CN108470896B - Lithium ion battery cathode material and preparation method thereof - Google Patents
Lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN108470896B CN108470896B CN201810239761.0A CN201810239761A CN108470896B CN 108470896 B CN108470896 B CN 108470896B CN 201810239761 A CN201810239761 A CN 201810239761A CN 108470896 B CN108470896 B CN 108470896B
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a lithium ion battery cathode material and a preparation method thereof. The invention firstly adopts an ultrasonic dispersion mode to obtain a carbon nano tube suspension, and then uses citric acid as a compatilizer and ammonium carbonate as a regulator to enable Fe to be heated3+、Co2+Depositing the hydroxide on the surface of the carbon nano tube, and finally preparing CoFe through pre-oxidation and calcination2O4-MWNTs composite material. Compared with the prior art, the invention has the following advantages: firstly, the carbon nano tube is used as a supporting framework, so that the structural stability of the material is improved; the carbon nano tube has good conductivity, so that the impedance of the material is reduced, and the overall performance of the material is improved; thirdly, the cobalt ferrite with the spinel structure has good circulation stability in the charging and discharging processes; fourthly, the preparation process is simple, safe and efficient.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a lithium ion battery cathode material and a preparation method thereof.
Background
With the continuous development of society and the advancement of technology, electronic products and electric devices are widely applied in our daily life, and these applications are inseparable from the rapid development of lithium ion battery technology. How to prepare more stable, higher capacity, cheaper and more environmentally friendly lithium ion batteries has always been the direction of research by scientists. The lithium ion battery cathode material is the focus of research, and the current commercialized lithium ion battery cathode material has only 372 mAh g of graphite theoretical capacity-1And the requirement of people on high energy storage batteries cannot be met. Silicon-based, tin-based and transition metal oxides and other negative electrode materials have been the content of research of scientists due to their larger theoretical specific capacity. Wherein, the transition metal oxide (M)xOyM = Fe, Co, Mn, Cu or Ni as the lithium ion battery cathode material has higher theoretical specific capacity (-1000 mAh.g)-1). However, the first coulombic efficiency of the material is low, resulting in fast capacity fade, poor conductivity and large volume expansion during charge and discharge cycles, which seriously affect the cycle stability and cycle life of the battery. Modification of materials is an inevitable approach to solving the above problems. One method is the compounding of the materials, and the synergistic effect among different metals or metal oxides is beneficial to improving the overall performance of the materials; the second method is to coat the material with a carbon shell, wherein the carbon shell can enhance the conductivity of the electrode material, accommodate the huge volume change of the material and improve the capacity retention rate of the material; the third method is to improve the morphology of the material, and the morphology improvement mainly comprises a nano structure, a core-shell structure, a micro structure and a porous structure so as to enhance the electrochemical performance of the material. The carbon nanotube has excellent properties such as light weight, high electrical conductivity, and high mechanical strength due to its unique hollow tubular structure. Therefore, the carbon nano tube is used as a framework to be compounded with the transition metal oxide to prepare the composite cathode material with the reinforced concrete structure, and the composite cathode material has a positive effect on improving the electrochemistry of the material.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a lithium ion battery cathode material and a preparation method thereof, and aims to solve the problems that the prior material has low coulombic efficiency for the first time, so that the capacity attenuation is fast, the poor conductivity and the large volume expansion in the charge-discharge cycle process seriously affect the cycle stability and the cycle life of the battery.
The technical scheme of the invention is as follows:
a preparation method of a lithium ion battery negative electrode material comprises the following steps:
(1) preparation of Fe (OH)x-Co(OH)yMWNTs precursors: firstly, putting carbon nano tubes into water for ultrasonic dispersion, then adding ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid in sequence under the condition of stirring to completely dissolve the carbon nano tubes to obtain a mixed solution, and then adding the mixed solution into the water for ultrasonic dispersionDrying the mixed solution at 80-100 ℃ for 24 hours to obtain Fe (OH)x-Co(OH)y-MWNTs precursors; wherein x =2 or 3, y = 2;
(2) preparation of carbon nanotube-based CoFe2O4MWNTs composite: mixing Fe (OH)x-Co(OH)yReacting the MWNTs precursor at 180 ℃ and 200 ℃ for 2-3h for pre-oxidation, grinding the pre-oxidized precursor into powder, calcining at 330 ℃ and 350 ℃ for 2-3h, and preparing the CoFe with the carbon nano tube as the framework2O4-MWNTs composite material, CoFe with carbon nanotube as skeleton2O4The MWNTs composite material is the lithium ion battery negative electrode material.
