# US 10,121,952 B2 · Materials and methods for the preparation of nanocomposites

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- Number: US 10,121,952 B2
- Document ID: US10121952B2
- Status: Granted
- Kind: B2
- Application number: 15/133,494
- Filed: 2016-04-20
- Published: 2016-10-20
- Granted: 2018-11-06
- Earliest claimed: 2009-04-23
- Assignees: The University of Chicago
- Applicants: The University of Chicago
- Inventors: Dmitri V. Talapin; Maksym V. Kovalenko; Jong-Soo Lee; Chengyang Jiang
- Web page: https://patentgrep.com/patent/US10121952B2

## CPC

- H10N 10/852: comprising tellurium, selenium or sulfur
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 19/002: {Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions}
- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- C09D 1/00: Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D 5/22: Luminous paints {(luminescent compositions C09K11/00)}
- C09D 5/24: Electrically-conducting paints {(conductive materials H01B1/00)}
- C09K 11/025: {non-luminescent particle coatings or suspension media}
- C09K 11/562: {Chalcogenides}
- C09K 11/565: {with zinc cadmium}
- C09K 11/883: {with zinc or cadmium}
- C30B 7/00: Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions (from molten solvents C30B9/00; by normal or gradient freezing C30B11/00; under a protective fluid C30B27/00)
- C30B 29/40: AIIIBV compounds {wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi}
- C30B 29/46: Sulfur-, selenium- or tellurium-containing compounds
- C30B 29/60: characterised by shape
- H01B 1/06: mainly consisting of other non-metallic substances
- H01B 1/10: sulfides
- C01P 2002/52: containing elements as dopants
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/84: by UV- or VIS- data
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/16: Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
- H10N: ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- 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})
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Disclosed herein is an isolable colloidal particle comprising a nanoparticle and an inorganic capping agent bound to the surface of the nanoparticle, a solution of the same, a method for making the same from a biphasic solvent mixture, and the formation of structures and solids from the isolable colloidal particle. The process can yield photovoltaic cells, piezoelectric crystals, thermoelectric layers, optoelectronic layers, light emitting diodes, ferroelectric layers, thin film transistors, floating gate memory devices, imaging devices, phase change layers, and sensor devices.

## Claims

### Claim 1

A solution comprising a colloidal particle and a solvent, wherein the colloidal particle comprises an inorganic capping agent bound to a surface of a nanoparticle; wherein the inorganic capping agent comprises a Zintl ion and is substantially free of an organic capping agent, and the solution is substantially free of an organic capping agent.

### Claim 2 (depends on 1)

The solution of claim 1, wherein the solvent is selected from a group consisting of water, dimethylsulfoxide, formamide, methylformamide, ethanolamine, dimethylformamide, benzonitrile, 1,3-butanediol, butanol, dimethylacetamide, dioxane, methoxyethanol, methylpyrrolidinone, pyridine, ethyleneglycol, glycerol, methanol, ethanol, trimethylamine, dimethylamine, methylamine, ammonia, triethylamine, tetramethylethylenediamine, trimethylethylenediamine, dimethylethylenediamine, ethylenediamine, acetonitrile, and a mixture thereof.

### Claim 3 (depends on 1)

The solution of claim 1, wherein the solvent is substantially free of hydrazine.

### Claim 4 (depends on 1)

The solution of claim 1, wherein the inorganic capping agent is selected from a group consisting of a polyatomic anion, a soluble metal chalcogenide, a soluble polyatomic metal chalcogenide anion, and a mixture thereof.

