Electrochromic devices and methods
View Patent ↗A heat treated electrochromic device comprising an anodic complementary counter electrode layer comprised of a mixed tungsten-nickel oxide and lithium, which provides a high transmission in the fully intercalated state and which is capable of long term stability, is disclosed. Methods of making an electrochromic device comprising an anodic complementary counter electrode comprised of a mixed tungsten-nickel oxide are also disclosed.
1. A method for the preparation of an electrochromic device comprising:
a) providing a first conductive layer,
b) depositing one of an electrochromic layer or a counter electrode layer on said first conductive layer, thereby providing a first deposited electrode,
c) depositing an ion-conductor layer on said first deposited electrode,
d) depositing the other of said electrochromic layer or said counter electrode layer on said ion-conductor layer, thereby providing a second deposited electrode,
e) depositing lithium onto said second deposited electrode whereby a mixed tungsten-nickel oxide of the counter electrode layer is reduced,
f) depositing a second conductive layer on said second deposited electrode, and
g) heat treating said electrochromic device,
wherein said counter electrode layer comprises a mixed tungsten-nickel oxide,
wherein said mixed tungsten-nickel oxide in said electrochromic device is substantially crystalline, and
wherein an amount of nickel in said mixed oxide ranges from 30% to 70% by weight of said mixed oxide.
2. The method of claim 1 , wherein said amount ranges from about 40% to about 60% by weight of said mixed oxide.
3. The method of claim 1 , wherein said electrochromic layer comprises a metal oxide.
4. The method of claim 3 , wherein said metal oxide is selected from the group consisting of tungsten oxide, vanadium oxide, molybdenum oxide, niobium oxide, titanium oxide, iridium oxide, chromium oxide, copper oxide, and manganese oxide.
5. The method of claim 3 , wherein said metal oxide is doped with one or more metals.
6. The method of claim 1 , comprising depositing said lithium in an amount which provides a maximum transmission through said counter electrode layer.
7. The method of claim 1 , comprising depositing said lithium in an amount in excess of an amount which provides a maximum transmission through said counter electrode layer.
8. The method of claim 7 , wherein said excess amount ranges from about 10% to about 40% above said amount which provides a maximum transmission through said counter electrode layer.
9. The method of claim 1 , comprising heating said electrochromic device to a temperature ranging from about 280° C. to about 500° C.
10. The method of claim 9 , comprising heating said electrochromic device to a temperature ranging from about 355° C. to about 395° C.
11. The method of claim 1 , comprising depositing said counter electrode layer by means of physical vapor deposition.
12. The method of claim 1 , comprising depositing said counter electrode layer by means of intermediate frequency reactive sputtering.
13. The method of claim 1 , comprising depositing said counter electrode layer by means of DC sputtering.
14. The method of claim 1 , comprising depositing said lithium on said counter electrode layer by means of wet chemical methods.
15. The method of claim 1 , comprising depositing said lithium on said counter electrode layer by means of physical vapor deposition.
16. A method of making a counter electrode layer for use in connection with an electrochromic device comprising:
a) depositing a film of mixed tungsten-nickel oxide on a substrate,
b) reducing said mixed tungsten-nickel oxide film by depositing lithium on said film, and
c) heating said counter electrode layer,
wherein said mixed tungsten-nickel oxide in said counter electrode layer is substantially crystalline, wherein an amount of nickel in said mixed oxide ranges from 30% to 70% by weight of said mixed oxide.
17. The method of claim 16 , wherein said amount ranges from about 40% to about 60% by weight of said mixed oxide.
18. The method of claim 16 , comprising depositing said lithium in an amount which provides a maximum transmission through said counter electrode layer.
19. The method of claim 16 , comprising depositing said lithium in an amount in excess of an amount which provides a maximum transmission through said counter electrode layer.
20. The method of claim 19 , wherein said excess amount ranges from about 10% to about 40% above said amount which provides a maximum transmission through said counter electrode layer.
21. The method of claim 16 , comprising depositing said counter electrode layer by means of physical vapor deposition.
22. The method of claim 16 , comprising depositing said counter electrode layer by means of intermediate frequency reactive sputtering.
23. The method of claim 16 , comprising depositing said counter electrode layer by means of DC sputtering.
24. The method of claim 16 , comprising depositing said lithium on said counter electrode layer by means of wet chemical methods.
25. The method of claim 16 , comprising depositing lithium on said counter electrode layer by means of physical vapor deposition.
26. A method for the preparation of an electrochromic device comprising:
a) providing a first conductive layer,
b) depositing one of an electrochromic layer or a counter electrode layer comprising a mixed tungsten-nickel oxide on said first conductive layer, thereby providing a first deposited electrode,
c) depositing an ion-conductor layer on said first deposited electrode,
d) depositing the other of said electrochromic layer or said counter electrode layer on said ion-conductor layer, thereby providing a second deposited electrode,
f) depositing lithium onto said second deposited electrode whereby the mixed tungsten-nickel oxide of the counter electrode is reduced, said lithium being deposited in an amount in excess of an amount which provides a maximum transmission through said counter electrode layer,
e) depositing a second conductive layer on said second deposited electrode, and
g) heating said electrochromic device,
wherein said mixed tungsten-nickel oxide in said electrochromic device is substantially crystalline, wherein an amount of nickel in said mixed oxide ranges from 30% to 70% by weight of said mixed oxide.
27. A method for the preparation of an electrochromic device comprising:
a) providing a first conductive layer,
b) depositing one of an electrochromic layer or a counter electrode layer comprising a mixed tungsten-nickel oxide in crystalline form on said first conductive layer, thereby providing a first deposited electrode,
c) depositing an ion-conductor layer on said first deposited electrode,
d) depositing the other of said electrochromic layer or said counter electrode layer on said ion-conductor layer, thereby providing a second deposited electrode,
e) depositing lithium onto said counter electrode layer whereby said mixed tungsten-nickel oxide is reduced, wherein said lithium is deposited in an amount of from 10% to 40% above an amount which provides a maximum transmission through said counter electrode layer,
f) depositing a second conductive layer on said second deposited electrode, and
g) heat treating said electrochromic device,
wherein an amount of nickel in said mixed oxide ranges from about 30% to about 70% by weight of said mixed oxide.