Improved process of ultrasonic spray pyrolysis deposition of one or more electrochromic and/or electrolytic films on a substrate

Patent metadata

Field	Value
Publication number	US-2017363928-A1
Application number	US-201515535433-A
Country	US
Kind code	A1
Filing date	Dec 11, 2015
Priority date	Jan 14, 2015
Publication date	Dec 21, 2017
Grant date	—

Abstract

A process of making an electrochromic or an electrolytic film by Ultrasonic Spray Pyrolysis (USP) deposition on a substrate comprising:
mixing a surfactant to an aqueous precursor solution comprising an electrochromic component or an electrolytic component to provide a spray solution; introducing the spray solution into an ultrasonic spray deposition nozzle at a constant flow rate between 0.1 mL/min and 2 mL/min and applying an ultrasonic frequency between 80 and 120 kHz to generate atomized droplets of the precursor solution; entraining the atomized droplets with a controlled jet of air as gas carrier at a pressure between 0.50 to 2.0 psi, onto a pre-heated substrate at a temperature of 200 to 450° C.; thermally converting the atomized droplets when depositing onto the pre-heated substrate to generate an electrochromic or an electrolytic film.

First claim

1 . A Process of making an electrochromic or an electrolytic film by Ultrasonic Spray Pyrolysis (USP)
mixing a surfactant with an aqueous precursor solution comprising an electrochromic component or an electrolytic component to provide a spray solution; introducing the spray solution into an ultrasonic spray deposition nozzle at a constant flow rate between 0.1 mL/min and 2 mL/min and applying an ultrasonic frequency between 80 and 120 kHz to generate atomized droplets of the precursor solution; entraining the atomized droplets in a controlled jet of air as gas carrier at a pressure between 0.50 to 2.0 psi, onto a pre-heated substrate at a temperature of 200 to 450° C.; thermally converting the atomized droplets when depositing onto the pre-heated substrate to generate an electrochromic or an electrolytic film.

2 . The process according to claim 1 wherein the constant flow rate is between 0.1 and 0.4 mL/min with a spray nozzle.

3 . The process according to claim 1 wherein the film deposition onto the preheated substrate is designed according to a three-dimensional pattern by the ultrasonic spray deposition nozzle.

4 . The process according to claim 1 wherein the three-dimensional pattern follows a S shape are move in the X-Y plane.

5 . The process according to claim 1 wherein both steps of entraining the atomized droplets and their thermal conversion onto the pre-heated substrate are repeated between 2 to 16 times, in order to generate an homogenous electrochromic or electrolytic layer.

6 . The process according to claim 1 wherein the electrochromic film comprises a metal oxide selected from tungsten oxide, molybdenum oxide, niobium oxide, titanium oxide, copper oxide, chromium oxide, manganese oxide, vanadium oxide, tantalum oxide, iron oxide, cobalt oxide, nickel oxide, ruthenium oxide, rhodium oxide, palladium oxide, osmium oxide, iridium oxide, platinum oxide or a combination thereof.

7 . The process according to claim 6 wherein the electrochromic film further comprises a dopant element selected from hydrogen ion, deuterium ion, lithium ion, sodium ion, potassium ion, rubidium ion, caesium ion, molybdenum ion, titanium ion, vanadium ion, calcium ion, barium ion, magnesium ion, strontium ion, tungsten ion, nickel ion and combination thereof.

8 . The process of making an electrochromic film according claim 1 wherein the aqueous precursor solution comprises an organic or inorganic salt or complex, selected from nitrate, chloride, acetate, acetylacetonate, citrate, sulphate, peroxometalate, containing metal selected from tungsten, molybdenum, niobium, titanium, copper, chromium, manganese, vanadium, tantalum, iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium, platinum or a combination thereof.

9 . The process according to claim 1 wherein the electrochromic layer is lithium doped nickel oxide or tungsten trioxide

10 . The process of making an electrolytic film according to claim 1 wherein the aqueous precursor composition comprises an electrolytic component selected from tetraethyl orthosilicate, lithium nitrate, aluminium nitrate, zinc nitrate, nitric acid, boric acid, phosphoric acid, lithium sulfate, or a combination thereof.

11 . The process according to claim 1 wherein the electrolytic film is selected from lithium aluminosilicate (LAS), lithium borosilicate (LBS) or lithium phosphosilicate (LPS).

12 . The process according to claim 1 wherein the surfactant is polyethylene glycol.

13 . The process according to claim 1 wherein the weight ratio of the electrochromic component to polyethylene glycol in the aqueous precursor solution is between 10:1 and 1:10.

14 . The process according to claim 1 wherein the ultrasonic frequency is 120 kHz.

15 . The process according to claim 1 wherein the carrier air gas pressure is 0.90 psi.

16 . The process according to claim 1 wherein the substrate is pre-heated at a temperature of 350° C.

17 . The process according to claim 1 wherein the substrate is fluorine doped tin oxide coated glass.

18 . A multilayer stacking construction on a substrate comprising at least one electrochromic layer and at least one electrolytic layer generated by the process according to claim 1 .

19 . The multilayer stacking construction on a substrate according to claim 18 further comprising an additional electrochromic layer acting as a counter electrode.

20 . The multilayer stacking construction according to claim 18 comprising:
a fluorine doped tin oxide coated glass substrate;
a first layer generated on the substrate and selected from lithium doped nickel oxide or tungsten oxide;
a second layer of lithium aluminosilicate generated on the first layer;
a third layer generated on the second layer and selected from tungsten oxide or lithium doped nickel oxide; as counter electrode and
a fourth conductive top layer.

Assignees

• Univ Liege
• Inisma

Inventors

• Cloots Rudi
• Henrist Catherine
• Denayer Jessica
• Maho Anthony
• Cambier Francis
• Lardot Véronique
• Bister Geoffroy
• Aubry Philippe

Classifications

• G02F1/1525

  characterised by a particular ion transporting layer, e.g. electrolyte · CPC title

• G02F1/155

  Electrodes · CPC title

• G02F1/1347

  Arrangement of liquid crystal layers or cells in which the final condition of one light beam is achieved by the addition of the effects of two or more layers or cells · CPC title

• C23C18/1291 Primary

  by heating of the substrate · CPC title

• C03C17/3417

  all coatings being oxide coatings · CPC title