NOVEL PROCESS FOR SCALABLE SYNTHESIS OF MOLYBDENUM DISULFIDE MONOLAYER AND FEW-LAYER FILMS

Brian C. Iezzi

Patent

Atlas literature

Patent

US 9,527,062

NOVEL PROCESS FOR SCALABLE SYNTHESIS OF MOLYBDENUM DISULFIDE MONOLAYER AND FEW-LAYER FILMS

Brian C. Iezzi, Yanpeng Li, Linyou Cao, Yifei Yu

2016-12-27·US

Drawings

Patent drawings and their descriptions. Click a drawing to enlarge it.

FIG. 1

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FIG. 9

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FIG. 28

FIG. 29

Claims

Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.

4 independent · 16 dependent

1
IndependentSMoCl₅MoS₂
A synthesis process comprising: sublimation of sulfur and MoCl s; reaction of MoCl s and S to produce gaseous MoS₂ species; transfer of the MoS₂ species by carrier gas; diﬀusion and precipitation of MoS₂ species from the gas phase onto a substrate under suitable conditions that one to four layer(s) of MoS₂ form on the substrate, wherein the substrate is highly ordered pyrol y tic graphite (HOPG).
1. 2
  Dependent← claim 1SMoCl₅MoS₂
  The synthesis process of claim 1, wherein MoCl s is reacted with sulfur at a temperature of about 300 0 C to about 1000 ° C to give rise to MoS₂ on the substrate.
2. 5
  Dependent← claim 1MoS₂
  The synthesis process of claim 1, wherein one layer of MoS₂ is formed on the substrate.
3. 6
  Dependent← claim 1MoS₂
  The synthesis process of claim 1, wherein two layers of MoS₂ are formed on the substrate. 2 TH Docket No₂₂₁₄₀₄-1020 U.S. S.N. 14/274,154 Filed: AMENDMENTS AND RESPONSE TO OFFICE ACTION
4. 7
  Dependent← claim 1MoS₂
  The synthesis process of claim 1, wherein four layers of MoS₂ are formed on the substrate.
4
Independent
canceled
8
IndependentMoS₂
A method of producing hydrogen which comprises contacting a suitable reactant under appropriate conditions with the layered MoS₂ substrate prepared by the synthesis process of claim
9
IndependentSMoCl₅MoS₂substrate
A method of making a large-area MoS₂ thin ﬁlm on a surface of a substrate, the method comprising the steps of: reacting MoCl s with a stoichiometric excess of S in a reactor at an elevated temperature to produce gaseous MoS2, depositing the gaseous MoS₂ at a pressure onto the surface of the substrate; wherein the amount of the MoCl s and the pressure are controlled to produce the large-area MoS₂ thin ﬁlm on the surface of the substrate; and wherein the substrate is selected from the group consisting of silicon, silicon oxide, sapphire, graphite, and a combination thereof.
1. 10
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm consists of about 1- 4 layers of MoS2.
2. 11
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm consists of a monolayer or a bilayer of MoS2.
3. 12
  Dependent← claim 9
  The method of claim 9, wherein the elevated temperature is about 300 C to about 1000 °C.
4. 13
  Dependent← claim 9
  The method of claim 9, wherein the pressure is about 2 Torr to 10 Torr. 3 TH Docket No₂₂₁₄₀₄-1020 U.S. S.N. 14/274,154 Filed: AMENDMENTS AND RESPONSE TO OFFICE ACTION
5. 14
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has an area of about 1 cm 2 or more.
6. 15
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has an area of about 1 cm 2 to about 3 cm 2.
7. 16
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has a Raman spectra with an E 2 g band associated with in-plane vibration of Mo in the MoS₂ thin ﬁlm, and the full width at half maximum of the E₂ g peak is about 4.2 cm ~ or less. 17 The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has an average thickness of about 0.68 nm to about 2.54 nm.
8. 18
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has a Raman spectra with an A i g band associated with out-of-plane vibration of sulfur atoms in the MoS₂ thin ﬁlm and an E 2 g band associated with in-plane vibration of Mo in the MoS₂ thin ﬁlm, and wherein there is a frequency diﬀerence in the A i g band and the E₂ g band of about 20.2 cm ~ to about 24.0 SVG 14274154.05-10-2016.IO₄LR₄₉₇PXXIFW1.CLM.3.18.928.2055.1012.2101.svg 0.153 0.28 Chemistry Black and white.
9. 19
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the large-area MoS₂ thin ﬁlm has a roughness of less than 0.2 nm.
10. 20
  Dependent← claim 9MoS₂
  The method of claim 9, wherein the method further comprises balancing the partial pressure of the gaseous MoS₂ and the vapor pressure of the MoS₂ thin ﬁlm on the substrate to produce the large-area MoS₂ thin ﬁlm on the surface of the substrate consisting of 1-4 layers of MoS2. 4 TI H Docket No₂₂₁₄₀₄-1020 U.S. S.N. 14/274,154 Filed: AMENDMENTS AND RESPONSE TO OFFICE ACTION
11. 21
  Dependent← claim 9SMoCl₅
  The method of claim 9, wherein the molar ratio of the S to the MoCl s is greater than 1000:1. 5 T I H Docket No₂₂₁₄₀₄-1020

Device structures

Layer stacks claimed or described, ordered top of device to substrate.

field-effect transistor (FET)

MoS₂channel

Materials

Materials described outside the worked examples.

sulfur

Precursor

molybdenum pentachloride

MoCl₅

Precursor

molybdenum disulfide

MoS₂

Process steps

Additional fabrication and treatment steps described in the patent.

Cvd Growth

Step 1

Temperature

850°C

Process details

notes:Typical experimental conditions from Fig. 20 caption: deposition temperature 850°C, total pressure 2-3 Torr, flow rate 50 sccm, amount of sulfur 1 g. Layer number controlled by amount of MoCl5.

precursors:MoCl5, S

flow rate sccm:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Optical Band Gap	1.8 eV	MoS₂
Raman E2g FWHM	≤ 4.2 cm⁻¹

Why these are connected

Related documents with shared materials, methods, properties, or citations.

NOVEL PROCESS FOR SCALABLE SYNTHESIS OF MOLYBDENUM DISULFIDE MONOLAYER AND FEW-LAYER FILMS | Matter42 Literature