CA2500077A1 - Production of ultra fine transition metal powders - Google Patents
Production of ultra fine transition metal powders Download PDFInfo
- Publication number
- CA2500077A1 CA2500077A1 CA 2500077 CA2500077A CA2500077A1 CA 2500077 A1 CA2500077 A1 CA 2500077A1 CA 2500077 CA2500077 CA 2500077 CA 2500077 A CA2500077 A CA 2500077A CA 2500077 A1 CA2500077 A1 CA 2500077A1
- Authority
- CA
- Canada
- Prior art keywords
- metal
- ultra fine
- powder
- transition metal
- inert solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
Abstract
A method of preparing ultra fine metal powder comprising pyrolizing a complex metal compound of the metal is in a valence state selected from 0 and 1, in an inert solvent at an effective temperature to produce the ultra fine powder, and removing the powder from the inert solvent.
Description
~ r PRODUCTION OF ULTRA FINE
TRANSITION METAL POWDERS
FIELD OF THE INVENTION
This invention relates to a process for the production of ultra fine transition metal powders, particularly, vanadium, niobium and tantalum powders by the pyrolysis of transition metal complexes in a high boiling point inert solvent, such as a hydrocarbon or higher alkyl alcohol.
PUBLICATIONS
1. "Highly Reduced Organometallic Complexes of Vanadium, Niobium, Tantalum and Chromium", a thesis submitted to the Faculty of the Graduate School of the University of Minnesota - by Marie Kathleen Pomije, (September 1995).
TRANSITION METAL POWDERS
FIELD OF THE INVENTION
This invention relates to a process for the production of ultra fine transition metal powders, particularly, vanadium, niobium and tantalum powders by the pyrolysis of transition metal complexes in a high boiling point inert solvent, such as a hydrocarbon or higher alkyl alcohol.
PUBLICATIONS
1. "Highly Reduced Organometallic Complexes of Vanadium, Niobium, Tantalum and Chromium", a thesis submitted to the Faculty of the Graduate School of the University of Minnesota - by Marie Kathleen Pomije, (September 1995).
2. Inorg. Chem. (1998), 37 6518-6527, - Barybim et al
3. Inorganica Chemica Acta. ( 1998), 269, 58-62 - Barybin
4. Chem. Euro. J. (1995), 1, No. 8 - Ellis et al
5. Inorg. Chem. (1983), 22, 1865-1870 - Calderazzo et al SUMMARY OF THE INVENTION
The present invention provides for the production of ultra fine transition metal complexes by the pyrolysis of the metal complex. Preferably, the heating of the metal complex is effected in a suitable inert solvent such as, for example, a hydrocarbon, alkyl alcohol, ether, diglyme, ester at an effective temperature for a sufficient period of time.
Examples of suitable metal complexes comprise carbonyl and trifluorophosphine groups wherein the metal has a valence of 0 or -1, such as [Et4N][Ta(PF3)6], [Et4N][Nb(PF3)6] and [Et4N][V(PF3)6].
Accordingly, in one aspect, the invention provides a method of preparing ultra fine metal powder comprising pyrolizing a complex metal compound of said metal, wherein said metal is in a valence state selected from 0 and 1, in an inert solvent at an effective temperature to produce said ultra fine powder, and removing said powder from said inert solvent.
Preferably, said hydrocarbon is of the formula C~HZ"+z wherein n is selected from 12 to 20.
Preferably, said alkanol is of the formula C"HZ"+~ OH wherein n is selected from 10 to 20.
We have found that the metal powder has a mean particle size of less than 10 microns, preferably 1 to 5 microns and more preferably, less than I micron.
The process of the invention is applicable to suitable metal complexes of the first, second and third transition metal series of the Periodic Table of the Elements. Most preferred are the Group VB elements, namely, vanadium, niobium and tantalum.
In a further aspect, the invention provides ultra fine metal powders produced by the processes as hereinabove defined.
In a further aspect, the invention provides for the use of the ultra fine metal powders according to the invention, particularly the use wherein the metal is tantalum in cell phones.
The metal complexes of use in the practise of the invention may be made by the reduction of salts of the metals in solution in the presence of ligand reagents, such as carbon monoxide, trifluorophosphine and naphthalene.
A two-step reductive trifluorophosphination to produce [Et4N][Ta(PF3)6], [Et4N][Nb(PF3)6] [Et4N] [V(PF3)6] has been described (1,2).
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In order that the invention may be better understood, preferred embodiments will now be described.
EXAMPLES
Cobalt carbonyl, Co2(CO)8, (lOg) was dissolved in warm toluene (20 mL) and the solution was slowly added to paraffin oil at 250 °C. The red solution immediately darkened and become black. Carbon monoxide gas and toluene vapours were evolved and removed.
