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US4299892A Expired / Lapsed US ⏱️ 0.0 years remaining

Amorphous and sheet dichalcogenides of Group IVb, Vb, molybdenum and tungsten

Assignee: ExxonMobil Technology and Engineering Co
•
Filing: 1980-07-28
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Granted: 1981-11-10
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Expires: 2000-07-28
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Abstract

Abstract Dichalcogenides of Group IVb, Vb, molybdenum and tungsten of two new forms have been discovered. The two new forms are the amorphous and layered-sheet configurations. In particular, the dichalcogenides of Group IVb, Ib, molybdenum and tungsten, i.e. Z(MX2)n wherein M is the metal and X is the chalcogen, n is at least about 20,000 and Z is the number of such (MX2)n sheets ranging from 1-10, can be described as possessing a "rag-like" structure representing a system consisting of single or several stacked but randomly folded and disordered layers or sheets having dimensions (as determined by TEM) corresponding to about 6.2 to 62 A in thickness, about 500 A minimum length by about 500 A minimum width. Broadly the rag-like (MX2)n can be likened to a stack of polymer sheets wherein each sheet is one atom thick. These sheets of (MX2)n are prepared by the controlled heating (in a flowing stream of H2/H2S) of amorphous MX2 obtained by the monaqueous low temperature precipitation of MX2 from mixtures of the metal salt and sources of sulfur, selenium or tellurium.

Inventors

  • 👤 Martin B. Dines
  • 👤 Russell R. Chianelli

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 21:13
CPC Classifications
C; C01; C01B; C01B19/00; C01B19/007; B; B82; B82Y; B82Y30/00; C01G; C01G1/00; C01G1/12; C01G23/00; C01G23/007; C01G31/00; H; H01; H01M; H01M4/00; H01M4/02; H01M4/36; H01M4/58; H01M6/00; H01M6/14; H01M6/16; C01P; C01P2002/00; C01P2002/02; C01P2002/20; C01P2002/22; C01P2002/60; C01P2002/70; C01P2002/72; C01P2002/80; C01P2002/82; C01P2004/00; C01P2004/01; C01P2004/03; C01P2004/60; C01P2004/62; C01P2004/64; C01P2006/00; C01P2006/12; C01P2006/80; H01M6/162; H01M6/164; H01M6/166; Y; Y10; Y10S; Y10S505/00; Y10S505/80; Y10S505/801; Y10S505/815; Y10S505/824