The preparation method of the lithium ion battery cathode material comprises the following steps of (1) preparing a lithium ion battery cathode material, wherein in the step (1), the molar ratio of ferric nitrate to cobalt nitrate to ammonium carbonate to citric acid is 4:2 (1-1.5): (1-1.5).
The preparation method of the lithium ion battery cathode material comprises the following step of mixing ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid in a molar ratio of 4:2:1: 1.
The preparation method of the lithium ion battery cathode material comprises the step (1) of placing the carbon nano tube into water for ultrasonic dispersion for 30 minutes.
The preparation method of the lithium ion battery negative electrode material comprises the step (1) of drying the mixed solution at 90 ℃ for 24 hours.
The preparation method of the lithium ion battery cathode material comprises the step (2) of mixing Fe (OH)x-Co(OH)yThe MWNTs precursor is reacted for 3h at 180 ℃ for pre-oxidation.
The preparation method of the lithium ion battery cathode material comprises the step (2) of grinding the pre-oxidized precursor into powder and calcining the powder at 350 ℃ for 2 hours.
The lithium ion battery cathode material is CoFe with carbon nano tubes as frameworks2O4-MWNTs composite material, said CoFe2O4The MWNTs composite material is prepared by the preparation method of the lithium ion battery negative electrode material.
Has the advantages that: compared with the prior art, the invention has the following advantages: firstly, the carbon nano tube is used as a supporting framework, so that the structural stability of the material is improved; the carbon nano tube has good conductivity, so that the impedance of the material is reduced, and the overall performance of the material is improved; thirdly, the cobalt ferrite with the spinel structure has good circulation stability in the charging and discharging processes; fourthly, the preparation process is simple, safe and efficient.
Drawings
FIG. 1 is a process flow diagram of an embodiment.
FIG. 2 is a scanning electron micrograph of the composite material of the example.
Fig. 3 is an XRD image of the composite material in example.
FIGS. 4 and 5 show the negative electrode of the composite material of the example at 100 mA · g-1And 1000mA · g-1Current density of (a).
Detailed Description
The invention provides a lithium ion battery cathode material and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a preparation method of a lithium ion battery cathode material, which comprises the following steps:
(1) preparation of Fe (OH)x-Co(OH)yMWNTs precursors: firstly, putting carbon nano tubes (MWNTs) into water for ultrasonic dispersion, then adding ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid in sequence under the condition of stirring to completely dissolve the carbon nano tubes to obtain a mixed solution, and drying the mixed solution at 80-100 ℃ for 24 hours to obtain Fe (OH)x-Co(OH)y-MWNTs precursors; wherein x =2 or 3, y = 2;
(2) preparation of carbon nanotube-based CoFe2O4MWNTs composite: mixing Fe (OH)x-Co(OH)yReacting the MWNTs precursor at 180-200 ℃ for 2-3h for pre-oxidation, and grinding the pre-oxidized precursorCalcining the formed powder at the temperature of 330-2O4-MWNTs composite material, CoFe with carbon nanotube as skeleton2O4The MWNTs composite material is the lithium ion battery negative electrode material.
In the step (1), the carbon nano tube is dispersed by adopting an ultrasonic dispersion method to obtain a uniformly dispersed carbon nano tube suspension; using citric acid as compatilizer and ammonium carbonate as regulator to make Fe under the condition of heating3+、Co2+Depositing on the surface of the carbon nano tube in the form of hydroxide; drying the mixed solution in a drying oven at 80-100 deg.C for 24 hr to obtain Fe (OH)x-Co(OH)yMWNTs precursors.
