent electrodes, e.g. transparent conductive oxides [TCO] or indium tin oxide [ITO] electrodes
• • 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
  • C23C18/02—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 thermal decomposition
  • C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
  • C23C18/125—Process of deposition of the inorganic material
  • C23C18/1254—Sol or sol-gel processing
• • 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
  • C23C18/02—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 thermal decomposition
  • C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
  • C23C18/125—Process of deposition of the inorganic material
  • C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E10/00—Energy generation through renewable energy sources
  • Y02E10/50—Photovoltaic [PV] energy

Definitions

• the invention relates to a process for the production of indium oxide-containing layers, to the process usable precursors and coating compositions, the processable layers and their use.
• Indium oxide indium (III) oxide, ln 2 O 3
• Indium (III) oxide, ln 2 O 3 ) is between 3.6 and 3.75 eV (measured for evaporated layers) due to the large band gap [HS Kim, PD Byrne, A. Facchetti, TJ Marks; J. Am. Chem. Soc. 2008, 130, 12580-12581] is a promising semiconductor.
• thin films of a few hundred nanometers in thickness can have a high transparency in the visible spectral range of greater than 90% at 550 nm.
• charge carrier mobilities of up to 160 cm 2 / Vs.
• Indium oxide is often used primarily together with tin (IV) oxide (SnO 2 ) as semiconducting mixed oxide ITO. Due to the relatively high conductivity of ITO layers with simultaneous transparency in the visible spectral range, it is used, inter alia, in the field of liquid crystal displays (LCDs), in particular as “transparent electrodes.” These mostly doped metal oxide layers become industrially above all else produced by cost-intensive Aufdampfmethoden in a high vacuum.
• ITO layers and pure indium oxide layers, and their preparation are thus of great importance for the
• indium oxide-containing layers A variety of classes of compounds are discussed as possible starting materials or precursors for the synthesis of indium oxide-containing layers. These include, for example, indium salts. Thus, Marks et al. Components in whose preparation a precursor solution of lnCl 3 and the base monoethanolamine (MEA) dissolved in methoxyethanol is used.
• MEA base monoethanolamine
• indium alkoxides are discussed as possible starting materials or precursors for indium oxide synthesis.
• indium alkoxides and indium oxoalkoxides are described in the prior art.
• indium oxoalkoxides also have at least one further oxygen radical (oxo radical) bonded directly to an indium atom or bridging at least two indium atoms.
• indium (III) chloride (InCl 3 ) with Na-OR, where R is methyl, ethyl, iso-propyl, n-, s-, t-butyl and -pentyl radicals.
• Metal oxide layers can be prepared in principle by various methods.
• metal oxide layers are based on sputtering techniques.
• metal oxide layers are based on chemical vapor deposition.
• indium oxide-containing layers of indium oxide precursors such as indium alkoxides or Indiumoxoalkoxiden on
• Gas phase deposition can be produced.
• metal oxide layers are advantageously produced by liquid-phase techniques, i. by processes comprising at least one process step before the conversion to the metal oxide, in which the substrate to be coated is coated with a liquid solution of at least one precursor of the metal oxide, optionally subsequently dried and converted.
• a metal oxide precursor in this case is a compound which can be decomposed thermally or with electromagnetic radiation and with which metal oxide-containing layers can be formed in the presence or absence of oxygen or other oxidizing substances.
• Prominent examples of metal oxide precursors are, for. B. metal alkoxides and
• the layer production can be carried out i) by sol-gel processes in which the metal alkoxides used are first converted into gels in the presence of water by hydrolysis and subsequent condensation and then converted into metal oxides, or ii) by conversion from non-aqueous solution.
• metal alkoxide eg, one of the generic formula R 1 M- (OR 2 ) yx
• a metal alkoxide eg, one of the generic formula R 1 M- (OR 2 ) yx
• the usable metal alkoxides may be, inter alia, those of indium, gallium, tin or zinc.
• indium oxide-containing layers which can be produced by this process are very inhomogeneous, have no satisfactory electrical properties and, in particular, are not sufficiently stable with regard to atmospheric influences and electrical stress.
