Precursors for the production of thin oxide layers and the use thereof

Patent metadata

Field	Value
Publication number	US-10060033-B2
Application number	US-201414915330-A
Country	US
Kind code	B2
Filing date	Aug 4, 2014
Priority date	Sep 3, 2013
Publication date	Aug 28, 2018
Grant date	Aug 28, 2018

Abstract

The present invention relates to novel precursors in the form of metal complexes with 2-substituted 1,3-diketones and to a process for the preparation thereof. The invention furthermore relates to the use thereof for the production of thin metal-oxide layers. The latter are constituents in a very wide variety of electronic components and devices having various functions.

First claim

The invention claimed is:

1. A process for preparing a thin metal-oxide layer, dissolving or dispersing one or more metal complex(es) according to formula (I) or a metal-complex cluster thereof in a solvent or solvent mixture
M l [R 1 —CO—C(H) m X—CO—R 2 ] n ,  (I)

in which
M denotes a metal atom selected from zinc, indium, gallium, tin, aluminum, zirconium, titanium and hafnium,
l denotes 1 or 2,
m denotes 0 or 1,
n denotes 1, 2, 3 or 4,
R 1 and R 2 , independently of one another, denote alkyl having 1 to 8 C atoms, cycloalkyl having 3 to 7 C atoms, alkoxy having 1 to 8 C atoms and/or amino, NHR 3 or NR 3 R 4 , where R 3 and R 4 , independently of one another, denote alkyl having 1 to 8 C atoms or cycloalkyl having 3 to 7 C atoms,
and
X denotes hydroxyimino, nitro, sulfo, —SO 2 -alkyl having 1 to 8 C atoms, phosphato, —PO(O—R*) 2 where R* is alkyl having 1 to 8 C atoms or alkoxy having 1 to 8 C atoms, —SnR** 3 where R** is alkyl having 1 to 8 C atoms; —SR*** where R*** is H, alkyl having 1 to 8 C atoms or cycloalkyl having 3 to 7 C atoms, halide, or pseudohalide;

optionally adding to the solution or dispersion obtained liquefiers, stabilizers, binders and/or antifoams,
applying the solution or dispersion obtained by wet coating to a substrate surface to be coated to form a layer,
drying the applied layer and converting the applied layer into a metal oxide in the form of a thin layer by heating and calcination at a temperature in the range of 150-350° C.

2. The process according to claim 1 , wherein said solution or dispersion comprises a solvent selected from methoxyethanol, dimethylformamide and dimethoxyethane, in pure form or in a mixture, optionally in the presence of water.

3. The process according to claim 1 , wherein said solution or dispersion is applied to the substrate surface by spin coating, dip coating, spray coating, ink-jet printing, flexographic printing or gravure printing.

4. The process according to claim 1 , wherein thin oxide layers of the metals zinc, indium, gallium, tin, aluminum, zirconium, titanium and/or hafnium are produced in which oxides are present in pure form or in a mixture, or as mixed oxides.

5. The process according to claim 1 , wherein said solution or dispersion is applied a plurality of times to the substrate surface before the heating and calcination, with each layer is dried and heated individually.

6. A process according to claim 1 , wherein the conversion of the applied layer into a metal oxide in the form of a thin layer is performed in by UV or IR irradiation.

7. A process according to claim 1 , wherein the conversion of the applied layer into a metal oxide in the form of a thin layer is performed in by laser irradiation.

8. A process according to claim 1 , wherein X is —SO 2 -alkyl having 1 to 8 C atoms, —PO(O—R*) 2 where R* is alkyl having 1 to 8 C atoms or alkoxy having 1 to 8 C atoms, —SnR** 3 where R** is alkyl having 1 to 8 C atoms, —SR*** where R*** is H, alkyl having 1 to 8 C atoms or cycloalkyl having 3 to 7 C atoms, F, Cl, Br, I, —CN, —N 3 , —OCN, —NCO, —CNO, —SCN or —SeCN.

9. The process according to claim 1 , wherein conversion of the applied, dried metal-complex layer is carried out by heating and calcination at temperatures in the range from 250-350° C.

10. A process according to claim 1 , wherein the conversion of the applied layer into a metal oxide in the form of a thin layer is performed in by heating in an oven or on a hotplate.

11. The process according to claim 1 , wherein the metal complex of formula (I) is a zinc complex with nitrodimethyl malonate, a zinc complex with hydroxyiminodimethyl malonate, a zinc complex with nitromalonic acid diamide, a tin(II) complex with nitrodimethyl malonate, an indium complex with nitrodimethyl malonate, a zirconium complex with hydroxyiminodimethyl malonate, or a zirconium complex with nitrodimethyl malonate.

Assignees

• Merck Patent Gmbh

Inventors

• Bonrad Klaus
• Schneider Joerg
• Hoffman Rudolf
• Kaloumenos Mareiki

Classifications

• H10P14/3434

  being oxide semiconductor materials (Group IIB-VIA semiconductor materials H10P14/3424) · CPC title

• H10P14/3426

  Oxides · CPC title

• H10P14/265

  using solutions · CPC title

• H10P14/47

  Electrolytic deposition, i.e. electroplating; Electroless plating · CPC title

• H10P14/38

  characterised by treatments done after the formation of the materials · CPC title