Preferably, in the step (1), the molar ratio of the ferric nitrate to the cobalt nitrate to the ammonium carbonate to the citric acid is 4:2 (1-1.5): (1-1.5).
Firstly, ultrasonically dispersing carbon nano tubes (MWNTs) in water uniformly to obtain MWNTs suspension, then sequentially adding ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid under the condition of continuously stirring to completely dissolve the MWNTs suspension, then putting the mixed solution into a drying box for drying, then carrying out pre-oxidation, and finally grinding the pre-oxidized precursor into powder and putting the powder into a muffle furnace for calcining; through the mode, the composite material prepared by the invention has very high cycle stability and rate capability, and simultaneously, the rigidity and the conductivity of the material are enhanced by introducing MWNTs.
The invention also provides a lithium ion battery cathode material, wherein the lithium ion battery cathode material is CoFe with the carbon nano tube as a framework2O4-MWNTs composite material, said CoFe2O4The MWNTs composite material is prepared by the preparation method of the lithium ion battery negative electrode material. The lithium ion battery cathode material has very high cycle stability and rate capability, and simultaneously, the rigidity and the conductivity of the material are enhanced by the introduction of MWNTs.
The invention is illustrated in detail below by way of examples:
examples
1. With reference to fig. 1, the preparation method of the negative electrode material of the lithium ion battery of the embodiment includes the following steps:
(1) preparation of Fe (OH)x-Co(OH)yMWNTs precursors:
firstly, putting carbon nano tubes into water, performing ultrasonic dispersion for 30 minutes to obtain MWNTs suspension, then sequentially adding ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid with the molar ratio of 4:2:1:1 under the condition of continuous stirring to completely dissolve the MWNTs suspension, and then putting the mixed solution into a drying oven to dry for 24 hours at 90 ℃ to obtain Fe (OH)x-Co(OH)y-MWNTs precursors;
(2) preparation of carbon nanotube-based CoFe2O4MWNTs composite:
mixing Fe (OH)x-Co(OH)yReacting the MWNTs precursor at 180 ℃ for 3h for pre-oxidation, grinding the pre-oxidized precursor into powder, and calcining the powder in a muffle furnace at 350 ℃ for 2h to obtain the CoFe with the carbon nano tube as the framework2O4-MWNTs composite material.
2. And (4) result characterization:
the scanning electron microscope image of the composite material is shown in fig. 2, and the carbon nanotubes can be clearly seen as a skeleton to be embedded in the matrix material; FIG. 3 is an XRD image of the composite material, from which it can be demonstrated that the composite material is CoFe2O4-MWNTs composite material; FIGS. 4 and 5 show the negative electrode of the composite material at 100 mA · g-1And 1000mA · g-1The cycle performance at the current density of (a) was imaged, and it can be seen that the cycle stability of the composite material was excellent.
In summary, according to the lithium ion battery negative electrode material and the preparation method thereof provided by the invention, firstly, a carbon nanotube suspension is obtained by adopting an ultrasonic dispersion mode, and then, Fe is enabled to be contained in the suspension under the heating condition by using citric acid as a compatilizer and ammonium carbonate as a regulator3+、Co2+Depositing the hydroxide on the surface of the carbon nano tube, and finally preparing CoFe through pre-oxidation and calcination2O4-MWNTs composite material. Compared with the prior art, the invention has the following advantages: firstly, the carbon nano tube is used as a supporting framework, so that the structural stability of the material is improved; the carbon nano tube has good conductivity, so that the impedance of the material is reduced, and the overall performance of the material is improved; thirdly, the cobalt ferrite with the spinel structure has good circulation stability in the charging and discharging processes; fourthly, the preparation process is simple, safe and efficient.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a lithium ion battery cathode material is characterized by comprising the following steps:
(1) preparation of Fe (OH)x-Co(OH)yMWNTs precursors: firstly, putting carbon nano-tubes into water for ultrasonic dispersion, then adding ferric nitrate, cobalt nitrate, ammonium carbonate and citric acid in sequence under the condition of stirring to completely dissolve the carbon nano-tubes to obtain a mixed solution, and drying the mixed solution at 80-100 ℃ for 24 hours to obtain Fe (OH)x-Co(OH)y-MWNTs precursors; wherein x is 2 or 3, and y is 2;
(2) preparation of carbon nanotube-based CoFe2O4MWNTs composite: mixing Fe (OH)x-Co(OH)yReacting the MWNTs precursor at 180 ℃ and 200 ℃ for 2-3h for pre-oxidation, grinding the pre-oxidized precursor into powder, calcining at 330 ℃ and 350 ℃ for 2-3h, and preparing the CoFe with the carbon nano tube as the framework2O4-MWNTs composite material, CoFe with carbon nanotube as skeleton2O4-MWNTs composite material is the lithium ion battery cathode material;
in the step (1), the molar ratio of the ferric nitrate to the cobalt nitrate to the ammonium carbonate to the citric acid is 4:2 (1-1.5): (1-1.5);
carbon nanotube as skeleton embedded CoFe2O4In the material.
