Indium oxoalkoxides for producing coatings containing indium oxide

Abstract

The present invention relates to halogenated indium oxo alkoxides of the generic formula In.sub.7O.sub.2(OH)(OR).sub.12X.sub.4(ROH).sub.x where R=C1-C15-alkyl, C1-C15-alkenyl, C1-C15-alkynyl, C1-C15-alkoxyalkyl, C6-C15-aryl- or C7-C15-alkoxyaryl, XF, Cl, Br, I and x=0 to 10, to processes for preparation thereof and to use thereof.

Claims

1. A halogenated indium oxo alkoxide of formula In.sub.7O.sub.2(OH)(OR).sub.12X.sub.4(ROH).sub.x wherein R is C1-C15-alkyl, C1-C15-alkenyl, C1-C15-alkynyl, C1-C15-alkoxyalkyl, C6-C15-aryl- or C7-C15-alkoxyaryl, X is F, Cl, Br, or I, and x is from 0 to 10.

2. The indium oxo alkoxide according to claim 1, of formula:
In.sub.7(.sub.4-O).sub.2(.sub.2-OH)(.sub.1-OEt).sub.3(.sub.2-OEt).sub.7(.sub.3-OET).sub.2(.sub.1-Cl).sub.4.

3. A process of preparing the indium oxo alkoxide according to claim 1, the process comprising: reacting a reaction mixture comprising an indium(III) halide InX.sub.3, a sodium or potassium isopropoxid; and isopropanol and optionally filtering off an intermediate solid and washing the intermediate solid with isopropanol, thereby obtaining an isopropanol-comprising wash solution, removing isopropanol from the reaction mixture, the isopropanol-comprising wash solution, or both, thereby obtaining a solid, taking up the solid obtained after removing isopropanol in an alcohol ROH, thereby obtaining a mixture, optionally filtering the mixture obtained in taking up the solid, and crystallizing the indium oxo alkoxide out of the mixture obtained in taking up the solid.

4. The process of claim 3, wherein the indium(III) halide InX.sub.3 is InCl.sub.3 and the alcohol is selected from the group consisting of CH.sub.3OH, HOCH.sub.2CH.sub.3, HOCH.sub.2CH.sub.2CH.sub.3, HOCH(CH.sub.3).sub.2, HOCH.sub.2CH.sub.2CH.sub.2CH.sub.3, HOCH(CH.sub.3)(CH.sub.2CH.sub.3) and HOC(CH.sub.3).sub.3.

5. A coating, comprising: the indium oxo alkoxide according to claim 1.

6. The coating according to claim 5, obtained by a process comprising depositing the coating from nonaqueous solution.

7. A liquid coating composition, comprising: the indium oxo alkoxide according to claim 1.

8. An electronic component, comprising: the indium oxo alkoxide according to claim 1.

9. The process of claim 3, wherein the process comprises filtering the mixture obtained in taking up the solid.

10. The electronic component of claim 8, wherein the component is a transistor, a display, an RFID tag, a circuit, a diode, a sensor, or a solar cell.

11. The process of claim 3, wherein a molar ratio of the sodium or potassium isopropoxide to the indium(III) halide InX.sub.3 in the reacting is from 2.0:1 to 2.51:1.

12. The process of claim 11, wherein the molar ratio of the sodium or potassium isopropoxide to the indium(III) halide InX.sub.3 in the reacting is from 2.4:1 to 2.5:1.

13. The process of claim 3, wherein a molar ratio of the isopropanol to the indium(III) halide InX.sub.3 in the reacting is from 5:1 to 3000:1.

14. The process of claim 13, wherein the molar ratio of the isopropanol to the indium(III) halide InX.sub.3 in the reacting is from 15:1 to 100:1.

15. The process of claim 3, wherein the reaction mixture comprises, as precursors, only precursors that comprise indium.

16. The process of claim 3, wherein the reaction mixture further comprises a precursor comprising a metal other than indium in a 0 oxidation state or a metal oxide precursor comprising a metal other than indium.

17. An anhydrous composition, comprising: the halogenated indium oxo alkoxide of claim 1, and a solvent.

18. The composition of claim 17, wherein a content of the alkoxide is from 0.1 to 15% by weight, based on a total mass of the composition.

19. The composition of claim 17, wherein a viscosity of the composition is from 1 to 10 mPa.Math.s determined to DIN 53019 parts 1 to 2 and measured at 20 C.

Description

WORKING EXAMPLES

Synthesis of In7(4-O)2(2-OH)(1-OEt)3(2-OEt)7(3-OET)2(1-Cl)4(1-HOEt)5

(1) In a 1 l glass round-bottom flask which had been freed of residual moisture, 1.3 g of sodium (56.55 mmol, 2.5 equivalents) were dissolved in 250 ml of isopropanol under a protective gas atmosphere and reflux. To the NaO.sup.iPr solution formed were added 5.0 g (22.6 mmol) of indium(III) chloride (InCl.sub.3) in 250 ml of dried isopropanol. The reaction mixture was stirred vigorously under reflux for two hours. After cooling, the solution was filtered and the precipitate was washed twice with 100 ml each time of isopropanol. The combined liquid fractions were concentrated under reduced pressure. The remaining solid was taken up in 200 ml of ethanol (<10 ppm of H.sub.2O) and filtered. At approx. 1 week, crystals were formed from the solution at 30 C. (yield approx. 20%). According to single crystal structure analysis, the molecular structure in the crystal corresponds to the formula
In.sub.7(.sub.4-O).sub.2(.sub.2-OH)(.sub.1-OEt).sub.3(.sub.2-OEt).sub.7(.sub.3-OET).sub.2(.sub.1-Cl).sub.4(.sub.1-HOEt).sub.5.
Production of Indium Oxide Layers

(2) A doped silicon substrate with an edge length of about 15 mm and with a silicon oxide coating of thickness approx. 200 nm and finger structures of ITO/gold was coated with 100 l of a 5% by weight solution of In.sub.7(.sub.4-O).sub.2(.sub.2-OH)(.sub.1-OEt).sub.3(.sub.2-OEt).sub.7(.sub.3-OET).sub.2(.sub.1-Cl).sub.4(.sub.1-HOEt).sub.5 in alcohol (methanol, ethanol or isopropanol) or toluene by spin-coating (2000 rpm). After the coating operation, the coated substrate was heat treated under air at a temperature of 260 C. or 350 C. for one hour.

(3) The inventive coating shows a charge carrier mobility of up to 1.5 cm.sup.2/Vs (at gate-source voltage 30 V, source-drain voltage 30 V, channel width 1 cm and channel length 20 m).

(4) TABLE-US-00001 TABLE 1 Charge carrier mobilities Charge carrier mobility/cm.sup.2V.sup.1s.sup.1 Solvents 260 C. 350 C. Methanol 0.2 1.0 Ethanol 0.25 1.1 Isopropanol 0.5 1.5 Toluene 0.1 0.8