# US 10,865,136 B2 · Transparent and insulating materials having evacuated capsules

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- Number: US 10,865,136 B2
- Document ID: US10865136B2
- Status: Granted
- Kind: B2
- Application number: 15/656,378
- Filed: 2017-07-21
- Published: 2018-01-25
- Granted: 2020-12-15
- Earliest claimed: 2016-07-22
- Assignees: Alliance for Sustainable Energy, LLC
- Applicants: Alliance for Sustainable Energy, LLC
- Inventors: Lin Jay Simpson; Chaiwat Engtrakul
- Web page: https://patentgrep.com/patent/US10865136B2

## CPC

- C03C 11/002: {Hollow glass particles}
- C03B 19/107: {Forming hollow beads (chemical aspects C03C11/002)}
- C01P 2004/32: Spheres
- C01P 2004/34: hollow
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2004/84: one phase coated with the other
- C03C 17/2453: {Coating containing SnO2}
- C03C 2217/211: SnO2
- C03C 2217/216: ZnO
- C03C 2218/15: from the vapour phase
- E06B 7/28: Other arrangements on doors or windows, e.g. door-plates, windows adapted to carry plants, hooks for window cleaners {(edge protecting devices for door leaves E06B3/88; special glazing; emergency glazing; double glazing E06B3/66)}
- Y10T 428/249974: Metal- or silicon-containing element
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03B: MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- E06B: FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES (shades or blinds for greenhouses A01G9/22; curtains A47H; lids for car boots or bonnets B62D25/10; skylights E04B7/18; sunshades, awnings E04F10/00)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Transparent and insulating materials having evacuated capsules are provided. According to an aspect of the invention, a method includes forming evacuated capsules within a solution, and dispersing and suspending the evacuated capsules within the solution such that a packing density of the evacuated capsules within the solution is greater than 30%, and a visible light transmission of the solution including the evacuated capsules is greater than 75%. According to another aspect of the invention, a layer includes a plurality of evacuated capsules distributed within a dried sol-gel. A thermal conductivity of the layer is between 0.02 W/m-K and 0.001 W/m-K, and the layer has a visible light transmission of greater than 30%.

## Claims

### Claim 1

A method comprising:
forming a composition consisting essentially of a plurality of hollow spherical silica shells within a solution;
dispersing and suspending the hollow spherical silica shells within the solution such that a packing density of the hollow spherical silica shells within the solution is greater than 30%, and a visible light transmission of the solution is greater than 75%;
processing the solution with a sol-gel method; and
drying the processed solution to form a secondary shell of silica, wherein:
the hollow spherical silica shells are integrated by the secondary shell to form a layer consisting essentially of the hollow spherical silica shells and the secondary shell,
at least a portion of the hollow spherical silica shells have an internal volume at a pressure of less than 1 microtorr,
each hollow spherical silica shell has a lateral dimension between 50 nm and 300 nm,
the layer has a thickness between 3.175 mm and 6.35 mm,
the layer has a thermal conductivity between 0.001 W/m-K and 0.02 W/m-K, and
the layer has a visible light transmission of greater than 30% and less than 70%.

### Claim 2 (depends on 1)

The method of claim 1, wherein the dispersing and suspending comprises:
adjusting a pH of the solution to a value between 9 and 14, and
adding a polycation or a polyanion to the solution.

### Claim 3 (depends on 1)

The method of claim 1, wherein the packing density is greater than 70%.

### Claim 4 (depends on 1)

The method of claim 1, further comprising adding a strengthening agent to the solution before processing the solution.

### Claim 5 (depends on 4)

The method of claim 4, wherein the strengthening agent comprises at least one of poly(vinyl alcohol) or boric acid.

### Claim 6 (depends on 1)

The method of claim 1, wherein the forming comprises:
creating a template using dodecanethiol and cetyl-trimethylammonium bromide;
coating the template with a silica-gel; and
heating the template to a temperature of at least 250° C. in vacuum, resulting in the hollow spherical silica shells.

### Claim 7 (depends on 6)

The method of claim 6, wherein the forming further comprises performing atomic layer deposition, physical vapor deposition, chemical vapor deposition, or solution phase deposition to deposit a low-emissivity coating on the hollow silica shells.

### Claim 8 (depends on 1)

The method of claim 1, wherein each of the hollow spherical silica shells has a lateral dimension between 50 nm and 300 nm.

### Claim 9 (depends on 8)

The method of claim 8, wherein the lateral dimension is between 80 nm and 100 nm.

### Claim 10

A composition comprising:
a layer consisting essentially of:
a plurality of hollow spherical primary silica shells; and
a secondary shell of silica integrated with the hollow spherical primary silica shells to form the layer, wherein:
each hollow spherical primary silica shell has a lateral dimension between 50 nm and 300 nm,
at least a portion of the hollow spherical primary silica shells have an internal volume at a pressure of less than 1 microtorr,
the layer has a thickness between 3.175 mm and 6.35 mm,
the layer has a thermal conductivity between 0.001 W/m-K and 0.02 W/m-K; and
the layer has a visible light transmission of greater than 30% and less than 70%.

### Claim 11 (depends on 10)

The composition of claim 10, wherein the lateral dimension is between 80 nm and 100 nm.

### Claim 12 (depends on 10)

The composition of claim 10, wherein at least a portion of the hollow spherical primary silica shells are concave.

### Claim 13 (depends on 10)

The composition of claim 10, wherein at least a portion of the hollow spherical primary silica shells has thickness between 3 nanometers and 20 nanometers.

### Claim 14 (depends on 10)

The composition of claim 10, wherein the secondary shell has a shape that is substantially cylindrical.

### Claim 15 (depends on 10)

The composition of claim 10, further comprising boric acid, wherein the boric acid strengthens the layer.

### Claim 16 (depends on 10)

The composition of claim 10, wherein at least a portion of the hollow spherical primary silica shells and the secondary shell form a pore.

### Claim 17 (depends on 10)

The composition of claim 10, wherein the secondary shell is produced by a sol-gel method.