After the cobalt carbonyl had decomposed, the paraffin oil was cooled, filtered and the residue washed with hexane and dried to provide sub-micron cobalt powder (3.4 g, 99 %).
Manganese carbonyl, Mn(CO)6, (5 g) was dissolved in warm acetone ( 10 mL) and added to n-hexadecanol and heated to 250 °C. Carbon monoxide gas and acetone vapours were evolved. The solution became black and after the manganese carbonyl had decomposed the n-hexadecane was cooled, filtered and the residue was washed with hexane and dried to provide sub-micron manganese powder (1.2 g, 99 %).
HTa(PF3)6 (5 g) was dispersed in paraffin oil and heated to 360 °C.
Immediate decomposition of the Ta complex was observed with evolution of hydrogen and PF3. After the complex was decomposed, the paraffin oil was cooled, filtered and the residue washed with n-hexane and dried. Sub-micron tantalum powder (1.25 g, 99 %) was obtained.
[Et4N] [Ta(PF3)6], (100g), was dissolved in acetone (50mL), added to boiling n-decanol (100mL) and stirred for 20 minutes. The black solution was filtered, and the collected powder was washed with acetone and air dried to given sub-micron tantalum powder (22g).
Although this disclosure has described and illustrated certain preferred embodiments of the invention, it is to be understood that the invention is not restricted to those particular embodiments. Rather, the invention includes all embodiments which are functional or mechanical equivalence of the specific embodiments and features that have been described and illustrated.
The present invention provides for the production of ultra fine transition metal complexes by the pyrolysis of the metal complex. Preferably, the heating of the metal complex is effected in a suitable inert solvent such as, for example, a hydrocarbon, alkyl alcohol, ether, diglyme, ester at an effective temperature for a sufficient period of time.
Examples of suitable metal complexes comprise carbonyl and trifluorophosphine groups wherein the metal has a valence of 0 or -1, such as [Et4N][Ta(PF3)6], [Et4N][Nb(PF3)6] and [Et4N][V(PF3)6].
Accordingly, in one aspect, the invention provides a method of preparing ultra fine metal powder comprising pyrolizing a complex metal compound of said metal, wherein said metal is in a valence state selected from 0 and 1, in an inert solvent at an effective temperature to produce said ultra fine powder, and removing said powder from said inert solvent.
Preferably, said hydrocarbon is of the formula C~HZ"+z wherein n is selected from 12 to 20.
Preferably, said alkanol is of the formula C"HZ"+~ OH wherein n is selected from 10 to 20.
We have found that the metal powder has a mean particle size of less than 10 microns, preferably 1 to 5 microns and more preferably, less than I micron.
The process of the invention is applicable to suitable metal complexes of the first, second and third transition metal series of the Periodic Table of the Elements. Most preferred are the Group VB elements, namely, vanadium, niobium and tantalum.
In a further aspect, the invention provides ultra fine metal powders produced by the processes as hereinabove defined.
In a further aspect, the invention provides for the use of the ultra fine metal powders according to the invention, particularly the use wherein the metal is tantalum in cell phones.
The metal complexes of use in the practise of the invention may be made by the reduction of salts of the metals in solution in the presence of ligand reagents, such as carbon monoxide, trifluorophosphine and naphthalene.
A two-step reductive trifluorophosphination to produce [Et4N][Ta(PF3)6], [Et4N][Nb(PF3)6] [Et4N] [V(PF3)6] has been described (1,2).
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In order that the invention may be better understood, preferred embodiments will now be described.
EXAMPLES
Cobalt carbonyl, Co2(CO)8, (lOg) was dissolved in warm toluene (20 mL) and the solution was slowly added to paraffin oil at 250 °C. The red solution immediately darkened and become black. Carbon monoxide gas and toluene vapours were evolved and removed.
After the cobalt carbonyl had decomposed, the paraffin oil was cooled, filtered and the residue washed with hexane and dried to provide sub-micron cobalt powder (3.4 g, 99 %).
Manganese carbonyl, Mn(CO)6, (5 g) was dissolved in warm acetone ( 10 mL) and added to n-hexadecanol and heated to 250 °C. Carbon monoxide gas and acetone vapours were evolved. The solution became black and after the manganese carbonyl had decomposed the n-hexadecane was cooled, filtered and the residue was washed with hexane and dried to provide sub-micron manganese powder (1.2 g, 99 %).
HTa(PF3)6 (5 g) was dispersed in paraffin oil and heated to 360 °C.
Immediate decomposition of the Ta complex was observed with evolution of hydrogen and PF3. After the complex was decomposed, the paraffin oil was cooled, filtered and the residue washed with n-hexane and dried. Sub-micron tantalum powder (1.25 g, 99 %) was obtained.
