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Patent US4604276A successfully refreshed from Google Patents.
US4604276A
Expired / Lapsed
US
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Intercalation of small graphite flakes with a metal halide
Assignee: Verizon Laboratories Inc
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Filing: 1983-09-19
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Granted: 1986-08-05
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Expires: 2003-09-19
Abstract
Abstract A method and apparatus for intercalating small graphite flakes with a metal halide. Graphite and a metal halide are placed in two chambers 12, 14 of a rotary vapor transport reactor assembly 10 and heated. The reactor is charged with a halogen gas and rotated by motor 24 during synthesis to produce a homogenous and uniform intercalated product.
Inventors
- 👤 Daniel W. Oblas
- 👤 Sophia R. Su
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 05:45
CPC Classifications
B; B01; B01J; B01J19/00; B01J19/28; C; C01; C01B; C01B32/00; C01B32/20; C01B32/21; C01B32/22; B01J2219/00; B01J2219/00049; B01J2219/00051; B01J2219/00132; B01J2219/0015; B01J2219/00162; B01J2219/00189
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
160 words
A method of intercalating small graphite flakes with an electron-acceptor metal halide, comprising: placing said graphite flakes in a first zone of a two zone vapor transport reactor; placing said metal halide in a second zone of said reactor; charging said reactor with an intercalation-promoting halogen gas; supplying heat to the second zone of said reacotr to provide a temperature therein sufficient to vaporize said metal halide and produce a partial pressure of the metal halide sufficent to promote intercalation; supplying sufficient heat to the first zone of said reactor to provide a temeprature therein slightly elevated with regard to the temperature in said second zone and sufficient to prevent condensation of the metal halide on the graphite; slowly rotating said reactor about its horizontal axis while supplying heat to the second zone of said reactor and to the first zone of said reactor; and maintaining said reaction conditions until the graphite flakes have been intercalated with said metal halide.
Claim 2
Independent Claim
160 words
A method of intercalating small graphite flakes with an electron-acceptor metal halide, comprising: placing said graphite flakes in a first zone of a two zone vapor transport reactor; placing said metal halide in a second zone of said reactor; charging said reactor with an intercalation-promoting halogen gas; supplying heat to the second zone of said reacotr to provide a temperature therein sufficient to vaporize said metal halide and produce a partial pressure of the metal halide sufficent to promote intercalation; supplying sufficient heat to the first zone of said reactor to provide a temeprature therein slightly elevated with regard to the temperature in said second zone and sufficient to prevent condensation of the metal halide on the graphite; slowly rotating said reactor about its horizontal axis while supplying heat to the second zone of said reactor and to the first zone of said reactor; and maintaining said reaction conditions until the graphite flakes have been intercalated with said metal halide.
Claim 3
Dependent Claim
20 words
The method of claim 1 wherein the aspect ratio of the graphite flakes is at least about 10 to 1.
Claim 4
Dependent Claim
30 words
The method of claim 2 wherein said graphite flakes have a mean flake diameter of less than about 10 microns and a mean thickness of less than about 1 micron.
Claim 5
Dependent Claim
11 words
The method of claim 3 wherein said intercalation-promoting gas is chlorine.
Claim 6
Dependent Claim
56 words
The method of claim 4 wherein said metal halide is selected from the group consisting of: FeCl 3 , CuCl 2 , SbCl 5 , SbCl 3 , PdCl 2 , NiCl 2 , MoCl 5 , ZrCl 4 , HgCl 2 , AlCl 3 , InCl 3 , TaCl 5 , and WCl 6 .
Claim 7
Dependent Claim
12 words
The method of claim 4 wherein said metal halide comprises ferric chloride.
Claim 8
Dependent Claim
12 words
The method of claim 6 wherein the graphite flakes comprise spun flakes.
Claim 9
Dependent Claim
13 words
The method of claim 6 wherein the graphite flakes comprise natural graphite flakes.
Claim 10
Dependent Claim
13 words
The method of claim 6 wherein the graphite flakes comprise synthetic graphite flakes.
Claim 11
Dependent Claim
16 words
A method of claim 6 in which the reactor is a horizontally positioned cylindrical rotary reactor.
Claim 12
Independent Claim
160 words
A method of intercalating small graphite flakes with ferric chloride, comprising: placing the graphite flakes in a first zone of a two zone vapor transport reactor; placing the ferric chloride in a second zone of a two zone vapor transport reactor; charging the reactor with chlorine gas; supplying heat to the second zone of the reactor to provide a temperature therein sufficient to vaporize the ferric chloride and produce a partial pressure of the ferric chloride sufficient to promote intercalation; supplying sufficient heat to the first zone of the reactor to provide a temperature therein slightly elevated with regard to the temperature in the second zone and sufficient to prevent condensation of the ferric chloride on the graphite; slowly rotating the reactor about its horizontal axis while supplying heat to the second zone of the reactor and to the first zone of the reactor; and maintaining the reaction conditions until the graphite flakes have been intercalated with the ferric chloride.
Claim 13
Independent Claim
160 words
A method of intercalating small graphite flakes with ferric chloride, comprising: placing the graphite flakes in a first zone of a two zone vapor transport reactor; placing the ferric chloride in a second zone of a two zone vapor transport reactor; charging the reactor with chlorine gas; supplying heat to the second zone of the reactor to provide a temperature therein sufficient to vaporize the ferric chloride and produce a partial pressure of the ferric chloride sufficient to promote intercalation; supplying sufficient heat to the first zone of the reactor to provide a temperature therein slightly elevated with regard to the temperature in the second zone and sufficient to prevent condensation of the ferric chloride on the graphite; slowly rotating the reactor about its horizontal axis while supplying heat to the second zone of the reactor and to the first zone of the reactor; and maintaining the reaction conditions until the graphite flakes have been intercalated with the ferric chloride.
References Cited (Backward Citations)
US3956194A
Cited
US4461719A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-08-04 | 1990-02-03 | 1990-08-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-08-04 | 1994-02-03 | 1994-08-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-08-04 | 1998-02-03 | 1998-08-05 | $7700.00 | Window Closed / Lapsed |