CN101859887A - Transition metal phosphate-clad composite lithium ion battery anode material - Google Patents

Transition metal phosphate-clad composite lithium ion battery anode material Download PDF

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CN101859887A
CN101859887A CN201010204782A CN201010204782A CN101859887A CN 101859887 A CN101859887 A CN 101859887A CN 201010204782 A CN201010204782 A CN 201010204782A CN 201010204782 A CN201010204782 A CN 201010204782A CN 101859887 A CN101859887 A CN 101859887A
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lithium
transition metal
metal phosphate
ion battery
lithium ion
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黄云辉
杨泽
夏圣安
李爽
张五星
袁利霞
胡先罗
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Huazhong University of Science and Technology
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Abstract

The invention discloses a transition metal phosphate-clad composite lithium ion battery anode material with lithium-storing active material as a main core and electrochemically active transition metal phosphate as a cladding layer. The active material core mainly carries out electrochemical reaction, and provides battery capacity; and the cladding layer not only can protect the lithium-storing active material and reduce the dissolution and erosion of the active material by electrolyte, but also can increase the battery capacity and improve the rate capability of the active material.

Description

The lithium ion battery composite cathode material that a kind of transition metal phosphate coats
Technical field
The invention belongs to electrochemistry, materials chemistry and chemical power source product technical field, be specifically related to a kind of lithium ion battery composite cathode material
Background technology
The energy is the basic support of national economy, is one of mankind's top 5 factor of depending on for existence.Energy security directly has influence on national security, sustainable development and social stability, and fossil energy provides the energy in the world 90%.Science result of calculation has been verified oil, coal, gas reserves and has been respectively 1,400 hundred million tons, 10,316 hundred million tons, 152m 3, can also exploit respectively 30 years, 200 years, 60 years by present mining level.Day by day the exhausted an urgent demand of fossil energy resource develops the novel renewable energy resources and the high-efficiency cleaning energy, and lithium ion battery because of its operating voltage height, energy density is big, self-discharge rate is low, environmentally friendlyly be subjected to extensive attention.
Lithium is the most negative metal of the lightest current potential, helps the storage of high density energy.After the invention seventies in last century lithium battery, the various lithium batteries of making negative pole with lithium metal constantly come out.1972 Exxon Mobil CorporationExxon company adopts TiS 2As positive pole, metal Li is as positive pole.TiS 2Good layer structure is arranged, embed compound being considered to desirable lithium ion at that time, but this battery produces Li dendrite easily in circulation, when it develops into to a certain degree, will pass barrier film and cause short circuit that battery is caught fire even explode.So people have replaced lithium metal with the Al alloy, but the too big variation cycle performance of the volume of material generation is relatively poor in the cyclic process.People can embed secondary material with ion and replaced lithium metal afterwards, had solved the problem of Li dendrite.Invented layered cathode material Li in 1980 xMO 2(M is Co, Ni or Mn), spinel-type LiMn has been invented in nineteen eighty-three in the back 2O 4, but up in June, 1991 Sony just with LiCoO 2/ C is the rocking chair type battery commercialization of system, and these materials are also using up to now.
Present stage, commercial positive electrode was LiCoO 2, because cobalt resource shortage, poisonous and dangerous is unsuitable for batteries of electric automobile and uses.Because Ni 3+Instability is difficult to prepare the LiNiO of stoichiometric proportion 2Spinel-type LiMn 2O 4Because Jahn-Teller effect and manganese ion easily are dissolved in electrolyte and cause its cycle performance poor when the electrolyte decomposition during the high charge current potential, low discharge current potential, have hindered its large-scale commercial applications application.And rich lithium composite material nLi 2MnO 3. (1-n) LiMO 2Li in (0＜n＜1) 2MnO 3Be insulator, cause its cycle performance bad, high rate performance is not good, and the first charge-discharge coulombic efficiency is low.The method that people adopt metal ions such as Mg, Al, Ti, V, Cr, Co, Ni to mix is carried out study on the modification, but effect is unsatisfactory.In addition, adopt difficult dissolving, constitutionally stable Al also morely 2O 3, MgO, SiO 2Carry out surface treatment and coat Deng oxide, cycle performance can improve, but because these oxides do not have electro-chemical activity, makes specific capacity incur loss, and the lithium ion transport access denial hinders and influences high rate performance.
