# US 2018/0023212 A1 · Synthesis, capping and dispersion of nanocrystals

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 2018/0023212 A1
- Document ID: US20180023212A1
- Status: Published application
- Kind: A1
- Application number: 15/701,821
- Filed: 2017-09-12
- Published: 2018-01-25
- Earliest claimed: 2010-04-23
- Assignees: Pixelligent Technologies, LLC
- Applicants: Pixelligent Technologies, LLC
- Inventors: Zehra Serpil GONEN WILLIAMS; Yijun WANG; Robert J. WIACEK; Xia BAI; Linfeng GOU; Selina I. THOMAS; Wei XU; Jun XU; Rakesh PATEL
- Web page: https://patentgrep.com/patent/US20180023212A1

## CPC

- C30B 29/16: Oxides
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C07F 7/1804: {Compounds having Si-O-C linkages (Si-O-acyl linkages C07F7/1896)}
- C07F 7/28: Titanium compounds
- C30B 7/10: by application of pressure, e.g. hydrothermal processes
- C30B 7/14: the crystallising materials being formed by chemical reactions in the solution
- C30B 29/32: Titanates; Germanates; Molybdates; Tungstates
- H01B 1/14: Conductive material dispersed in non-conductive inorganic material
- H01B 1/20: Conductive material dispersed in non-conductive organic material {(organic macromolecular compounds or compositions C08)}
- H01B 1/22: the conductive material comprising metals or alloys
- H10K 85/40: Organosilicon compounds, e.g. TIPS pentacene
- H10K 85/60: Organic compounds having low molecular weight (H10K85/10 - H10K85/50 take precedence)
- H10P 14/265: {using solutions}
- H10P 14/3434: {being oxide semiconductor materials (Group IIB-VIA semiconductor materials H10P14/3424)}
- H10P 14/3461: {Nanoparticles}
- Y10S 977/774: Exhibiting three-dimensional carrier confinement, e.g. quantum dots
- Y10S 977/896: Chemical synthesis, e.g. chemical bonding or breaking
- Y10S 977/932: for electronic or optoelectronic application
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

Preparation of semiconductor nanocrystals and their dispersions in solvents and other media is described. The nanocrystals described herein have small (1-10 nm) particle size with minimal aggregation and can be synthesized with high yield. The capping agents on the as-synthesized nanocrystals as well as nanocrystals which have undergone cap exchange reactions result in the formation of stable suspensions in polar and nonpolar solvents which may then result in the formation of high quality nanocomposite films.

## Claims

### Claim 1

Nanocrystals formed by a solvothermal method, said method comprising
dissolving or mixing at least one precursor of said nanocrystals in at least one solvent to produce a solution,
heating said solution to a temperature in the range of greater than a temperature of 250° C. to a temperature of 350° C. and a pressure in the range of 100-900 psi to form said nanocrystals,
wherein
said nanocrystals are comprised of at least one of hafnium oxide, zirconium oxide, hafnium-zirconium oxide and titanium-zirconium oxide.

### Claim 2 (depends on 1)

The nanocrystals of claim 1 wherein said at least one precursor is selected from the group consisting of at least one of an alkoxide, an acetate, an acetylacetonate, and a halide.

### Claim 3 (depends on 1)

The nanocrystals of claim 1 wherein said pressure is in the range of 100-500 psi.

### Claim 4 (depends on 3)

The nanocrystals of claim 3 wherein said temperature is in the range of 300-350° C.

### Claim 5 (depends on 4)

The nanocrystals of claim 4 wherein said heating comprises heating for 1-2 hours.

### Claim 6 (depends on 1)

The nanocrystals of claim 1 wherein said nanocrystals are capped with at least one agent to increase the solubility or dispersibility of said nanocrystals.

### Claim 7 (depends on 6)

The nanocrystals of claim 6 wherein said at least one agent comprises at least one organosilane, organocarboxylic acid or organoalcohol.

### Claim 8 (depends on 6)

The nanocrystals of claim 6 wherein said at least one agent to cap said nanocrystals is included in the solution.

### Claim 9 (depends on 8)

The nanocrystals of claim 8 wherein said at least one agent to cap said nanocrystals is contacted with said solution prior, during or after said reacting.

### Claim 10 (depends on 1)

The nanocrystals of claim 1 further comprising purifying and/or separating said nanocrystals.

### Claim 11 (depends on 10)

The nanocrystals of claim 10 further comprising capping said purified and/or separated nanocrystals with at least one capping agent to produce at least partially capped nanocrystals.

### Claim 12 (depends on 6)

The nanocrystals of claim 6 further comprising purifying and/or separating said at least partially capped nanocrystals.

### Claim 13 (depends on 10)

The nanocrystals of claim 10 further comprising contacting said purified and/or separated nanocrystals with a solvent.

### Claim 14 (depends on 12)

The nanocrystals of claim 12 further comprising contacting said at least partially capped nanocrystals with a solvent.

### Claim 15 (depends on 10)

The nanocrystals of claim 10 wherein said nanocrystals are dispersed in a further material.

### Claim 16 (depends on 15)

The nanocrystals of claim 15 wherein said further material is a polymer.

### Claim 17 (depends on 1)

A film or coating formed by a method comprising dispersing the nanocrystals of claim 1 in at least one further material to form a dispersion and applying said dispersion to a surface.