• JP 2007-042689 A describes metal alkoxide solutions which may contain indium alkoxides, as well as processes for the production of semiconductor components which use these metal alkoxide solutions.
• the metal alkoxide films are thermally treated and converted to the oxide layer transformed.
• these systems also do not provide sufficiently homogeneous films with sufficiently good electrical properties and sufficient stability with respect to atmospheric influences and electrical stress. Pure indium oxide layers can furthermore not be produced by the process described there.
• WO 2010/094581 A1 describes the use of indium alkoxides in the production of indium oxide-containing layers from anhydrous solutions. Although the resulting layers are more homogeneous than those produced by sol-gel processes, the use of indium alkoxides in anhydrous systems still has the disadvantage that the conversion of indium alkoxide-containing formulations to indium oxide-containing layers does not provide sufficiently good electrical performance and performance there is no sufficient stability with respect to atmospheric influences and electrical stress of the resulting layer.
• WO 2011/072887 A1 discloses a process for the preparation of indium halodialkoxides of the generic formula lnX (OR) 2 and WO 2011/073005 A2 a liquid phase process for producing indium oxide-containing layers employing compositions comprising at least one such Indiumhalogendialkoxid lnX (OR) 2 .
• the electrical properties are already improved over the prior art heretofore cited, the resulting indium alkoxide-containing layers do not yet have sufficiently good electrical properties and sufficient stability with respect to atmospheric influences and electrical stress. This may possibly be attributed to the fact that chloride residues are attributed to a saturation of the valences of the oxygen in the resulting metal oxide semiconductor and thus to a
• WO 201 1/020781 A1 finally describes a liquid-phase process for producing indium-oxide-containing layers employing compositions containing indium oxoalkoxides of the generic formula M x Oy (OR) z [O (RO) c H] a X b [R "OH] d , the indium oxide Layers with targeted, uniform and reproducible stoichiometry, high homogeneity and better electrical performance leads.
• these indium oxide-containing layers do not yet have sufficiently good electrical properties and, above all, insufficient stability with respect to atmospheric influences (in particular with respect to oxygen and / or water contained in the atmosphere) and electrical stress
• a method is to be provided which leads to indium oxide layers with targeted, uniform and reproducible stoichiometry, high homogeneity, good electrical performance and good stability with regard to atmospheric influences and electrical stress.
• R, R 'and R "are C 1 -C 15 -alkyl, -alkoxyalkyl, -aryl or -oxyarylalkyl groups (where the prefix C 1 -C 15 is in each case radicals with 1 to 15 carbon atoms), and particularly preferred radicals R , R 'and R "are -CH 3 , - -CH 2 CH 2 OCH 3 , -CH (CH 3 ) 2 , -CH (CH 3 ) CH 2 OCH 3 , -C (CH 3 ) 3 and
• liquid phase process according to the invention for producing indium oxide-containing layers from solution is a process comprising at least one
• Process step in which the substrate to be coated is coated with a liquid solution containing at least one metal oxide precursor and optionally subsequently dried.
• this is not a sputtering or CVD process.
• the liquid phase process according to the invention can be carried out either with non-aqueous Compositions or as a sol-gel process with aqueous compositions.
• the process according to the invention is preferably an anhydrous process.
• Under a metal oxide precursor is a thermal or with
• liquid compositions are to be understood as meaning those which are stable under SATP conditions ("Standard Ambient
• a solution or an anhydrous composition is a solution or
• aqueous compositions have overlying water contents.
• the layer containing indium oxide is to be understood as meaning a metal- or semimetallin-containing layer which has indium atoms or ions which are substantially oxidic.
• the indium oxide-containing layer may also carbene, halogen or alkoxide fractions resulting from incomplete conversion or incomplete removal
• the indium oxide-containing layer may be a pure indium oxide layer, i. when ignoring any carbene, alkoxide or halogen fractions essentially consist of oxidically present indium atoms or ions, or proportionally even more metals, which may be present even in elemental or oxidic form having.
