# US 10,767,143 B2 · Particle removal from electrochromic films using non-aqueous fluids

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- Number: US 10,767,143 B2
- Document ID: US10767143B2
- Status: Granted
- Kind: B2
- Application number: 14/198,824
- Filed: 2014-03-06
- Published: 2015-09-10
- Granted: 2020-09-08
- Earliest claimed: 2014-03-06
- Assignees: Sage Electrochromics, Inc.
- Applicants: SAGE Electrochromics, Inc.
- Inventors: Harvey Kalweit; Satya Ajjarapu; Jean-Christophe Giron
- Web page: https://patentgrep.com/patent/US10767143B2

## CPC

- H10K 71/60: Forming conductive regions or layers, e.g. electrodes
- C11D 1/006: {Surface-active compounds containing fluorine and phosphorus}
- C11D 1/12: Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D 1/14: derived from aliphatic hydrocarbons or mono-alcohols
- C11D 1/29: Sulfates of polyoxyalkylene ethers
- G02F 1/15: based on an electrochromic effect
- H10K 77/10: Substrates, e.g. flexible substrates
- C11D 2111/18: Glass; Plastics
- C11D 2111/22: Electronic devices, e.g. PCBs or semiconductors
- Y02E 10/549: Organic PV cells
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES
- C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- G02F: OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Several of the films that comprise various energy producing or control devices, for example, electrochromic devices, lithium batteries, and photovoltaic cells, are sensitive to moisture in some way. They may be especially vulnerable to moisture at particular stages during their fabrication. It may also be highly desirable during fabrication to be able to wash particulates from the surface. The particulates may be generated some aspect of the fabrication process, or they may arise from the environment in which the fabrication takes place. This invention shows ways to remove said particles from the surface without incurring the damage associated with typical washing processes, resulting in higher manufacturing yields and better device performance.

## Claims

### Claim 1

A method of forming an electrochromic device comprising:
depositing a first conductive layer over a substrate;
depositing a first electrode layer over the first conductive layer, wherein the first electrode layer is one of an electrochromic layer or a counter electrode layer;
depositing an ion conductor layer over the first electrode layer, wherein a film stack includes the first conductive layer, the first electrode layer, and the ion conductor layer;
exposing the ion conductor layer to a non-aqueous liquid to remove particulate material having a size between about 0.1 μm and about 1000 μm, wherein the non-aqueous liquid is selected from the group consisting of a hydrofluorocarbon, a fluorocarbon, a polymeric fluorinated solvent, and a fluoride surfactant;
depositing a second electrode layer over the film stack after exposing the ion conductor layer to the non-aqueous liquid, wherein the second electrode layer is the other of the electrochromic layer or the counter electrode layer; and
depositing a second conductive layer on the second electrode layer, wherein the electrochromic device has a defect density of less than 1 defect/m2, and wherein the electrochromic device is configured for use in a window.

### Claim 2 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid is delivered to a surface of the substrate in the form of a stream or jet of sufficient velocity to dislodge at least some of the particulate material from the surface on which it impinges.

### Claim 3 (depends on 1)

The method of claim 1, wherein the temperature of the non-aqueous liquid and of a surface of the substrate are independently controlled.

### Claim 4 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid comprises less than about 0.1% of water.

### Claim 5 (depends on 1)

The method of claim 1, wherein the first electrode layer is the electrochromic layer, and the second electrode layer is the counter electrode layer.

### Claim 6 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid is non-polar.

### Claim 7 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid is polar.

### Claim 8 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid comprises a fluorocarbon, hydrofluorocarbon, or a polymeric fluorinated solvent.

### Claim 9 (depends on 1)

The method according to claim 1, wherein an energy is applied, the energy selected from the group consisting of ultrasonic agitation of the liquid, bubble jet agitation, and thermal heating of the liquid.

### Claim 10 (depends on 1)

The method of claim 1, further comprising lithiating the electrochromic layer, the ion conductor layer, or the counter electrode layer.

### Claim 11 (depends on 1)

The method of claim 1, further comprising patterning the film stack before exposing the film stack to the non-aqueous liquid.

### Claim 12 (depends on 1)

The method of claim 1, wherein the defect density is less than 1 short circuit/m2.

### Claim 13 (depends on 1)

The method of claim 1, wherein the defect density is less than 1 visible defect/m2.

### Claim 14 (depends on 1)

The method of claim 1, wherein the non-aqueous liquid has a fluoride concentration, by weight, based on active content, ranging between about 1 ppm and about 50,000 ppm.

### Claim 15 (depends on 1)

The method of claim 1, wherein the fluoride surfactant includes:
Rf—SO3−M+, where the Rf is a C1 to C12 perfluoroalkyl group, and M+is a cation, a H30 atom or an ammonia group; or
Rf—SO2N−—R1M+, where the Rf is a C1 to C12 perfluoroalkyl group; R1 is H, an alkyl group, a hydroxyalkyl group, an alkylamine oxide group, an alkylcarboxylate group or aminoalkyl group; and M+is a cation, a H+atom or an ammonia group.

### Claim 16

A method of forming an electrochromic device comprising:
depositing a first conductive layer over a substrate;
depositing a first electrode layer over the first conductive layer, wherein the first electrode layer is one of an electrochromic layer or a counter electrode layer;
depositing an ion conductor layer over the first electrode layer, wherein a film stack includes the first conductive layer, the first electrode layer, and the ion conductor layer;
exposing the ion conductor layer to a non-aqueous liquid to remove particulate material having a size between about 0.1 μm and about 1000 μm, wherein the non-aqueous liquid is selected from the group consisting of a hydrofluorocarbon, a fluorocarbon, a polymeric fluorinated solvent, and a fluoride surfactant;
depositing a second electrode layer over the ion conductor layer after exposing the film stack to the non-aqueous liquid, wherein the second electrode layer is the other of the electrochromic layer or the counter electrode layer; and
depositing a second conductive layer on the second electrode layer, wherein the electrochromic device has a defect density of less than 1 defect/m2, wherein the electrochromic device is configured to be part of an insulated glass unit, and wherein the electrochromic device is configured for use in a window.