### Claim 18 (depends on 2)

A film or coating formed by a method comprising dispersing the nanocrystals of claim 2 in at least one further material to form a dispersion and applying said dispersion to a surface.

### Claim 19 (depends on 6)

A film or coating formed by a method comprising dispersing the nanocrystals of claim 6 in at least one further material to form a dispersion and applying said dispersion to a surface.

### Claim 20 (depends on 17)

The film or coating of claim 17 wherein said applying comprises spin coating, spraying, dipping, screen printing, rolling, painting, printing, ink jet printing, depositing by evaporation and/or vapor deposition.

### Claim 21 (depends on 1)

A nanocomposite formed by a method comprising combining the nanocrystals of claim 1 with at least one further material and forming the nanocomposite.

### Claim 22 (depends on 1)

The nanocrystals of claim 1 wherein said at least one solvent comprises benzyl alcohol, phenol, oleyl alcohol, toluene, butanol, propanol, isopropanol, ethanol, methanol, propylene glycol monomethyl ether (PGME), propylene glycol methyl ether acetate (PGMEA), ethyl lactate (EL), and 2-propoxy-propanol (PnP), acetonitrile, acetone, tetrahydrofuran, cyclic ketones and mixtures thereof.

### Claim 23 (depends on 6)

The nanocrystals of claim 6 wherein said at least one agent comprises at least one of n-propyltrimethoxysilane, n-propyltriethoxysilane, n-octyltrimethoxysilane, n-octyltriethoxysilane, phenyltrimethoxysilane, 2-[methoxy(polyethyleneoxy)propyl]-trimethoxysilane, methoxytri(ethyleneoxy)propyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-(methacryloyloxy)propyl trimethoxysilane, 3-isocyanatopropyltriethoxysilane, 3-isocyanatopropyltrimethoxysilane, and glycidoxypropyltrimethoxysilane, heptanol, hexanol, octanol, benzyl alcohol, phenol, ethanol, propanol, butanol, oleylalcohol, dodecylalcohol, octadecanol and triethylene glycol monomethyl ether, octanoic acid, acetic acid, propionic acid, 2-[2-(2-methoxyethoxy)ethoxy] acetic acid, oleic acid, benzoic acid or a mixture thereof.

### Claim 24 (depends on 15)

The nanocrystals of claim 15 wherein said further material comprises a fluoroplastic, a polyacrylate (Acrylic), a polyamide (PA or Nylon), a polyamide-imide (PAI), a polyketone (PK), a polyester, a polyimide (PI), a polysulfone (PSU), a polyurethane (PU), a spin-on-glass (SOG) polymer, a silicone, or mixtures thereof.

### Claim 25 (depends on 1)

The nanocrystals of claim 1 wherein water is present in said solution at a molar ratio of water to precursor in a range from 1:1 to 4:1.

### Claim 26 (depends on 25)

The nanocrystals of claim 25 wherein said nanocrystals are in the average size range of 1 nm to 5 nm.

### Claim 27 (depends on 13)

The nanocrystals of claim 13 wherein said solvent comprises benzyl alcohol, phenol, oleyl alcohol, toluene, butanol, propanol, isopropanol, ethanol, methanol, propylene glycol monomethyl ether (PGME), propylene glycol methyl ether acetate (PGMEA), ethyl lactate (EL), and 2-propoxy-propanol (PnP), acetonitrile, acetone, tetrahydrofuran, cyclic ketones and mixtures thereof.

### Claim 28 (depends on 14)

The nanocrystals of claim 14 wherein solvent comprises benzyl alcohol, phenol, oleyl alcohol, toluene, butanol, propanol, isopropanol, ethanol, methanol, propylene glycol monomethyl ether (PGME), propylene glycol methyl ether acetate (PGMEA), ethyl lactate (EL), and 2-propoxy-propanol (PnP), acetonitrile, acetone, tetrahydrofuran, cyclic ketones and mixtures thereof.

### Claim 29 (depends on 15)

The nanocrystals of claim 15 wherein said further material comprises poly(acrylonitrile-butadiene-styrene) (ABS), poly(methyl methacrylate) (PMMA), celluloid, cellulose acetate, poly(ethylene-vinyl acetate) (EVA), poly(ethylene vinyl alcohol) (EVOH), polyacrylonitrile (PAN), polyaryletherketone (PAEK), polybutadiene (PBD), polybutylene (PB), polybutylene terephthalate (PBT), polycaprolactone (PCL), polychlorotrifluoroethylene (PCTFE), polyethylene terephthalate (PET), polycyclohexylene dimethylene terephthalate (PCT), polycarbonate (PC), polyhydroxyalkanoates (PHAs), polyethylene (PE), polyetheretherketone (PEEK), polyetherketoneketone (PEKK), polyetherimide (PEI), polyethersulfone (PES), polyethylenechlorinates (PEC) , polylactic acid (PLA), polymethylpentene (PMP), polyphenylene oxide (PPO), polyphenylene sulfide (PPS), polyphthalamide (PPA), polypropylene (PP), polystyrene (PS), polytrimethylene terephthalate (PTT), polyvinyl acetate (PVA), polyvinyl chloride (PVC), polyvinylidene chloride (PVDC), poly(styrene-acrylonitrile) (SAN), a siloxane-spin-on polymer, polydimethylsiloxane (PDMS) or polymethylphenylsiloxane, or mixtures thereof.