• indium-containing precursors preferably only indium oxoalkoxide compounds and optionally indium alkoxides, should be used in the process according to the invention.
• other layers comprising metals in addition to the indium-containing precursors, are also precursors of metals in the oxidation state 0 (for producing layers containing further metals in neutral form) or metal oxide precursors (such as, for example, other metal alkoxides or - oxoalkoxides).
• inventive precursors of the generic formula M x O y (OR) z [O (RO) eH] a X b Yc [R "OH] d which have not hitherto been described in the literature, can be prepared, for example, by reacting AgNO 3 or a tendency to be ionic Compound whose cation is a sparingly soluble
• the present inventive method is particularly well suited for the production of indium oxide layers, when the Indiumoxoalkoxid is used as the sole metal oxide precursor. Very good layers result when the sole metal oxide precursor has the generic formula ln 6 O (OCH 2 CH 2 OCH 3 ) 10 (NO 3 ) 6.
• the at least one indium oxoalkoxide is preferably present in proportions of from 0.1 to 15% by weight, more preferably from 1 to 10% by weight, very preferably from 2 to 5% by weight, based on the total weight of the composition.
• the composition further contains at least one solvent, i. the composition may contain both a solvent or a mixture of different solvents.
• aprotic and weakly protic solvents i. those selected from the group of aprotic nonpolar solvents, i. alkanes, substituted alkanes, alkenes, alkynes, aromatics with or without aliphatic or aromatic substituents, halogenated hydrocarbons, tetramethylsilane, the group of aprotic polar solvents, i.
• Particularly preferably usable solvents are alcohols and toluene, xylene, anisole, mesitylene, n-hexane, n-heptane, tris (3,6-dioxaheptyl) -amine (TDA), 2-aminomethyltetrahydrofuran, phenetole, 4-methylanisole, 3 Methylanisole, methyl benzoate, N-methyl-2-pyrrolidone (NMP), tetralin, ethyl benzoate and diethyl ether.
• Very particularly preferred solvents are methanol, ethanol, isopropanol, tetrahydrofurfuryl alcohol,
• composition used in the process according to the invention preferably has a viscosity of from 1 mPa.s to 10 Pa.s, in particular from 1 mPa.s to 100 mPa.s determined in accordance with DIN 53019 Parts 1 to 2 and to achieve particularly good printability or coatability at 20 ° C on. Corresponding viscosities can be achieved by adding
• Polymers cellulose derivatives, or, for example under the trade name Aerosil available Si0 2 , and in particular by PMMA, polyvinyl alcohol, urethane thickener or
• Polyacrylatverdicker be adjusted.
• the substrate used in the method according to the invention is preferably a substrate consisting of glass, silicon, silicon dioxide, a metal or transition metal oxide, a metal or a polymeric material, in particular PI or PET.
• the process according to the invention is particularly advantageously a coating process selected from printing processes (in particular flexographic / gravure printing, inkjet printing, offset printing, digital offset printing and screen printing), spraying processes, spin-coating processes, dip processes (dip -coating ”) and methods selected from Meniscus Coating, Slit Coating, Slot Die Coating, and Curtain Coating.
• the coating process of the invention is a printing process.
• the coated substrate After coating and before conversion, the coated substrate can continue to be dried. Corresponding measures and conditions for this are known to the person skilled in the art.
• the conversion to an indium oxide-containing layer can be effected by thermal means and / or by irradiation with electromagnetic, in particular actinic radiation.
• the conversion takes place on the thermal paths through temperatures of greater than 150 ° C. Particularly good results can be achieved, however, if temperatures of 250 ° C to 360 ° C are used for the conversion.
• the thermal conversion can furthermore be assisted by irradiating UV, IR or VIS radiation before or during the thermal treatment or by treating the coated substrate with air or oxygen.
• the quality of the layer produced by the process according to the invention can furthermore be determined by a combined temperature and gas treatment (with H 2 or O 2 ), plasma treatment (Ar, N 2 , O 2 or H 2 plasma) following the conversion step, laser treatment. Treatment (with wavelengths in the UV, VIS or IR range) or an ozone treatment can be further improved.
