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US4822590A
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Forms of transition metal dichalcogenides
Assignee: SIMON FRASER UNIVERSITY BURNABY BC CANADA V5A 1S6
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Filing: 1986-04-23
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Granted: 1989-04-18
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Expires: 2006-04-23
Abstract
Abstract Novel single layer materials of the form MX 2 , where MX 2 is a layer-type dichalcogenide such as MoS 2 , TaS 2 , WS 2 , or the like, exfoliated by intercalation of an alkali metal, and immersion in water, are disclosed. MoS 2 has been exfoliated into monolayers by intercalation with lithium followed by reaction with water. X-ray diffraction analysis demonstrates that the exfoliated MoS 2 in suspension is in the form of one-molecule-thick sheets. X-ray patterns from dried and re-stacked films of exfoliated MoS 2 indicate that the layers are randomly stacked. By adsorbing monolayers or precipitating clusters of various species such as compounds of Co, Ni, Pb, Cd, Al, Ce, In and Zn, on MoS 2 while the sulfide is suspended as single layers and then recrystallizing, a new group of inclusion compounds can be formed. In the re-crystallized or re-stacked materials, the inter-layer spacing can be expanded or contracted compared to MoS 2 .
Inventors
- 👤 S. Roy Morrison
- 👤 Robert F. Frindt
- 👤 Per Joensen
- 👤 Michael A. Gee
- 👤 Bijan K. Miremadi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 16:27
CPC Classifications
H; H01; H01M; H01M4/00; H01M4/02; H01M4/36; H01M4/58; H01M4/581; H01M4/5815; C; C01; C01B; C01B17/00; C01B17/20; C01B19/00; C01B19/002; C01B19/007; C01G; C01G35/00; C01G39/00; C01G39/06; C01G41/00; C01P; C01P2002/00; C01P2002/20; C01P2002/70; C01P2002/72; C01P2002/80; C01P2002/85; C01P2006/00; C01P2006/12; C01P2006/80; Y; Y02; Y02E; Y02E60/00; Y02E60/10; Y10; Y10S; Y10S106/00; Y10S106/02
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
106 words
An exfoliation process for preparing a single layer substance of the form MX.sub.2 wherein MX 2 is a layer type transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; and (b) immersing the alkali metal intercalated MX 2 in a liquid that generates a gas upon reaction with the alkali metal to thereby with suitable agitation cause the layers of MX 2 to separate.
Claim 2
Dependent Claim
106 words
An exfoliation process for preparing a single layer substance of the form MX.sub.2 wherein MX 2 is a layer type transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; and (b) immersing the alkali metal intercalated MX 2 in a liquid that generates a gas upon reaction with the alkali metal to thereby with suitable agitation cause the layers of MX 2 to separate.
Claim 3
Dependent Claim
15 words
A process as defined in claim 1 wherein the MX 2 is MoS 2 .
Claim 4
Dependent Claim
15 words
A process as defined in claim 1 or 2 wherein the alkali metal is lithium.
Claim 5
Dependent Claim
143 words
A process of preparing a simple substance of the form MX.sub.2 :Y wherein MX 2 is a layered transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 , and Y is a foreign substance or substances which can be associated with the MX 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; (b) immersing the alkali metal intercalated MX 2 in water or other suitable liquid to thereby with suitable agitation cause the layers of MX 2 to separate; (c) precipitating or adsorbing ions of a Y substance on the surfaces of the MX 2 ; and (d) washing, if appropriate, and drying the resulting MX 2 :Y product.
Claim 6
Dependent Claim
143 words
A process of preparing a simple substance of the form MX.sub.2 :Y wherein MX 2 is a layered transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 , and Y is a foreign substance or substances which can be associated with the MX 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; (b) immersing the alkali metal intercalated MX 2 in water or other suitable liquid to thereby with suitable agitation cause the layers of MX 2 to separate; (c) precipitating or adsorbing ions of a Y substance on the surfaces of the MX 2 ; and (d) washing, if appropriate, and drying the resulting MX 2 :Y product.
Claim 7
Dependent Claim
147 words
A process of preparing a substance of the form MX.sub.2 :Y wherein MX 2 is a layered transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 and Y is a foreign substance or substances which can be associated with the MX 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; (b) immersing the alkali intercalated MX 2 in water or other suitable liquid which contains ions of Y to thereby with suitable agitation cause the layers of MX 2 to separate and the Y ions to adsorb or precipitate on the surfaces of the separated layers of MX 2 ; and (c) washing, if appropriate, and drying the resulting MX 2 :Y product.
Claim 8
Dependent Claim
147 words
A process of preparing a substance of the form MX.sub.2 :Y wherein MX 2 is a layered transition metal dichalcogenide selected from the group consisting of MoS 2 , TaS 2 , WS 2 and Y is a foreign substance or substances which can be associated with the MX 2 , which comprises: (a) intercalating multi-layer MX 2 with an alkali metal in a dry environment for sufficient time to enable the alkali metal to substantially intercalate the layers of the MX 2 ; (b) immersing the alkali intercalated MX 2 in water or other suitable liquid which contains ions of Y to thereby with suitable agitation cause the layers of MX 2 to separate and the Y ions to adsorb or precipitate on the surfaces of the separated layers of MX 2 ; and (c) washing, if appropriate, and drying the resulting MX 2 :Y product.
Claim 9
Dependent Claim
29 words
A process as defined in claim 5 wherein the pH of the water is maintained at a sufficiently low level to cause the Y ions to remain in solution.
Claim 10
Dependent Claim
13 words
A process as defined in claim 4 wherein the alkali metal is lithium.
Claim 11
Dependent Claim
13 words
A process as defined in claim 5 wherein the alkali metal is lithium.
Claim 12
Dependent Claim
15 words
A process as defined in claim 4 wherein the MX 2 is MoS 2 .
Claim 13
Dependent Claim
15 words
A process as defined in claim 5 wherein the MX 2 is MoS 2 .
Claim 14
Dependent Claim
21 words
A process as defined in claim 4 wherein two or more different species of MX 2 are present in the process.
Claim 15
Dependent Claim
21 words
A process as defined in claim 5 wherein two or more different species of MX 2 are present in the process.
Claim 16
Dependent Claim
31 words
A process as defined in claim 4 wherein the Y substance is selected from the group consisting of compounds of Co, Ni, Pb, Cd, Al, Ce, In, Pd, Sr and Zr.
Claim 17
Dependent Claim
31 words
A process as defined in claim 5 wherein the Y substance is selected from the group consisting of compounds of Co, Ni, Pb, Cd, Al, Ce, In, Pd, Sr and Zr.
Claim 18
Dependent Claim
31 words
A process as defined in claim 4 wherein the Y substance is precipitated on the surfaces of the separated layers of MX 2 in a single molecular layer or in clusters.
Claim 19
Dependent Claim
31 words
A process as defined in claim 5 wherein the Y substance is precipitated on the surfaces of the separated layers of MX 2 in a single molecular layer or in clusters.
Claim 20
Dependent Claim
32 words
A process as defined in claim 11 wherein upon ultimate drying, the different species of MX 2 restack so that layers of one species are located between layers of the other species.
Claim 21
Dependent Claim
19 words
A process as defined in claim 4 followed by changing the chemical form of Y by dehydration or reduction.
Claim 22
Dependent Claim
18 words
A process as defined in claim 1 wherein the alkali metal is lithium and the liquid is water.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1992-04-17 | 1992-10-17 | 1993-04-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-04-17 | 1996-10-17 | 1997-04-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-04-17 | 2000-10-17 | 2001-04-18 | $7700.00 | Window Closed / Lapsed |