Phosphorus-doped nickel nanoparticle and method of manufacturing the same

Patent metadata

Field	Value
Publication number	US-9339870-B2
Application number	US-201214363011-A
Country	US
Kind code	B2
Filing date	Dec 4, 2012
Priority date	Dec 9, 2011
Publication date	May 17, 2016
Grant date	May 17, 2016

Abstract

The present invention provides a method of manufacturing a phosphorus-doped nickel nanoparticle. The method includes the steps of: mixing a nickel solution including a nickel compound and a solvent, a seed particle, and a phosphorus-containing reductant in an arbitrary order to prepare a mixed solution; and adjusting pH of the mixed solution such that the mixed solution becomes acidic. According to the method, a phosphorus-doped nickel nanoparticle that is suitable to be applied to solar cell electrodes requiring low contact resistance can be manufactured.

First claim

The invention claimed is:

1. A method of manufacturing a phosphorus-doped nickel nanoparticle, comprising the steps of:
mixing a nickel solution including a nickel compound and a solvent, a seed particle, and a phosphorus-containing reductant in an arbitrary order to prepare a mixed solution; and
adjusting pH of the mixed solution to 4 to 6,
wherein the pH in the early stage of the mixed solution reaction is lower than in the latter stage.

2. The method of claim 1 , wherein the seed particle is a transition metal including one or more selected from the group consisting of Pd, Cu, Ru, Pt, Ag and Co.

3. The method of claim 1 , wherein the seed particle is prepared by adding a reductant to a transition metal solution including a transition metal compound, ultra-pure water and a high boiling point alcohol of 2 to 10 carbon atoms and then recovering a transition metal from the transition metal solution.

4. The method of claim 3 , wherein the transition metal solution has a concentration of 0.01 to 100 g/L.

5. The method of claim 1 , wherein the nickel solution includes a nickel compound, ultra-pure water, and a high boiling point alcohol of 2 to 10 carbon atoms.

6. The method of claim 5 , wherein the nickel compound is at least one selected from the group consisting of nickel chloride (NiCl 2 ), nickel sulfate (NiSO 4 ), nickel acetate (Ni(OCOCH 3 ) 2 ), nickel acetylacetonate (Ni(C 5 H 7 O 2 ) 2 ), nickel halide (NiX 2 , where X is F, Br, or I), nickel carbonate (NiCO 3 ), nickel cyclohexanebutyrate ([C 6 H 11 (CH 2 ) 3 CO 2 ] 2 Ni), nickel nitrate (Ni(NO 3 ) 2 ), nickel oxalate (NiC 2 O 4 ), nickel stearate (Ni(H 3 C(CH 2 ) 16 CO 2 ) 2 ), nickel octanoate ([CH 3 (CH 2 ) 6 CO 2 ] 2 Ni), and hydrates thereof.

7. The method of claim 5 , wherein the high boiling point alcohol is at least one selected from the group consisting of 1-heptanol, 1-octanol, decanol, ethylene glycol, propylene glycol, triethylene glycol, and diethylene glycol.

8. The method of claim 1 , wherein, in the step of mixing the nickel solution including a nickel compound and a solvent, the seed particle and the phosphorus-containing reductant in an arbitrary order, a surface tension depressing compound is further mixed.

9. The method of claim 8 , wherein the surface tension depressing compound is at least one selected from the group consisting of polyethylene glycol having a molecular weight of 200 to 20,000, polyvinyl pyrrolidone having a molecular weight of 500 to 400,000, polyalkylene alkyl ether, and polyalkylene alkylethyl.

10. The method of claim 1 , wherein the phosphorus-containing reductant is at least one selected from the group consisting of ammonium dihydrogen phosphate, sodium hypophosphite, sodium hypophosphate, and sodium hexametaphosphate.

11. The method of claim 1 , wherein the step of mixing the nickel solution including a nickel compound and a solvent, the seed particle and the phosphorus-containing reductant in an arbitrary order is performed at a temperature of 80 to 150° C.

12. The method of claim 1 , wherein the step of adjusting the pH of the mixed solution is performed by adding at least one pH adjuster selected from the group consisting of citric acid, oxalic acid, acetic acid, and sodium or potassium salts thereof.

13. A phosphorus-doped nickel nanoparticle, manufactured by the method of claim 1 .

14. The phosphorus-doped nickel nanoparticle of claim 13 , wherein the phosphorus-doped nickel nanoparticle has an average particle size of 5 to 200 nm.

15. The phosphorus-doped nickel nanoparticle of claim 13 , wherein the phosphorous is included in an amount of 1 to 25 wt % based on a total amount of the phosphorus-doped nickel nanoparticle.

16. A phosphorus-doped nickel nanoparticle, comprising:
a seed particle; and
a nickel layer formed on the seed particle and doped with phosphorus,
wherein the phosphorus-doped nickel nanoparticle has a nanosized diameter,
wherein the phosphorus-doped nickel nanoparticle has an average particle size of 5 to 200 nm.

17. The phosphorus-doped nickel nanoparticle of claim 16 , wherein the seed particle includes one or more selected from the group consisting of Pd, Cu, Ru, Pt, Ag and Co.

18. The phosphorus-doped nickel nanoparticle of claim 16 , wherein the phosphorous is included in an amount of 1 to 25 wt % based on a total amount of the phosphorus-doped nickel nanoparticle.

Assignees

• Hanwha Chemical Corp

Inventors

• Son Won Il
• Sim You-Jin
• Kim Eui-Duk

Classifications

• B22F1/054

  Nanosized particles · CPC title

• B22F1/102

  Metallic powder coated with organic material · CPC title

• B22F1/056

  Submicron particles having a size above 100 nm up to 300 nm · CPC title

• B22F1/103

  containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent · CPC title

• B22F1/17

  Metallic particles coated with metal · CPC title