# US 5,348,936 A · Metal-doped fullerenes and synthetic methods therefor

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- Number: US 5,348,936 A
- Document ID: US5348936A
- Status: Granted
- Kind: A
- Application number: 08/048,651
- Filed: 1993-04-16
- Granted: 1994-09-20
- Earliest claimed: 1991-08-01
- Assignees: The Trustees of the University of Pennsylvania
- Inventors: John P. McCauley, Jr.; Qing Zhu; Gavin Vaughan; Nicole Coustel
- Web page: https://patentgrep.com/patent/US5348936A

## CPC

- C01B 32/15: Nano-sized carbon materials
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 32/156: After-treatment
- Y10S 505/725: Process of making or treating high tc, above 30 k, superconducting shaped material, article, or device
- Y10S 505/775: High tc, above 30 k, superconducting material
- Y10S 505/81: Compound
- Y10S 505/815: Process of making per se
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

Superconducting, metal-doped fullerenes are provided, along with processes for their preparation in relatively high stoichiometric purity. In one embodiment, the processes provide fullerenes of the formula M.sub.x C.sub.q, where M is a metal, x is greater than 0 but less than about 10, and q is at least 60. The processes comprise contacting C.sub.q with metal in an amount and under reaction conditions effective to produce a compound having the formula M.sub.y C.sub.q, and contacting said M.sub.y C.sub.q with a portion of C.sub.q in an amount and under reaction conditions effective to produce said M.sub.x C.sub.q, wherein y is greater than x.

## Claims

### Claim 1

A process for preparing a compound having the formula M.sub.3 C.sub.60, comprising the steps of:
contacting C.sub.60 with metal under reaction conditions effective to produce a compound having the formula M.sub.6 C.sub.60 ; and
contacting one equivalent of said MeC.sub.60 with an equivalent of C.sub.60 under reaction conditions effective to produce said M.sub.3 C.sub.60.

### Claim 2 (depends on 1)

The process of claim 1 wherein the metal is potassium, rubidium, or combinations thereof.

### Claim 3

A process for preparing a compound having the formula M.sub.x C.sub.60 where M is metal and x is greater than 0 and less than about 10, comprising the steps of:
contacting C.sub.60 with metal in an amount and under reaction conditions effective to produce a compound having the formula M.sub.y C.sub.60, where y is greater than x; and
contacting said M.sub.y C.sub.60 with a portion of C.sub.60 in an amount and under reaction conditions effective to produce said M.sub.x C.sub.60.

### Claim 4

A process for preparing a compound having the formula M.sub.x C.sub.q where M is metal, x is greater than 0 and less than about 10, and q is greater than about 60, comprising the steps of:
contacting C.sub.q with metal in an amount and under reaction conditions effective to produce a compound having the formula M.sub.y C.sub.q, where y is greater than x; and
contacting said M.sub.y C.sub.q with C.sub.q in an amount and under reaction conditions effective to produce said M.sub.x C.sub.q.

### Claim 5 (depends on 4)

The process of claim 4 wherein M is lithium, sodium, potassium, rubidium, cesium, francium, or combinations thereof.

### Claim 6 (depends on 4)

The process of claim 4 wherein M is potassium, rubidium, cesium, or combinations thereof.

### Claim 7 (depends on 4)

The process of claim 4 wherein x is about 2 to about 4.

### Claim 8 (depends on 4)

The process of claim 4 wherein x is about 3.

### Claim 9 (depends on 4)

The process of claim 4 wherein q is 60, 70, 76, 84, 90, or 94.

### Claim 10 (depends on 4)

The process of claim 4 wherein q is 60.

### Claim 11 (depends on 4)

The process of claim 4 wherein 1 equivalent of said C.sub.q is contacted with at least 6 equivalents of said metal.

### Claim 12 (depends on 4)

The process of claim 4 wherein said C.sub.q is contacted with said metal at a temperature from about 150.degree. C. to about 450 .degree. C.

### Claim 13 (depends on 4)

The process of claim 4 wherein said C.sub.q is contacted with said metal at a temperature about 250.degree. C.

### Claim 14 (depends on 4)

The process of claim 4 wherein y is about 3 to about 12.

### Claim 15 (depends on 4)

The process of claim 4 wherein y is about 4 to about 8.

### Claim 16 (depends on 4)

The process of claim 4 wherein y is about 6.

### Claim 17 (depends on 4)

The process of claim 4 wherein x is about 3 and y is about 6.

### Claim 18 (depends on 17)

The process of claim 17 wherein one equivalent of said M.sub.6 C.sub.q is contacted with 1 equivalent of said C.sub.q.

### Claim 19 (depends on 4)

The process of claim 4 wherein said M.sub.y C.sub.q is contacted with said C.sub.q at a temperature from about 150.degree. C. to about 450.degree. C.

### Claim 20 (depends on 4)

The process of claim 4 wherein said M.sub.y C.sub.q is contacted with said C.sub.q at a temperature about 350.degree. C.