Solution process for transparent conductive oxide coatings
View Patent ↗A process according to the present invention comprises combining in a reaction mixture at least one metal alkyl compound of formula MR x with at least one silanol compound of formula; forming a film from the reaction mixture; and treating the film with heat and moisture; wherein an amount of the at least one silanol compound present ranges from about one quarter to about three quarters of an amount required to replace all alkyl groups of the at least one metal alkyl compounds with groups derived from the at least one silanol compound; M is, independently at each occurrence, Zn, Cd, Al, Ga, In, Tl, Hg, Pb, Bi or a combination thereof; x is, independently at each occurrence, an integer equal to 2 or 3; z is 0, 1 or 2; R is, independently at each occurrence, alkyl; and R 1 -R 5 is independently H, alkyl, or hydroxyl.
1. A process comprising
combining in a reaction mixture at least one metal alkyl compound of formula MR x with at least one silanol compound of formula;
forming a film from the reaction mixture; and
treating the film with heat and moisture to form a metal oxide film comprising ≦0.6 atomic % silicon;
wherein an amount of the at least one silanol compound present ranges from about one quarter to about three quarters of an amount required to replace all alkyl groups of the at least one metal alkyl compounds with groups derived from the at least one silanol compound;
M is, independently at each occurrence, Zn, Cd, Al, Ga, In, Tl, Hg, Pb, Bi or a combination thereof;
x is, independently at each occurrence, an integer equal to 2 or 3;
z is 1 or 2;
R is, independently at each occurrence, alkyl; and
R 1 -R 5 is independently H or alkyl.
2. A process according to claim 1 , comprising combining at least two metal alkyl compounds of formula MR x with the at least one silanol compound.
3. A process according to claim 1 , wherein the at least one metal alkyl compound of formula MR x is ZnR 2 .
4. A process according to claim 1 , comprising combining ZnR 2 and AlR 3 with the at least one silanol compound of formula I.
5. A process according to claim 1 , wherein R is C 1-12 alkyl.
6. A process according to claim 1 , wherein R is C 1-4 alkyl.
7. A process according to claim 1 , wherein M is Zn, Al, In, Ga, or Cd.
8. A process according to claim 1 , wherein M is Zn, Cd, Al, Ga, In, Pb, Bi or a combination thereof.
9. A process according to claim 1 , wherein the amount of the at least one silanol compound present ranges from about one third to about two thirds of the amount required to replace all alkyl groups of the at least one metal alkyl compounds with groups derived from the at least one silanol compound.
10. A process according to claim 1 , wherein the amount of the at least one silanol compound present ranges from about two fifths to about three fifths of the amount required to replace all alkyl groups of the at least one metal alkyl compounds with groups derived from the at least one silanol compound.
11. A process according to claim 1 wherein both the metal alkyl compound of formula MR x and the at least one silanol compound are dissolved in one or more solvents.
12. A process according to claim 1 , wherein the amount of the at least one silanol compound present is about two thirds of the amount required to replace all alkyl groups of the at least one metal alkyl compounds with groups derived from the at least one silanol compound.