IP Library Granted Patent US 9,309,595
Granted Patent B2
US 9,309,595 · App. 13/390,840 · Granted Apr 12, 2016

Method for the production of metal oxide-containing layers

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Quick Facts
Patent No.
US 9,309,595
App. No.
13/390,840
Granted
Apr 12, 2016
Kind
B2
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.

Claims (39)

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 .

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 11, 2012
From: STEIGER, JUERGEN; PHAM, DUY VU; THIEM, HEIKO; MERKULOV, ALEXEY; HOPPE, ARNE
To: EVONIK DEGUSSA GMBH
Reel/Frame 028026/0765 →