Spherical micro-nano ferric phosphate/carbon composite material and preparation method thereof

A carbon composite material, micro-nano technology, applied in the field of lithium-ion batteries, can solve the problems of ineffective material modification, uncontrollable mixing degree of reaction raw materials, immaturity, etc.

Active Publication Date: 2016-03-30
ENERGY RES INST OF SHANDONG ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Spherical lithium iron phosphate micro-nanostructure materials meet the design requirements of high energy density and high rate performance lithium-ion batteries, but most of the existing technologies directly use iron salts, phosphates, and carbon materials as raw materials to prepare lithium iron phosphate. On the one hand, the mixing degree of the reaction raw materials is uncontrollable, on the other hand, t

Method used

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  • Spherical micro-nano ferric phosphate/carbon composite material and preparation method thereof
  • Spherical micro-nano ferric phosphate/carbon composite material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0026] Weigh equimolar Fe(NO 3 ) 3 ·9H 2 O and H 3 PO 4 Prepare a 0.2mol / L mixed acid solution, measure a certain amount of ammonia and dilute to 0.5mol / L, and input the two into the crystallization reactor in parallel and continuously. The reaction temperature is 50°C, and the pH of the reaction system is adjusted and maintained at about 2 to control The stirring intensity is 200r / s, and the reaction solution overflows naturally after filling the reactor. After stirring for 10 hours, it is centrifuged, washed and dried to obtain FePO. 4 ·XH 2 O powder. The precursor powder is heat-treated at 500℃ for 10h to obtain nano-FePO 4 Precursor, using carbothermic reduction method to prepare nano-LiFePO 4 / C Cathode material. Weigh 12g FePO 4 Precursor, 2.982g Li 2 CO 3 Add 2.5g of sucrose and 5ml of deionized water to mix well, put it in a tube furnace, pass in high-purity nitrogen, heat treatment at 700℃ for 16h, and obtain nano-LiFePO after high-temperature carbothermic reduction rea...

Embodiment 2

[0028] Weigh equimolar Fe(NO 3 ) 3 ·9H 2 O and H 3 PO 4 Make 0.2mol / L mixed acid solution, weigh FePO 4 After 0.5wt% of the theoretical mass of polyacrylamide is dissolved in the acid solution, a certain amount of ammonia is diluted to 0.5mol / L, and the two are continuously fed into the controlled crystallization reactor in parallel. The reaction temperature is 50°C, and the reaction system is adjusted and maintained. The pH is around 2, and the stirring intensity is controlled to 200r / s. The reaction solution overflows naturally after filling the reactor. After stirring for 10 hours, it is centrifuged, washed and dried to obtain 0.5wt% PAM-FePO 4 ·XH 2 O powder. PAM-FePO is obtained after heat treatment of the precursor powder at 500℃ for 10h 4 Precursor, prepare nano LiFePO modified by PAM according to the method of Example 1. 4 / C Cathode material. Such as figure 1 As shown, the PAM-FePO obtained in this example 4 The particle D50 is 4.3um, the carbon content is 4.4028%, and ...

Embodiment 3

[0030] Weigh equimolar Fe(NO 3 ) 3 ·9H 2 O and H 3 PO 4 Make 0.2mol / L mixed acid solution, weigh FePO 4 After the theoretical mass of 0.5wt% soluble starch is dissolved in the acid solution, measure a certain amount of ammonia to dilute to 0.5mol / L, and input the two in parallel and continuously into the controlled crystallization reactor. The reaction temperature is 50℃, and the pH of the reaction system is adjusted and maintained. At about 2, control the stirring intensity to 200r / s, and the reaction liquid will overflow naturally after filling the reactor. After stirring for 1 hour, after centrifugation, washing and drying, 0.5wt% soluble starch-FePO is obtained. 4 ·XH 2 O powder. The precursor powder is heat-treated at 600℃ for 10h to obtain spherical micro-nano FePO 4 Precursor, according to the method of Example 1 to prepare micro-nano LiFePO modified with soluble starch 4 / C Cathode material. Such as figure 1 As shown, the soluble starch-FePO obtained in this example 4 Th...

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Abstract

The invention discloses a spherical micro-nano ferric phosphate/carbon composite material and a preparation method thereof. The preparation method comprises the following steps: (1) preparing aqueous solution of ferric salt and a phosphorous compound, wherein the mole ratio of the ferric element to the phosphorus element is (0.9-1.2): 1, and the solution concentration is 0.2-5 mol/L; (2) dispersing a high polymer material binder in the solution in the step (1), wherein the dosage of the high polymer material binder is 0.5-90 wt/% of the ferric salt; (3) adding the solution prepared in the step (2) into a reaction still, continuously adding alkali solution to ensure that the pH in the reaction still is kept in 2-4, and reacting at a temperature of 20-90DEG C for 1-60 hours to obtain a crystal water-containing spherical micro-nano ferric phosphate/carbon composite material; and (4) under an inert atmosphere, roasting the spherical micro-nano ferric phosphate/carbon composite material prepared in the step (3) at a temperature of 300-800DEG C for 3-12 hours, and cooling to obtain the product. According to the preparation method, the coating of carbon materials is realized, and a crucial role is played in subsequently preparing high-density high-performance lithium ion battery LiFePO4 anode materials.

Description

Technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular a spherical micro-nano iron phosphate / carbon composite material and a preparation method thereof. Background technique [0002] Iron Phosphate (FePO 4 ) Is a monoclinic crystal with a white or off-white powder appearance. It was initially widely used in agriculture, ceramic glass, steel and surface passivation, and later research found FePO 4 It also has applications in the fields of oxidative dehydrogenation catalysis, ion exchange and electrochemical performance. In the application of electrochemistry, FePO 4 Can be used as LiFePO for preparing lithium ion batteries 4 The framework material of the cathode material. Research shows that using FePO 4 Preparation of LiFePO as a precursor 4 Cathode materials have the following advantages: (1) FePO 4 Has a fixed Fe / P ratio, so it is easier to obtain pure LiFePO 4 Cathode material; (2) FePO 4 And LiFePO 4 Has a similar crystal s...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/583H01M4/139H01M10/0525
CPCH01M4/139H01M4/366H01M4/5825H01M4/583H01M10/0525Y02E60/10
Inventor 杨改秦显忠高剑蔡飞鹏蒋波王波谭春晖
Owner ENERGY RES INST OF SHANDONG ACAD OF SCI
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