# US 10,118,833 B2 · Dimensionally focused nanoparticle synthesis methodology

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- Number: US 10,118,833 B2
- Document ID: US10118833B2
- Status: Granted
- Kind: B2
- Application number: 15/516,131
- Filed: 2015-10-02
- Published: 2017-09-07
- Granted: 2018-11-06
- Earliest claimed: 2014-10-02
- Assignees: Cornell University
- Applicants: Cornell University
- Inventors: Richard D. Robinson; Tobias Hanrath; Curtis Williamson; Douglas Nevers
- Web page: https://patentgrep.com/patent/US10118833B2

## CPC

- C01G 3/12: Sulfides
- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- C01G 11/02: Sulfides
- C01G 21/21: Sulfides
- B82Y 20/00: Nanooptics, e.g. quantum optics or photonic crystals
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/88: by thermal analysis data, e.g. TGA, DTA, DSC
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/52: highly monodisperse size distribution
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/22: Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
- Y10S 977/773: Nanoparticle, i.e. structure having three dimensions of 100 nm or less
- Y10S 977/824: Group II-VI nonoxide compounds, e.g. CdxMnyTe
- Y10S 977/825: Heterojunction formed between semiconductor materials that differ in that they belong to different periodic table groups
- Y10S 977/896: Chemical synthesis, e.g. chemical bonding or breaking
- Y10S 977/95: Electromagnetic energy
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

A methodology for synthesizing a nanoparticle batch, such as but not limited to a metal chalcogenide nanoparticle batch and further such as but not limited to a metal sulfide nanoparticle batch is predicated upon an expectation and observation that at elevated concentrations of at least one reactant material within a heat-up nanoparticle batch synthesis method, the resulting nucleated batch comprises nanoparticles that may be dimensionally focused to provide a substantially monodisperse nanoparticle batch. The embodied methodology is also applicable to a continuous reactor. The embodied methodology also considers viscosity as a dimensionally focusing result effective variable.

## Claims

### Claim 1

A nanoparticle synthesis method comprising:
mixing together at a first temperature at least:
a first reactant material at a first concentration; and
a second reactant material at a second concentration, to provide a reactant composition,
wherein the first reactant material is present at 50% or greater of the saturation limit of the first reactant material and/or the second reactant material is present at 50% or greater of the saturation limit of the second reactant material;
thermally adjusting the reactant composition to a second temperature to provide a nucleated virgin nanoparticle population within a nucleated reactant composition; and
thermally soaking the nucleated virgin nanoparticle population in the nucleated reactant composition to provide a substantially monodisperse nanoparticle population.

### Claim 2 (depends on 1)

The method of claim 1 wherein the nanoparticle synthesis method comprises a batch nanoparticle synthesis method.

### Claim 3 (depends on 1)

The method of claim 1 wherein the nanoparticle synthesis method comprises a continuous nanoparticle synthesis method.

### Claim 4 (depends on 1)

The method of claim 1 wherein the substantially monodisperse nanoparticle population comprises a material selected from the group consisting of metal carbide materials, metal nitride materials and metal oxide materials.

### Claim 5 (depends on 1)

The method of claim 1 wherein the reactant composition also comprises a diluent.

### Claim 6 (depends on 1)

The method of claim 1 wherein the thermally soaking of the nucleated virgin nanoparticle population is undertaken at a thermal soak temperature less than the second temperature.

### Claim 7 (depends on 1)

The method of claim 1 wherein the thermally soaking of the nucleated virgin nanoparticle population is undertaken at a thermal soak temperature equal to the second temperature.

### Claim 8 (depends on 1)

The method of claim 1 wherein the thermally soaking of the nucleated virgin nanoparticle population is undertaken at a thermal soak temperature greater than the second temperature.

### Claim 9 (depends on 1)

The method of claim 1 wherein the first temperature is less than the second temperature.

### Claim 10 (depends on 1)

The method of claim 1 wherein the first temperature is equal to the second temperature.

### Claim 11 (depends on 1)

The method of claim 1 wherein the first temperature is greater than the second temperature.

### Claim 12 (depends on 1)

The method of claim 1 wherein the second concentration is different than the first concentration.

### Claim 13 (depends on 1)

The method of claim 1 wherein at least one of the first concentration and the second concentration is at least about 70 percent of a saturation limit of the at least one of the first reactant material and the second reactant material within the reactant composition.