Claims Analysis

Total Claims: 29
Claim 1
Independent Claim 47 words
A composition of the formula MX 2 which is amorphous to X-rays, wherein M is a metal selected from the group consisting of Group IVb, Group Vb, molybdenum and tungsten transition metals and X is a chalcogen selected from the group consisting of sulfur, selenium and tellurium.
Claim 2
Dependent Claim 47 words
A composition of the formula MX 2 which is amorphous to X-rays, wherein M is a metal selected from the group consisting of Group IVb, Group Vb, molybdenum and tungsten transition metals and X is a chalcogen selected from the group consisting of sulfur, selenium and tellurium.
Claim 3
Dependent Claim 14 words
The amphorous compositions of claim 1 wherein M is molybdenum and X is sulfur.
Claim 4
Dependent Claim 14 words
The amorphous compositions of claim 1 wherein M is niobium and X is sulfur.
Claim 5
Dependent Claim 14 words
The amorphous compositions of claim 1 wherein M is vanadium and X is sulfur.
Claim 6
Dependent Claim 111 words
A composition of the formula Z(MX 2 ) n wherein M is a metal selected from the group consisting of Group IVb, Vb, molybdenum and tungsten, X is a chalcogen selected from the group consisting of sulfur, selenium and tellurium and n is at least 20,000, the formula (MX 2 ) n representing a single sheet of the material (MX 2 ) and Z is the number of such sheets from 1 to 10 existing in a stack, wherein the sheet or stack of sheets have the dimensions of about 6.2 to 62 A in thickness, at least about 500 A in length and at least about 500 A in width.
Claim 7
Dependent Claim 111 words
A composition of the formula Z(MX 2 ) n wherein M is a metal selected from the group consisting of Group IVb, Vb, molybdenum and tungsten, X is a chalcogen selected from the group consisting of sulfur, selenium and tellurium and n is at least 20,000, the formula (MX 2 ) n representing a single sheet of the material (MX 2 ) and Z is the number of such sheets from 1 to 10 existing in a stack, wherein the sheet or stack of sheets have the dimensions of about 6.2 to 62 A in thickness, at least about 500 A in length and at least about 500 A in width.
Claim 8
Dependent Claim 41 words
The composition of claims 5 wherein the sheet or stack of sheets are from about 6.2 to 62 A in thickness, at least about 1000 A in length and at least about 1000 A in width, and n is about 80,000.
Claim 9
Dependent Claim 13 words
The composition of claim 6 wherein M is molybdenum and X is sulfur.
Claim 10
Dependent Claim 13 words
The composition of claim 6 wherein M is titanium and X is sulfur.
Claim 11
Dependent Claim 13 words
The composition of claim 6 wherein M is niobium and X is sulfur.
Claim 12
Dependent Claim 186 words
Homogeneous dispersions of metal chalcogenides of the formula MX 2 wherein M is a transition metal selected from the group consisting of Group IVb, Vb, molybdenum and tungsten transition metals and X is a chalcogen selected fromthe group consisting of sulfur, selenium, and tellurium prepared by mixing in the presence of a non-aqueous, aprotic polar organic solvent at at temperature of between -78° to 400° C.: a. metal salts, the metal being selected from the group consisting of Group IVb, Group Vb, molybdenum and tungsten transition metals, and b. sources of sulfide, selenide or telluride ion, wherein said sources are selected from the group consisting of Li 2 X, Na 2 X, K 2 X, LiHX, NaHX, KHX, (NH 4 ) 2 X, (NH 4 )HX, (RNH 3 ) 2 X, (RR'NH 2 ) 2 X, (RR'R"NH) 2 X wherein R, R' and R" are the same or different and are selected from the group consisting of C 1 to C 20 alkyl and C 6 to C 20 aryl groups and X is the chalcogen selected from the group consisting of sulfur, selenium, and tellurium.
Claim 13
Dependent Claim 186 words
Homogeneous dispersions of metal chalcogenides of the formula MX 2 wherein M is a transition metal selected from the group consisting of Group IVb, Vb, molybdenum and tungsten transition metals and X is a chalcogen selected fromthe group consisting of sulfur, selenium, and tellurium prepared by mixing in the presence of a non-aqueous, aprotic polar organic solvent at at temperature of between -78° to 400° C.: a. metal salts, the metal being selected from the group consisting of Group IVb, Group Vb, molybdenum and tungsten transition metals, and b. sources of sulfide, selenide or telluride ion, wherein said sources are selected from the group consisting of Li 2 X, Na 2 X, K 2 X, LiHX, NaHX, KHX, (NH 4 ) 2 X, (NH 4 )HX, (RNH 3 ) 2 X, (RR'NH 2 ) 2 X, (RR'R"NH) 2 X wherein R, R' and R" are the same or different and are selected from the group consisting of C 1 to C 20 alkyl and C 6 to C 20 aryl groups and X is the chalcogen selected from the group consisting of sulfur, selenium, and tellurium.
Claim 14
Dependent Claim 33 words
The homogeneous dispersions prepared as in claim 10 wherein the polar organic solvent is selected from the group consisting of propylene carbonate, dimethylformamide, pyridine, acetonitrile, benzonitrile, propionitrile, 1,2 demethoxyethane, diglyme and N-methyl formamide.
Claim 15
Dependent Claim 21 words
The homogeneous dispersions prepared as in claim 10 or 11 wherein the reaction temperature ranges from between 25° to 300° C.
Claim 16
Dependent Claim 15 words
The homogeneous dispersion prepared as in claims 10 or 11 wherein the chalcogen is sulfur.
Claim 17
Dependent Claim 42 words
The homogeneous dispersions prepared as in claims 10 or 11 further comprising the deposition of said homogeneous dispersion on high surface area supports, said supports being selected from the group consisting of high surface area refractory oxides and high surface area carbon.
Claim 18