• the present invention furthermore relates to the indium oxoalkoxides of the generic formula M x Oy (OR) z [O (RO) eH] a X b Yc [R "OH] d
• the composition may contain both a solvent and a mixture of different solvents.
• aprotic and weakly protic solvents ie. H. those selected from the group of aprotic nonpolar solvents, d. H. alkanes, substituted alkanes, alkenes, alkynes, aromatics with or without aliphatic or aromatic substituents, halogenated hydrocarbons, tetramethylsilane, the group of aprotic polar solvents, i.
• Propylene carbonate and the weak protic solvent d. H. alcohols, primary and secondary amines and formamide.
• Particularly preferably usable solvents are alcohols and toluene, xylene, anisole, mesitylene, n-hexane, n-heptane, tris (3,6-dioxaheptyl) -amine (TDA), 2-aminomethyltetrahydrofuran, phenetole, 4-methylanisole, 3 Methylanisole, methyl benzoate, N-methyl-2-pyrrolidone (NMP), tetralin, ethyl benzoate and diethyl ether.
• Very particularly preferred solvents are methanol, ethanol, isopropanol, tetrahydrofurfuryl alcohol,
• the invention furthermore relates to indium oxide-containing layers which can be prepared by the process according to the invention.
• Particularly good properties have indium oxide-containing layers which can be prepared by the process according to the invention, the pure ones
• Indium oxide layers are.
• the indium oxide-containing layers which can be produced by the process according to the invention are advantageously suitable for the production of electronic components, in particular the production of transistors (in particular thin-film transistors), diodes, sensors or solar cells.
• the synthesis is carried out in the absence of atmospheric oxygen.
• the synthesis is carried out in the absence of atmospheric oxygen.
• a doped silicon substrate having an edge length of about 15 mm and having an approximately 200 nm thick silicon oxide coating and ITO / gold finger structures was coated with 100 ⁇ of a 5% by weight solution containing the product formed according to example 1 b) in 2. Methoxyethanol by spin coating (2000 rpm 30s) coated. After the coating operation, the coated substrate was annealed in the air at a temperature of 350 ° C for 1 hour.
• the semiconductor layer was passivated with a layer of polydimethylsiloxane (PDMSi).
• PDMSi polydimethylsiloxane
• a doped silicon substrate having an edge length of about 15 mm and having an approximately 200 nm thick silicon oxide coating and ITO / gold finger structures was spin-coated with 100 ⁇ of a 5% by weight solution containing indium chlorodimethoxide in 2-methoxyethanol (2000 rpm 30s). After the coating operation, the coated substrate was annealed in the air at a temperature of 350 ° C for 1 hour.
• the semiconductor layer was passivated with a layer of polydimethylsiloxane (PDMSi). The solution of PDMSi from BuOH was spin-coated and the sample was then annealed at 350 ° C. for 1 h.
• PDMSi polydimethylsiloxane
• the shift of the OnSet voltage is -3.5V and -7.5V.
• the coating of the invention has a better stability to atmospheric influences, in particular.

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• General Physics & Mathematics (AREA)
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• Health & Medical Sciences (AREA)
• Chemically Coating (AREA)
• Oxygen, Ozone, And Oxides In General (AREA)
• Formation Of Insulating Films (AREA)
• Thin Film Transistor (AREA)
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• 2012
  • 2012-06-13 DE DE102012209918A patent/DE102012209918A1/de not_active Withdrawn
• 2013
  • 2013-06-04 EP EP13726540.1A patent/EP2861782B1/de not_active Not-in-force
  • 2013-06-04 CN CN201380030864.1A patent/CN104350179B/zh not_active Expired - Fee Related
  • 2013-06-04 US US14/407,681 patent/US9293326B2/en not_active Expired - Fee Related
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  • 2013-06-04 JP JP2015516550A patent/JP6195916B2/ja not_active Expired - Fee Related
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