### Claim 14 (depends on 1)

The method of claim 1 wherein:
one of the first concentration and the second concentration is at least about 1000 mM; and
the other of the first concentration and the second concentration is at least about 100 mM.

### Claim 15 (depends on 1)

The method of claim 1 wherein the first temperature is at or above the melting point of at least one of the reactant materials.

### Claim 16 (depends on 1)

The method of claim 1 wherein the first temperature is below the nanoparticle nucleation temperature.

### Claim 17 (depends on 1)

The method of claim 1 wherein the second temperature is at or above the nucleation temperature.

### Claim 18 (depends on 1)

The method of claim 1 wherein the reactant composition at the first temperature has a first viscosity of 0.01 to 1 poise, and
wherein the reactant composition at the second temperature has a second viscosity of 1 to 100 poise.

### Claim 19 (depends on 1)

The nanoparticle synthesis method of claim 1 wherein prior to the mixing together of the first reactant material and the second reactant material the first reactant material and/or second reactant material are present as solutions.

### Claim 20

A metal chalcogenide nanoparticle synthesis method comprising:
mixing together at a first temperature at least:
a first metal reactant material at a first concentration; and
a second chalcogen reactant material at a second concentration, to provide a metal-chalcogen reactant composition,
wherein the first metal reactant material is present at 50% or greater of the saturation limit of the first metal reactant material and/or the second chalcogen reactant material is present at 50% or greater of the saturation limit of the second chalcogen reactant material;
thermally adjusting the metal-chalcogen reactant composition to a second temperature to provide a nucleated virgin metal chalcogenide nanoparticle population within a nucleated metal-chalcogenide reactant composition; and
thermally soaking the nucleated virgin metal chalcogenide nanoparticle population in the nucleated metal-chalcogen reactant composition to provide a substantially monodisperse metal chalcogenide nanoparticle population.

### Claim 21 (depends on 20)

The method of claim 20 wherein the metal-chalcogen reactant composition also comprises a diluent.

### Claim 22 (depends on 20)

The method of claim 20 wherein the metal chalcogenide nanoparticle population comprises:
a least one metal reactant material selected from the group consisting of copper, lead, cadmium, indium and zinc; and
a least one chalcogen reactant material selected from the group consisting of selenium and tellurium.

### Claim 23 (depends on 20)

The method of claim 20 wherein:
one of the first concentration and the second concentration is at least about 1000 mM; and
the other of the first concentration and the second concentration is at least about 100 mM.

### Claim 24 (depends on 20)

The method of claim 20 wherein the reactant composition at the first temperature has a first viscosity of 0.01 to 1 poise, and
wherein the reactant composition at the second temperature has a second viscosity of 1 to 100 poise.

### Claim 25

A metal sulfide nanoparticle synthesis method comprising:
mixing together at a first temperature at least:
a first metal reactant material at a first concentration; and
a second sulfur reactant material at a second concentration, to provide a metal-sulfur reactant composition,
wherein the first metal reactant material is present at 50% or greater of the saturation limit of the first metal reactant material and/or the second sulfur reactant material is present at 50% or greater of the saturation limit of the second sulfur reactant material;
thermally adjusting the metal-sulfur reactant composition to a second temperature to provide a nucleated virgin metal sulfide nanoparticle population within a nucleated metal-sulfur reactant composition; and
thermally soaking the nucleated virgin metal sulfide nanoparticle population in the nucleated metal-sulfur composition to provide a substantially monodisperse metal sulfide nanoparticle population.

### Claim 26 (depends on 25)

The method of claim 25 wherein the metal-sulfur reactant composition also comprises a diluent.

### Claim 27 (depends on 25)

The method of claim 25 wherein the metal sulfide nanoparticle population comprises:
at least one metal reactant material selected from the group consisting of copper, lead, cadmium, indium and zinc; and
a sulfur reactant material comprising ammonium sulfide.

### Claim 28 (depends on 25)

The method of claim 25 wherein:
one of the first concentration and the second concentration is at least about 1000 mM; and
the other of the first concentration and the second concentration is at least about 100 mM.

### Claim 29 (depends on 25)

The method of claim 25 wherein the reactant composition at the first temperature has a first viscosity of 0.01 to 1 poise, and
wherein the reactant composition at the second temperature has a second viscosity of 1 to 100 poise.