Dependent Claim 35 words
The supported homogeneous dispersions prepared as in claim 14 wherein the high surface area supports are selected from the group consisting of CAO, MgO, Al 2 O 3 , silica-alumina and high surface area carbon.
Claim 19
Dependent Claim 46 words
The homogeneous dispersion prepared as in claim 10 or 11 wherein the anion of the metal salt is selected from the group comprising halides, sulfates, nitrates, carboxylates, perfluorocarboxylates wherein the carbonaceous moiety of the anion is a C 1 to C 8 hydrocarbon or fluorocarbon radical.
Claim 20
Dependent Claim 274 words
An electric current-producing cell, comprising: (a) an anode having as its anode-active material one or more metals selected from the group consisting of Group IA metals, Group IB metals, Group IIA metals and Group IIB metals of the Periodic Table of the Elements; (b) a cathode having as its cathode active material one or more compounds selected from the group consisting of amorphous MX 2 wherein M is a Group IVB, Group VB, molybdenum or tungsten transition metal and X is a chalcogen selected from the group consisting of sulfur, selenum and lithium which MX 2 material is prepared by the method comprising reacting at a temperature of between -78° to 400° C; (i) metal salts, the metal being selected from the group consisting of Group IVB, Group VB, molybdenum and tungsten transition metals, and (ii) sources of sulfide, selenide or lelluride ion, wherein said sources are selected from the group consisting of Li 2 X, Na 2 X, K 2 X, LiHX, NaHX, KHX, (NH 4 ) 2 X, (NH 4 )HX, (RNH 3 ) 2 X, (RR'NH 2 ) 2 X, (RR'R"NH) 2 X wherein R, R' and R" are the same or different and are selected from the group consisting of C 1 to C 20 alkyl and C 10 to C 20 aryl groups and X is the chalcogen selected from the group consisting of sulfur, selenium and tellurium, reactants (i) and (ii) being reacted in the absence of an aqueous-protic solvent. (iii) an electrolyte which is chemically inert with respect to said anode and said cathode and which permits the migration of ions between said anode and said cathode.
Claim 21
Dependent Claim 274 words
An electric current-producing cell, comprising: (a) an anode having as its anode-active material one or more metals selected from the group consisting of Group IA metals, Group IB metals, Group IIA metals and Group IIB metals of the Periodic Table of the Elements; (b) a cathode having as its cathode active material one or more compounds selected from the group consisting of amorphous MX 2 wherein M is a Group IVB, Group VB, molybdenum or tungsten transition metal and X is a chalcogen selected from the group consisting of sulfur, selenum and lithium which MX 2 material is prepared by the method comprising reacting at a temperature of between -78° to 400° C; (i) metal salts, the metal being selected from the group consisting of Group IVB, Group VB, molybdenum and tungsten transition metals, and (ii) sources of sulfide, selenide or lelluride ion, wherein said sources are selected from the group consisting of Li 2 X, Na 2 X, K 2 X, LiHX, NaHX, KHX, (NH 4 ) 2 X, (NH 4 )HX, (RNH 3 ) 2 X, (RR'NH 2 ) 2 X, (RR'R"NH) 2 X wherein R, R' and R" are the same or different and are selected from the group consisting of C 1 to C 20 alkyl and C 10 to C 20 aryl groups and X is the chalcogen selected from the group consisting of sulfur, selenium and tellurium, reactants (i) and (ii) being reacted in the absence of an aqueous-protic solvent. (iii) an electrolyte which is chemically inert with respect to said anode and said cathode and which permits the migration of ions between said anode and said cathode.
Claim 22
Dependent Claim 24 words
The electric current producing cell of claim 17 wherein the MX 2 material is amorphous VS 2 , MoS 2 or TiS 2 .
Claim 23
Dependent Claim 18 words
The electric current producing cell of claim 17 wherein the MX 2 material is amorphous VS 2 .
Claim 24
Dependent Claim 18 words
The electric current producing cell of claim 17 wherein the MX 2 material is amorphous MoS 2 .
Claim 25
Dependent Claim 76 words
The electric current producing cell of claim 17, 18, 19 or 20 wherein the amorphous MX 2 material is prepared in the absence of a non-aqueous solvent selected from the group consisting of acetonitule benzonitule, propronitule, acetone, C 1 -C 20 aryl-halides 1,2 demethoxyelhane, deqlyne, N-methyl formamide, dimethylformamide, aromatics of C 6 -C 30 amines, C 5 -C 12 alkanes, C 4 -C 8 ethers, propylene carbonate C 4 -C 8 esters, molten sulfur, sulfur dioxide.
Claim 26
Dependent Claim 31 words
The electric current producing cell of claims 17, 18, 19 or 20 wherein said anode has as its anode active material one or more metals selected from the Group IA metals.
Claim 27
Dependent Claim 22 words
The electric current producing cell of claims 17, 18, 19 or 20 wherein the anode has lithium as its anode active material.
Claim 28
Dependent Claim 18 words
The electric current producing cell of claim 21 wherein the anode has lithium as its anode active material.
Claim 29
Dependent Claim 47 words
The electric current producing cell of claim 17 wherein the anion of the metal salt of (b) (i) is selected from the group comprising halides, sulfates, nitrates, carboxylates, perfluorocarboxylates wherein the carbonaceous moiety of the anion is a C 1 to C 8 hydrocarbon or fluorocarbon radical.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-11-09 1985-05-11 1985-11-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-11-09 1989-05-11 1989-11-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-11-09 1993-05-11 1993-11-10 $7700.00 Window Closed / Lapsed

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