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Preparation method for nanometer oxide doped with boric acid ferrous lithium cathode materials

A technology of nano-oxide and lithium iron borate, which is applied in the direction of boron oxides, borates, battery electrodes, etc., can solve the problems of unsatisfactory performance and achieve low cost, good rate performance, and short process.

Inactive Publication Date: 2014-11-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, V.Aravindan et al. prepared carbon-coated cathode material LiFeBO with fatty acid as carbon source. 3 / C(Aravindan V, Umadevi M. Synthesis and characterization of novel LiFeBO 3 / C cathodes for lithium batteries[J]. Ionics, 2012, 18(1-2): 27-30), the first discharge specific capacity of the prepared material is only 93mAh g at 1 / 20C rate -1 , decayed to 53mAh g after 30 cycles -1 , the performance is still not ideal

Method used

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  • Preparation method for nanometer oxide doped with boric acid ferrous lithium cathode materials
  • Preparation method for nanometer oxide doped with boric acid ferrous lithium cathode materials
  • Preparation method for nanometer oxide doped with boric acid ferrous lithium cathode materials

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Embodiment 1

[0020] This embodiment includes the following steps:

[0021] (1) Prepare the precursor: mix lithium carbonate, iron nitrate, nano-nickel oxide, boric acid, and glucose according to the ratio of atomic molar ratio Li:Fe:Ni:B:C=1.04:0.9:0.1:1:1.5, Put it into a ball mill tank, add absolute ethanol to immerse the raw material, use a ball mill to mechanically mill for 3 hours at room temperature at a speed of 200r / min, and then dry it in an oven at 60°C for 12 hours to obtain a powdery precursor;

[0022] (2) The powdery precursor obtained in step (1) was sintered at 500°C for 15 hours in a nitrogen atmosphere, and cooled naturally to room temperature to obtain the nano-nickel oxide-doped lithium iron borate cathode material.

[0023] The SEM image of the nano-nickel oxide doped lithium iron borate cathode material obtained in this example is shown in figure 1 . The obtained nano-nickel oxide-doped lithium ferrous borate positive electrode material is used as the positive elect...

Embodiment 2

[0026] This embodiment includes the following steps:

[0027] (1) Preparation of precursor: Lithium nitrate, ferric chloride, nano-magnesium oxide, ammonium borate, and citric acid are prepared according to the atomic molar ratio Li:Fe:Mg:B:C=1:0.99:0.01:1:2.5 Mix evenly, put it into a ball mill jar, add absolute ethanol to immerse the raw material, use a planetary ball mill for 7 hours at room temperature at a speed of 150r / min, and then place it in an oven at 120°C for 6 hours to obtain a powdery precursor;

[0028] (2) The powdery precursor obtained in step (1) was sintered at 700° C. for 1 h in an argon atmosphere, and cooled naturally to room temperature to obtain the nano-magnesium oxide-doped lithium iron borate cathode material.

[0029] The obtained nano-magnesium oxide doped with lithium ferrous borate was used as the positive electrode material, and the metal lithium sheet was used as the negative electrode material, and assembled into a CR2025 button battery in a g...

Embodiment 3

[0032] This embodiment includes the following steps:

[0033] (1) Prepare the precursor: mix lithium metaborate, ferric oxide, nano-cadmium oxide, and tartaric acid according to the atomic molar ratio Li:Fe:Cd:B:C=1:0.93:0.07:1:1.5 , put it into a ball mill tank, add absolute ethanol to immerse the raw material, use a planetary ball mill to mechanically mill for 4 hours at a speed of 250r / min at room temperature, and then place it in an oven for 10 hours at 100°C to obtain a powdery precursor;

[0034] (2) Place the powdery precursor obtained in step (1) in an argon-hydrogen mixture (volume ratio: hydrogen / argon = 1:9) and sinter at 400°C for 7 hours, then cool naturally to room temperature to obtain nano-cadmium oxide doping Lithium iron borate cathode material.

[0035] The obtained nano-cadmium oxide-doped lithium iron borate is used as the positive electrode material, and the metal lithium sheet is used as the negative electrode material, and assembled into a CR2025 butto...

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Abstract

The invention provides a preparation method for nanometer oxide doped with boric acid ferrous lithium cathode materials. The method comprises the following steps that (1) an lithium source, an iron lithium, nanometer oxide MxOy, a boron source and a carbon source are evenly mixed according to the molar ratio of Li, Fe, M, B and C: (1-1.04):(0.99-0.9):(0.01-0.1):1(0.5-2.5) and put into a milling tank, absolute ethyl alcohol is added to immerse raw materials, the mixture is subjected to mechanical milling through a milling machine at the 150-250 r / min rotating speed at the normal temperature for 3 hours to 7 hours and then transferred to a baking oven to be baked for 6 hours to 12 hours at 60 DEG C to 120 DEG C, and powder-like precursors are obtained; (2) the precursors are placed in an inoxidizability atmosphere, are subjected to heat treatment for 1 hour to 20 hours at 400 DEG C to 700 DEG C and then are cooled naturally to the room temperature, and the nanometer oxide doped with boric acid ferrous lithium materials are obtained. The preparation method is simple in operation, short in process and low in cost, and the prepared boric acid ferrous lithium of cathode materials for lithium ion cells is good in circulation performance and rate performance.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material of a lithium ion battery, in particular to a preparation method of a nanometer oxide-doped lithium ferrous borate positive electrode material. Background technique [0002] LiFeBO 3 It is a new type of lithium-ion battery cathode material, which has a high theoretical specific capacity (220mAh g -1 ), good conductivity, very small volume change rate (≤2%), at the same time, borate (BO 3 ) 3- Has a small molar mass (58.8), much smaller than the same kind of phosphate (PO 4 ) 3- Polyanion (95), and its structure can provide lithium ion conduction and electron conduction at the same time, so it has become a hot spot of recent research. At the same time, the content of iron in the earth's crust is very high, ranking fourth after oxygen, silicon, and aluminum, with an abundance of 4.75%. my country is also a country with large iron resources, and the proven reserves of iron ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12H01M4/58H01M4/62
CPCY02E60/10
Inventor 郑俊超明磊张宝张佳峰沈超韩亚东
Owner CENT SOUTH UNIV