[Et4N] [Ta(PF3)6], (100g), was dissolved in acetone (50mL), added to boiling n-decanol (100mL) and stirred for 20 minutes. The black solution was filtered, and the collected powder was washed with acetone and air dried to given sub-micron tantalum powder (22g).
Although this disclosure has described and illustrated certain preferred embodiments of the invention, it is to be understood that the invention is not restricted to those particular embodiments. Rather, the invention includes all embodiments which are functional or mechanical equivalence of the specific embodiments and features that have been described and illustrated.
Claims (13)
1. A method of preparing ultra fine metal powder comprising pyrolizing a complex metal compound of said metal wherein said metal is in a valence state selected from 0 and 1, in an inert solvent at an effective temperature to produce said ultra fine powder, and removing said powder from said inert solvent.
2. A method as defined in claim 1 wherein said solvent is selected from the group consisting of a long chain alkyl hydrocarbon and a long chain alkyl alkanol.
3. A method as defined in claim 2 wherein said hydrocarbon is of the formula C
n H2n+2 wherein n is selected from 12 to 20.
n H2n+2 wherein n is selected from 12 to 20.
4. A method as defined in claim 2 wherein said alkanol is of the formula C n H2n+1OH
wherein n is selected from 10 to 20.
wherein n is selected from 10 to 20.
5. A method as defined in any one of claims 1 to 4 wherein said effective temperature is greater than 300°C.
6. A method as defined in any one of claims 1 to 5 wherein said powder has a mean particle size of less than 10 microns.
7. A method as defined in claim 6 wherein said mean particle size is selected from 1 to 5 microns.
8. A method as defined in any one of claims 1 to 7 wherein said metal is a transition metal.
9. A method as defined in claim 8 wherein said metal is selected from the first, second and third transition metal series of the Periodic Table of the elements.
10. A method as defined in claim 9 wherein said metal is selected from the Group VB
metals selected from V, Nb and Ta.
metals selected from V, Nb and Ta.
11. An ultra fine metal powder when made by a process as defined in any one of claims 1 to 10.
12. An ultra fine metal powder selected from the group consisting of having a mean particle size of less than 10 microns.
13. Use of an ultra fine metal powder as defined in any one of claims 1 to 12 in cell phones.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 2500077 CA2500077A1 (en) | 2005-03-09 | 2005-03-09 | Production of ultra fine transition metal powders |
| AU2005234714A AU2005234714B2 (en) | 2005-03-09 | 2005-11-21 | Production of ultra fine transition metal powders |
| ZA200509386A ZA200509386B (en) | 2005-03-09 | 2005-11-22 | Production of ultra fine transition metal powders |
| CNA2006100061551A CN1830607A (en) | 2005-03-09 | 2006-01-19 | Production of ultra fine transition metal powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 2500077 CA2500077A1 (en) | 2005-03-09 | 2005-03-09 | Production of ultra fine transition metal powders |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2500077A1 true CA2500077A1 (en) | 2006-09-09 |
Family
ID=36955299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 2500077 Abandoned CA2500077A1 (en) | 2005-03-09 | 2005-03-09 | Production of ultra fine transition metal powders |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN1830607A (en) |
| AU (1) | AU2005234714B2 (en) |
| CA (1) | CA2500077A1 (en) |
| ZA (1) | ZA200509386B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7087100B2 (en) * | 2001-01-31 | 2006-08-08 | General Electric Company | Preparation of nanosized copper and copper compounds |
| KR100867281B1 (en) * | 2001-10-12 | 2008-11-06 | 재단법인서울대학교산학협력재단 | Synthesis of Monodisperse and Highly-Crystalline Nanoparticles of Metals, Alloys, Metal Oxides, and Multi-metallic Oxides without a Size-selection Process |
| DE10227779A1 (en) * | 2002-06-21 | 2004-01-08 | Studiengesellschaft Kohle Mbh | Monodisperse, magnetic nanocolloids of adjustable size and process for their production |
-
2005
- 2005-03-09 CA CA 2500077 patent/CA2500077A1/en not_active Abandoned
- 2005-11-21 AU AU2005234714A patent/AU2005234714B2/en active Active
- 2005-11-22 ZA ZA200509386A patent/ZA200509386B/en unknown
-
2006
- 2006-01-19 CN CNA2006100061551A patent/CN1830607A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| CN1830607A (en) | 2006-09-13 |
| ZA200509386B (en) | 2008-05-28 |
| AU2005234714B2 (en) | 2007-05-24 |
| AU2005234714A1 (en) | 2006-09-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| FZDE | Dead |
Effective date: 20131218 |