Production method of iron phosphate nano powder body with controllable size and granularity

A technology of nano powder and production method, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, and can solve the problem of difficult control of material purity, different sizes of iron phosphate particles, and batches of iron phosphate Poor stability and other problems, to achieve the effect of reflecting low requirements, high product utilization rate and high yield

Inactive Publication Date: 2013-04-03
山东天润丰新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ferric phosphate produced by the above method has different particle sizes, the mate

Method used

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  • Production method of iron phosphate nano powder body with controllable size and granularity
  • Production method of iron phosphate nano powder body with controllable size and granularity
  • Production method of iron phosphate nano powder body with controllable size and granularity

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Take 75mL of ultrapure water to dissolve 0.4mol phosphoric acid and 0.1mol disodium hydrogen phosphate, adjust the pH of the solution to 4.0 with 5M sodium hydroxide and concentrated phosphoric acid solution, and finally obtain 100mL of 5mol / L phosphate base solution A 1 . Prepare 2mol / L ferric nitrate solution B 1 .

[0060] 100mL A 1 Place in a three-necked bottle and heat at a constant temperature of 90°C in an oil bath. After the temperature of the solution in the three-necked bottle is stable, quickly dissolve 150mL 1 , 2g of glucose, and 1g of tapioca starch were added to A 1 , mechanically stirred evenly, then slowly added 100mL B at 10mL / min 1 solution, adjust the pH of the solution to 3.0. After the dropwise addition, the three-neck flask was stirred at a constant temperature of 90°C in a water bath for 60 minutes, and the obtained ferric phosphate precipitate was washed with deionized water and centrifuged 4 times. The precursor was dried at 120°C for 1 ...

Embodiment 2

[0062] Mix ultrapure water and ethylene glycol at a ratio of 3:1, take 75mL of mixed solvent to dissolve 0.3mol phosphoric acid and 0.3mol disodium hydrogen phosphate, adjust the pH of the solution to 5.0 with 5M sodium hydroxide solution and concentrated phosphoric acid, and obtain 100mL of 6mol / L Phosphate base solution A 2 . Prepare 4mol / L ferric chloride aqueous solution B 2 .

[0063] 100mL A 2 Put it in a three-necked bottle and heat it in a 90°C oil bath. After the temperature of the solution in the three-necked bottle is stable, quickly add 100mL of B 2 Add to A together with 2g maltose and 1g SDBS 2 , mechanically stirred evenly, then slowly added 100mL B at 10mL / min 1 solution, adjust the pH of the solution to 3.0. Stir at a constant temperature of 90° C. for 120 minutes, and the obtained ferric phosphate precipitate is washed with deionized water and centrifuged 4 times. The precursor was dried at 120°C for 1 hour, and the resulting powder was subjected to a...

Embodiment 3

[0065] Mix ultrapure water and ethylene glycol at 3:1, take 80mL of mixed solvent to dissolve 0.2mol phosphoric acid and 0.4mol disodium hydrogen phosphate, adjust the pH of the solution to 5.0 with 5M sodium hydroxide solution and concentrated phosphoric acid, and obtain 100mL of 6mol / L Phosphate base solution A 3 . Prepare 3mol / L ferric nitrate aqueous solution B 3 .

[0066] 100mL A3 Put it in a three-necked bottle and heat it in a 90°C oil bath. After the temperature of the solution in the three-necked bottle is stable, quickly add 100mL of B 3 , 1g soluble starch, 1g fructose, 1g CTAB were added to A 3 , mechanically stirred evenly, then slowly added 50mL of B at a rate of 10mL / min 3 solution, adjust the pH of the solution to 3.5. Stir at constant temperature at 90° C. for 60 minutes, and the obtained precipitate is washed with deionized water and centrifuged 4 times. The precursor was dried at 120°C for 1 hour, and the obtained powder was subjected to constant tem...

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Abstract

The invention discloses a production method of an iron phosphate nano powder body with controllable size and granularity. The production process of battery level iron phosphate has the defects of slightly large size, impure phase, complex process, high production cost and the like generally; and especially, a defined proportion of crystal water is carried in the phase, which directly causes phase, performance and the like of the post-synthesized lithium iron phosphate powder body to be instable. The synthetic process provided by the invention comprises the steps of: preparing a phosphate organic/pure water mixed base solution within a certain pH range; adding multiple additives; adding an iron salt solution by steps at a constant temperature; regulating pH of the solution in a dropping process; stirring for a certain time at a constant temperature; and filtering, washing and washing a product and finally annealing a temperature of 300-600 DEG C for a period of time to obtain the iron phosphate nano powder body. The iron phosphate nano powder body produced by adopting the method has the advantages of controllable size and components, simple process, low cost, high powder body activity and great market competitiveness, and is easy to produce on large scale.

Description

technical field [0001] The invention belongs to the field of positive electrode materials of lithium ion batteries, and in particular relates to a production method of iron phosphate nano powder. Background technique [0002] As a kind of clean energy, lithium-ion battery has received extensive attention and development in recent years, and has been widely used in mobile phones, notebook computers and electric tools. The "New Energy Vehicle Demonstration Promotion Notice" and other relevant policies vigorously develop new energy vehicles and supporting related technologies. Lithium iron phosphate, as the positive electrode material of lithium-ion batteries, has high mass specific capacity (170mAh / g), stable working voltage (3.5V voltage platform), stable crystal structure, and excellent overcharge resistance. In particular, high-power batteries have outstanding advantages, and the raw materials of the products have a wide range of sources, low prices, and no environmental p...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y30/00
Inventor 杨立山丁轶
Owner 山东天润丰新能源科技有限公司
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