Electrode material and method of synthesizing

Patent metadata

Field	Value
Publication number	US-10090516-B2
Application number	US-201314395921-A
Country	US
Kind code	B2
Filing date	Apr 23, 2013
Priority date	Apr 24, 2012
Publication date	Oct 2, 2018
Grant date	Oct 2, 2018

Abstract

The present disclosure provides a phosphate framework electrode material for sodium ion battery and a method for synthesizing such electrode material. A surfactant and precursors including a sodium precursor, a phosphate precursor, a transition metal precursor are dissolved in a solvent and stirred for sufficient mixing and reaction. The precursors are reacted to yield a precipitate of particles of Na x A b M y (PO 4 ) z X n compound and with the surfactant attached to the particles. The solvent is then removed and the remaining precipitate is sintered to crystallize the particles. During sintering, the surfactant is decomposed to form a carbon network between the crystallized particles and the crystallized particles and the carbon matrix are integrated to form the electrode material.

First claim

The invention claimed is:

1. A method for synthesizing an electrode material, the method comprising:
preparing a precipitate of particles by a step consisting of dissolving a surfactant, a sodium precursor, a phosphate precursor and a transition metal precursor in a solvent to cause reaction of the sodium, phosphate and transition metal precursors to yield the precipitate of particles, wherein the surfactant is attached to the particles;
removing the solvent; and
sintering the precipitate to crystallize the particles,
wherein during sintering the surfactant is decomposed to form a carbon matrix between the crystallized particles;
wherein the crystallized particles and the carbon matrix are integrated to form the electrode material;
wherein the crystallized particles have a grain size between 20 nm and 200 nm; and
wherein the particles include Na 3 V 2 (PO 4 ) 3 .

2. The method of claim 1 , wherein the surfactant is selected from the group consisting of sodium dodecyl sulfate (SDS), octyltrimethyl ammonium bromide (OTAB), dodecyltrimethyl ammonium bromide (DOTAB), cetyltrimethyl ammonium bromide (CTAB), and gluconic acid lactone.

3. The method of claim 1 , wherein the sodium precursor is a sodium salt.

4. The method of claim 1 , wherein the phosphate precursor is an ammonium phosphate salt or a phosphoric acid.

5. The method of claim 1 , wherein the solvent is one of alcohol and a mixture of de-ionized water and alcohol.

6. The method of claim 1 , wherein the transitional metal precursor is selected from a metal acetate, metal nitrate, metal chloride, metal acetyl acetonate, metal hydroxide, and combinations thereof.

7. The method of claim 1 , wherein the carbon matrix forms a carbon layer coated on the crystallized particles, and wherein the carbon layer has a thickness of 2 to 10 nm.

8. The method of claim 1 , wherein removing the solvent consists of drying the precipitate.

9. The method of claim 1 , wherein sintering is carried out in one of a flowing oxidizing atmosphere, an inert atmosphere and a reducing atmosphere.

10. The method of claim 1 , wherein removing the solvent consists of separating the precipitate from the solvent.

11. A method for synthesizing an electrode material, the method comprising:
preparing a precipitate of particles by a step consisting of dissolving a surfactant, a sodium precursor, a phosphate precursor, a transition metal precursor, and a compound having fluorine in a solvent to cause reaction of the sodium, phosphate and transition metal precursors to yield the precipitate of particles, wherein the surfactant is attached to the particles;
removing the solvent; and
sintering the precipitate to crystallize the particles,
wherein during sintering the surfactant is decomposed to form a carbon matrix between the crystallized particles;
wherein the crystallized particles and the carbon matrix are integrated to form the electrode material;
wherein the crystallized particles have a grain size between 20 nm and 200 nm; and
wherein the particles include Na 3 V 2 (PO 4 ) 2 F 3 and NaVPO 4 F.

12. A method for synthesizing an electrode material, the method comprising:
preparing a precipitate of particles by a step consisting of dissolving a surfactant, a sodium precursor, a phosphate precursor, a transition metal precursor, and a compound having manganese in a solvent to cause reaction of the sodium, phosphate and transition metal precursors to yield the precipitate of particles, wherein the surfactant is attached to the particles;
removing the solvent; and
sintering the precipitate to crystallize the particles,
wherein during sintering the surfactant is decomposed to form a carbon matrix between the crystallized particles;
wherein the crystallized particles and the carbon matrix are integrated to form the electrode material;
wherein the crystallized particles have a grain size between 20 nm and 200 nm; and
wherein the particles include Na 2 V 0.5 Mn 0.5 PO 4 F.

Assignees

• Nat Univ Singapore

Inventors

• Balaya Palani
• Kuppan Saravanan
• Liu Bing
• Mason Chad William

Classifications

• H01M4/1397

  of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy · CPC title

• H01M10/054

  Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium · CPC title

• H01M4/364 Primary

  as mixtures · CPC title

• H01M4/133

  Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx · CPC title

• H01M4/60

  of organic compounds · CPC title