Method for the production of metal oxide-containing layers

Patent metadata

Field	Value
Publication number	US-9309595-B2
Application number	US-201013390840-A
Country	US
Kind code	B2
Filing date	Aug 13, 2010
Priority date	Aug 21, 2009
Publication date	Apr 12, 2016
Grant date	Apr 12, 2016

Abstract

The invention relates to a liquid-phase method for producing metal oxide-containing layers from nonaqueous solution. In said method, an anhydrous composition containing i) at least one metal oxo-alkoxide of generic formula M x O y (OR) z [O(R′O) c H] a X b [R″OH] d , where M=In, Ga, Sn, and/or Zn, x=3-25, y=1-10, z=3-50, a=0-25, b=0-20, c=0-1, d=0-25, R, R′, R″=organic group, X═F, Cl, Br, I, and ii) at least one solvent is applied to a substrate, is optionally dried, and is converted into a metal oxide-containing layer. The invention also relates to the layers that can be produced using the method of the invention and to the use thereof.

First claim

The invention claimed is:

1. A process for producing a metal oxide-containing layer, the process comprising applying an anhydrous solution to a substrate, optionally drying a resulting coated substrate and converting a coating formed from said anhydrous solution to form a metal oxide-containing layer, wherein the anhydrous solution comprises:
i) a metal oxo alkoxide of formula (I):
M x O y (OR) z [O(R′O) c H] a X b [R″OH] d   (I),

wherein
x=3-25,
y=1-10,
z=3-50,
a=0-25,
b=0-20,
c=0-1,
d=0-25,
M=In, Ga, Sn, Zn, or a mixture thereof,
R, R′, R″ individually represent an organic radical,
X=F, Cl, Br, or I; and

ii) a solvent.

2. The process of claim 1 , wherein the metal oxo alkoxide is an oxo alkoxide of formula (II):
M x O y (OR) z   (II),

wherein
x=3-20,
y=1-8,
z=1-25, and
OR=C1-C15-alkoxy, -oxyalkylalkoxy, -aryloxy- or -oxyarylalkoxy group.

3. The process of claim 2 , wherein the metal oxo alkoxide is selected from the group consisting of [In 5 (μ 5 -O)(μ 3 -O i Pr) 4 (μ 2 -O i Pr) 4 (O i Pr) 5 ], [Sn 3 O(O i Bu) 10 ( i BuOH) 2 ], [Sn 6 O 4 (OR) 4 ], or a mixture thereof.

4. The process of claim 1 , wherein the metal oxo alkoxide is the only metal oxide precursor in the process.

5. The process of claim 1 , wherein the metal oxo alkoxide is present in a proportion of 0.1 to 15% by weight, based on a total mass of the anhydrous solution.

6. The process of claim 1 , wherein the solvent is an aprotic or weakly protic solvent.

7. The process of claim 1 , wherein the solvent is at least one selected from the group consisting of methanol, ethanol, isopropanol, tetrahydrofurfuryl alcohol, tert-butanol and toluene.

8. The process of claim 1 , wherein the anhydrous solution has a viscosity of 1 mPa·s to 10 Pa·s.

9. The process of claim 1 , wherein the substrate comprises at least one selected from the group consisting of glass, silicon, silicon dioxide, a metal oxide, a transition metal oxide, a metal and a polymeric material.

10. The process of claim 1 , wherein the anhydrous solution is applied to the substrate by a printing process, a spraying process, a rotary coating process, a dipping process, or a process selected from the group consisting of meniscus coating, slit coating, slot-die coating and curtain coating.

11. The process of claim 1 , further comprising:
heating the resulting coated substrate at temperatures greater than 150° C.

12. The process of claim 11 , further comprising:
irradiating the resulting coated substrate with UV, IR or VIS radiation before, during or after the heating.

13. The process of claim 2 , wherein
x=3-15,
y=1-5,
z=10-20, and
OR=-OCH 3 , —OCH 2 CH 3 , —OCH 2 CH 2 OCH 3 , —OCH(CH 3 ) 2 or —O(CH 3 ) 3 .

Assignees

• Steiger Juergen
• Pham Duy Vu
• Thiem Heiko
• Merkulov Alexey
• Hoppe Arne
• Evonik Degussa Gmbh

Inventors

• Steiger Juergen
• Pham Duy Vu
• Thiem Heiko
• Merkulov Alexey
• Hoppe Arne

Classifications

• C23C18/1258

  Spray pyrolysis · CPC title

• C23C18/1216 Primary

  Metal oxides (C23C18/1212 takes precedence) · CPC title