2. The preparation method of the negative electrode material of the lithium ion battery as claimed in claim 1, wherein the molar ratio of the ferric nitrate to the cobalt nitrate to the ammonium carbonate to the citric acid is 4:2:1: 1.
3. The preparation method of the negative electrode material of the lithium ion battery according to claim 1, wherein in the step (1), the carbon nanotubes are placed in water for ultrasonic dispersion for 30 minutes.
4. The method for preparing the negative electrode material for the lithium ion battery according to claim 1, wherein in the step (1), the mixed solution is dried at 90 ℃ for 24 hours.
5. The method for preparing the anode material of the lithium ion battery according to claim 1, wherein in the step (2), Fe (OH)x-Co(OH)yThe MWNTs precursor is reacted for 3h at 180 ℃ for pre-oxidation.
6. The preparation method of the negative electrode material of the lithium ion battery as claimed in claim 1, wherein in the step (2), the pre-oxidized precursor is ground into powder and calcined at 350 ℃ for 2 h.
7. The lithium ion battery cathode material is characterized in that the lithium ion battery cathode material is CoFe with a carbon nano tube as a framework2O4-MWNTs composite material, said CoFe2O4-MWNTs composite material is prepared by the method for preparing the lithium ion battery negative electrode material according to any one of claims 1 to 6.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2163517A1 (en) * | 2008-09-04 | 2010-03-17 | Korea Institute Of Science And Technology | Transition metal oxides/multi-walled carbon nanotube nanocomposite and method for manufacturing the same |
| CN103151495A (en) * | 2013-03-20 | 2013-06-12 | 河南师范大学 | Method for preparing hybrid negative electrode materials of lithium ion battery |
| CN107093746A (en) * | 2017-04-28 | 2017-08-25 | 深圳市航盛新材料技术有限公司 | Iron cobalt carbon composite oxides and preparation method thereof, metal-air battery |
| CN107256954A (en) * | 2017-06-16 | 2017-10-17 | 天津大学 | A kind of transition metal oxide carbon nano tube compound material and its preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2163517A1 (en) * | 2008-09-04 | 2010-03-17 | Korea Institute Of Science And Technology | Transition metal oxides/multi-walled carbon nanotube nanocomposite and method for manufacturing the same |
| CN103151495A (en) * | 2013-03-20 | 2013-06-12 | 河南师范大学 | Method for preparing hybrid negative electrode materials of lithium ion battery |
| CN107093746A (en) * | 2017-04-28 | 2017-08-25 | 深圳市航盛新材料技术有限公司 | Iron cobalt carbon composite oxides and preparation method thereof, metal-air battery |
| CN107256954A (en) * | 2017-06-16 | 2017-10-17 | 天津大学 | A kind of transition metal oxide carbon nano tube compound material and its preparation method and application |
Non-Patent Citations (1)
| Title |
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| 柠檬酸修饰碳纳米管及其分散性能;陈传盛等;《四川大学学报(工程科学版)》;20080531;第40卷(第3期);第108-111页 * |
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