### Claim 5 (depends on 1)

The solution of claim 1, wherein the inorganic capping agent further comprises an ion selected from the group consisting of As33−, As42−, As53−, As73−, As113−, AsS33−, As2Se63−, As2Te63−, As10Te32−, Au2Te42−, Au3Te43−, Bi33−, Bi42−, Bi53−, Bi73−, GaTe2−, Ge92−, Ge94−, Ge2S64−, HgSe22−, Hg3Se42−, In2Se42−, In2Te42−, Ni5Sb174−, Pb52−, Pb74−, Pb94−, Pb2Sb22−, Sb33−, Sb42−, Sb73−, SbSe43−, SbSe45−, SbTe45−, Sb2Se3, Sb2Te54−, Sb2Te74−, Sb4Te44−, Sb9Te63−, Se22−, Se32−, Se42−, Se5,62−, Se62−, Sn42−, Sn52−, Sn93−, Sn94−, SnS44−, SnSe44−, SnTe44−, SnS4Mn25−, Sn2S64−, Sn2Se64−, Sn2Te64−, Sn2Bi22−, Sn8Sb3−, Te22−, Te32−, Te42−, Tl2Te22−, TlSn83−, TlSn85−, TlSn93−, TlTe22−, and a mixture thereof.

### Claim 6 (depends on 1)

The solution of claim 1, wherein the inorganic capping agent further comprises a metal selected from the group consisting of a transition metal, a lanthanide, an actinide, a main group metal, a metalloid, and a mixture thereof.

### Claim 7 (depends on 1)

The solution of claim 1, wherein the inorganic capping agent further comprises a soluble metal chalcogenide selected from the group consisting of molecular compounds derived from CuInSe2, CuInxGa1-xSe2, Ga2Se3, In2Se3, In2Te3, Sb2S3, Sb2Se3, Sb2Te3, ZnTe, and a mixture thereof.

### Claim 8 (depends on 1)

The solution of claim 1, wherein the nanoparticle is selected from the group consisting of a nanocrystal, a nanorod, a nanowire, and a mixture thereof.

### Claim 9 (depends on 1)

The solution of claim 1, wherein the nanoparticle is selected from a group consisting of AlN, AlP, AlAs, Ag, Au, Bi, Bi2S3, Bi2Se3, Bi2Te3, CdS, CdSe, CdTe, Co, CoPt, CoPt3, Cu, Cu2S, Cu2Se, CuInSe2, CuIn(1-x)Gax(S,Se)2, Cu2ZnSn(S,Se)4, Fe, FeO, Fe2O3, Fe3O4, FePt, GaN, GaP, GaAs, GaSb, GaSe, Ge, HgS, HgSe, HgTe, InN, InP, InSb, InAs, Ni, PbS, PbSe, PbTe, Pd, Pt, Ru, Rh, Si, Sn, ZnS, ZnSe, ZnTe, Au/PbS, Au/PbSe, Au/PbTe, Ag/PbS, Ag/PbSe, Ag/PbTe, Pt/PbS, Pt/PbSe, Pt/PbTe, Au/CdS, Au/CdSe, Au/CdTe, Ag/CdS, Ag/CdSe, Ag/CdTe, Pt/CdS, Pt/CdSe, Pt/CdTe, Au/FeO, Au/Fe2O3, Au/Fe3O4, Pt/FeO, Pt/Fe2O3, Pt/Fe3O4, FePt/PbS, FePt/PbSe, FePt/PbTe, FePt/CdS, FePt/CdSe, FePt/CdTe, CdSe/CdS, CdSe/ZnS, InP/CdSe, InP/ZnS, InP/ZnSe, InAs/CdSe, InAs/ZnSe, and a mixture thereof.

### Claim 10

A method of making a colloidal particle comprising
admixing a solution of an inorganic capping agent in a first solvent and a solution of a nanoparticle in a second solvent, wherein the second solvent is appreciably immiscible in the first solvent,
wherein the colloidal particle comprises the inorganic capping agent bound to a surface of the nanoparticle; and the inorganic capping agent comprises a Zintl ion and is substantially free of an organic capping agent.

### Claim 11 (depends on 10)

The method of claim 10, wherein the first solvent and the second solvent are substantially free of hydrazine.

### Claim 12 (depends on 10)

The method of claim 10 further comprising isolating the colloidal particle from the second solvent.