Continuous hydrothermal synthetic method for lithium ion cell nano anode material

A technology for lithium ion batteries and cathode materials, applied in the field of energy material preparation, can solve the problems of large particle size of materials, cumbersome preparation steps, time-consuming and the like, and achieve the effects of high electrochemical activity, simple process flow, and strong operability

Inactive Publication Date: 2007-08-15
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Li Wei etc. adopt solid-phase synthesis method (Chinese patent, publication number CN1821064, the method for preparing high-density lithium iron phosphate by microwave heating) spherical high-density ferrous ammonium phosphate and lithium acetate are uniformly mixed with molar ratio 1: 1, add appropriate amount of carbon Source, drying, pressing, heating and calcining to obtain spherical lithium iron phosphate; although this method is simple to operate and convenient for industrial production, the reaction time is long, the material prepared at high temperature has a large particle size, and the mixing is uneven, and the electrochemical activity is insufficient; Zhu Bingquan et al. adopted the co-precipitation method ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Configure 0.02M LiOH, 0.02 M Fe(CH 3 COO) 2 , 0.02M NH 2 HPO 4 According to the volume ratio of 1:1:1, the raw material liquid is continuously injected into the high-temperature and high-pressure reactor through three syringe pumps respectively, so that the raw material liquid is mixed, and the temperature of the reactor is controlled at 374 ° C, the reaction pressure is 50 MPa, and the mixing reaction time is 1 min. , hydrothermal crystallization of the mixed solution to obtain the product solution. Then the product liquid is directly sprayed into the low-pressure flash chamber equipped with a cyclone separator connected to the high-temperature and high-pressure reactor through the pipeline of the reactor outlet. The temperature of the flash chamber is controlled at 80°C and the pressure is 104Pa. The water in the liquid is quickly vaporized into water vapor, and is discharged through the top of the cyclone separator, while the solid particles settle at the bottom o...

Embodiment 2

[0019] Prepare 0.02M LiCH 3 COO, 0.02 M FeSO 4 , 0.02M NH 3 PO 4 According to the volume ratio of 1:1:1, three injection pumps are respectively used to inject the raw material liquid continuously into the high temperature and high pressure reactor, so that the raw material liquid is mixed. Control the temperature of the reactor to 600° C., the reaction pressure to 25 MPa, and the mixing reaction time to 4 minutes to hydrothermally crystallize the mixed liquid to obtain the product liquid. Then the product liquid is directly sprayed into the low-pressure flash chamber equipped with a cyclone separator connected to the high-temperature and high-pressure reactor through the pipeline of the reactor outlet. The water in the liquid is quickly vaporized into water vapor and discharged through the top of the cyclone separator, while the solid particles settle at the bottom of the flash chamber, and finally the dry powder product is collected, with a particle size of 10-20nm. Electr...

Embodiment 3

[0021] Configure 0.02M LiCH 3 COO, 0.02 M FeSO 4 , 0.002M MgCl 2 , 0.02M H 3 PO 4 solution, and then MgCl 2 Prepare a doped and modified iron source solution with FeSO4 solution at a volume ratio of 0.98:0.02, and then continuously pump the raw material solution into a high-temperature and high-pressure reactor through three syringe pumps to mix the raw material solution. The temperature of the reactor is controlled to be 300° C., the reaction pressure is 30 MPa, the mixing reaction time is 1 h, and the mixed liquid is hydrothermally crystallized to obtain the product liquid. Then the product liquid is directly sprayed into a low-pressure flash chamber equipped with a cyclone separator connected to the high-temperature and high-pressure reactor through the outlet pipe of the reactor. The temperature of the flash chamber is 100 ° C and the pressure is 4 × 10 4 Pa, the water in the product liquid in the flash chamber is quickly vaporized into water vapor, and is discharged ...

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Abstract

The invention discloses a continual hydrothermal synthesizing method of lithium ion battery nanometer anode, which comprises the following steps: adopting continual hyper (sub) clinical hydrothermal synthetic technique to make nanometer graded LiFePO4 particle through hypercritical flow transfer mass and crystallizing elementary; adding conductive material to make electrode material; spraying the product liquid into low-pressure flashing room with cyclone separator directly; gasifying water in the flashing room into steam; draining out from the top of cyclone separator; sedimenting solid particle on the bottom of flashing room; collecting dry powder as product.

Description

technical field [0001] The invention relates to a continuous hydrothermal synthesis method of nanometer cathode materials for lithium-ion batteries, which mainly adopts super (sub) critical hydrothermal crystallization synthesis technology to obtain lithium ferrous phosphate (LiFePO 4 ) and its modified lithium-ion battery cathode material nanoparticles. The invention belongs to the technical field of energy material preparation. Background technique [0002] Since the commercialization of lithium-ion batteries, cathode materials have always been a research hotspot in the field of batteries. Among them, LiCoO, the cathode material for lithium-ion batteries that has been industrialized 2 It pollutes the environment and is expensive, which greatly limits its future development. Lithium iron phosphate (LiFePO) with olivine structure 4 ) as a new type of lithium-ion battery cathode material has the advantages of wide material sources, low price, high theoretical specific cap...

Claims

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Application Information

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IPC IPC(8): C01B25/45B22F9/00B82B3/00H01M4/04H01M4/58
CPCY02E60/10Y02P20/54
Inventor 于文利
Owner SHANGHAI JIAO TONG UNIV
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