# US 9,517,937 B2 · Method to synthesize metal chalcogenide monolayer nanomaterials

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- Number: US 9,517,937 B2
- Document ID: US9517937B2
- Status: Granted
- Kind: B2
- Application number: 14/660,702
- Filed: 2015-03-17
- Published: 2015-09-24
- Granted: 2016-12-13
- Earliest claimed: 2014-03-20
- Assignees: Sandia Corporation
- Applicants: Sandia Corporation
- Inventors: Bernadette A. Hernandez-Sanchez; Timothy J. Boyle
- Web page: https://patentgrep.com/patent/US9517937B2

## CPC

- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- C01B 17/20: Methods for preparing sulfides or polysulfides, in general (ammonium sulfides or polysulfides C01C; sulfides or polysulfides of metals, other than alkali metals, magnesium, calcium, strontium and barium, see the relevant groups of subclasses C01F or C01G, according to the metal)
- C01B 17/42: Sulfides or polysulfides of magnesium, calcium, strontium, or barium
- C01F 11/00: Compounds of calcium, strontium, or barium (C01F7/00 takes precedence)
- C01G 39/06: Sulfides
- C01G 41/00: Compounds of tungsten
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/77: by unit-cell parameters, atom positions or structure diagrams
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2002/88: by thermal analysis data, e.g. TGA, DTA, DSC
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; 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 cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- 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)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Metal chalcogenide monolayer nanomaterials can be synthesized from metal alkoxide precursors by solution precipitation or solvothermal processing. The synthesis routes are more scalable, less complex and easier to implement than other synthesis routes.

## Claims

### Claim 1

A method to synthesize a metal chalcogenide nanomaterial according to the reaction:
wherein M is an alkaline earth metal or a transition metal and X is the oxidation state of the metal.

### Claim 2 (depends on 1)

The method of claim 1, wherein the transition metal comprises tungsten or molybdenum.

### Claim 3 (depends on 2)

The method of claim 2, wherein M(OR)x comprises W(OEt)5.

### Claim 4 (depends on 1)

The method of claim 1, wherein the alkaline earth metal comprises calcium, strontium, or barium.

### Claim 5 (depends on 4)

The method of claim 4, wherein M(OR)x comprises Ca(OAr)2.

### Claim 6 (depends on 4)

The method of claim 4, wherein M(OR)x comprises AE(ONep)2 and AE comprises strontium or barium and wherein ONep is neopentoxide.

### Claim 7

A method to synthesize a metal chalcogenide nanomaterial according to the reaction:
wherein M is an alkaline earth metal or a transition metal and TOP=E is trioctylphoshine selenide or telluride and X is the oxidation state of the metal.

### Claim 8 (depends on 7)

The method of claim 7, wherein the alkaline earth metal comprises calcium, strontium, or barium.

### Claim 9 (depends on 8)

The method of claim 8, wherein M(OR)x comprises Ca(OAr)2.

### Claim 10 (depends on 8)

The method of claim 8, wherein M(OR)x comprises AE(ONep)2 and AE comprises strontium or barium and wherein ONep is neopentoxide.

### Claim 11 (depends on 7)

The method of claim 7, wherein the transition metal comprises cadmium.

### Claim 12 (depends on 11)

The method of claim 11, wherein M(OR)x comprises Cd(OAr)2 or Cd(ONep)2.

### Claim 13 (depends on 7)

The method of claim 7, wherein the transition metal comprises tungsten or molybdenum.

### Claim 14 (depends on 13)

The method of claim 13, wherein the nanomaterial comprises a layered structure.

### Claim 15 (depends on 2)

The method of claim 2, wherein the nanomaterial comprises a layered structure.