Summary of the invention
The objective of the invention is to disclose the lithium ion battery composite cathode material that a kind of transition metal phosphate coats, improved the specific capacity of active lithium storage materials, improved cycle performance and high rate performance.
The lithium ion battery composite cathode material that a kind of transition metal phosphate coats is with LiMn2O4 LiMn 2O 4, lithium nickelate LiNiO 2, LiFePO4 LiFePO 4, lithium titanate Li 4Ti 5O 12, lithium-rich anode material bLi 2MnO 3(1-b) LiMO 2, a kind of in 0＜b＜1 perhaps carries out element doping or/and the composite material of surface modification gained is a kernel to above-mentioned any one material, is shell with the transition metal phosphate, wherein, and LiMO 2Be LiCo xNi yMn zO 2, x+y+z=1 or LiMn2O4 LiMn 2O 4Or Li 4Mn 5O 9Or Li 4Mn 5O 12
Described transition metal phosphate is expressed as A aPO 4, 0＜a＜2 wherein, A is any one among Ti, V, Cr, Mn, Fe, Co, Ni, Cu and the Zn.
The present invention compares with current material and has the following advantages: the present invention is a kernel with storage lithium active material, has the A of electro-chemical activity aPO 4Be shell, active material core is mainly carried out electrochemical reaction, and battery capacity is provided, and its shell not only can be protected storage lithium active material, reduces the erosion of electrolyte to active material, but also plays cycle performance and the high rate performance that improves battery.This product is at EC: DMC (1: 1)+1mol/L LiPF 6Show excellent cycle performance and high rate performance in the electrolyte, capacity is held the rate height.Composite material manufacture craft of the present invention is simple and easy to control, with low cost, but large-scale industrial production.
Description of drawings
Fig. 1 is the high rate performance schematic diagram of LiMn2O4 LiMn2O4.
Embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this following examples can only be used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art of this area makes some nonessential improvement and adjusts according to the content of the invention described above and still belongs to protection scope of the present invention.
Embodiment 1 kernel is LiMn2O4 LiMn 2O 4, shell is ferric phosphate FePO 4Combination electrode material
The LiMn2O4 LiMn of solid sintering technology preparation will be adopted 2O 4Attritive powder is dispersed in ferrous sulfate FeSO 4In the aqueous solution, after stirring a period of time, with Fe 2+With PO 4 3-Mol ratio be 1: 1 ammonium dihydrogen phosphate NH 4H 2PO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and mechanical agitation is after a period of time, and the product that obtains refilters separation, and products therefrom is dry under 130 ℃, and then in 550 ℃ of sintering.Shell ferric phosphate FePO in the gained combination electrode material 4Account for kernel LiMn2O4 LiMn 2O 41% of mass ratio.With the lithium sheet is negative pole, records the LiMn2O4 LiMn that this does not at room temperature coat 2O 4With ferric phosphate FePO 4The LiMn2O4 LiMn that coats 2O 4High rate performance as shown in Figure 1, specific capacity and capability retention are as shown in table 1.Curve a represents not coat among Fig. 1, and b represents FePO 4Coat, abscissa is represented specific capacity, and ordinate is represented voltage.
Table 1
Figure GDA0000022538200000041
Figure GDA0000022538200000051
Embodiment 2 kernels are the LiMn2O4 LiAl of adulterated al element 0.02Mn 1.98O 4, shell is titanium phosphate TiPO 4Combination electrode material.
LiMn2O4 LiAl with the adulterated al element of sol-gel process preparation 0.02Mn 1.98O 4Attritive powder is dispersed in Titanium Nitrate Ti (NO 3) 3In the aqueous solution, ultrasonic stirring is after a period of time, with Ti 3+With PO 4 3-Mol ratio be 1: 1 ammonium dihydrogen phosphate NH 4H 2PO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 80 ℃, and then in 300 ℃ of sintering.Shell titanium phosphate TiPO in the gained combination electrode material 4Account for the LiMn2O4 LiAl of kernel adulterated al element 0.02Mn 1.98O 40.01% of mass ratio.
Embodiment 3 kernels are lithium nickelate LiNiO 2, shell is phosphoric acid vanadium VPO 4Combination electrode material
Lithium nickelate LiNiO with the hot method preparation of hydrothermal/solvent 2Attritive powder is dispersed in vanadium chloride VCl 3In the aqueous solution, magnetic agitation is after a period of time, with V 3+With PO 4 3-Mol ratio be 1: 1 ammonium dihydrogen phosphate NH 4H 2PO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 90 ℃, and then in 350 ℃ of sintering.Shell phosphoric acid vanadium VPO in the gained combination electrode material 4Account for kernel lithium nickelate LiNiO 20.1% of mass ratio.
Embodiment 4 kernels are coated aluminum oxide Al 2O 3And the lithium nickelate LiAl of adulterated al element and titanium elements 0.01Ti 0.02Ni 1.97O 2, shell is chromium phosphate CrPO 4Composite material
With coated aluminum oxide Al 2O 3And the lithium nickelate LiAl of adulterated al element and titanium elements 0.01Ti 0.02Ni 1.97O 2Attritive powder is dispersed in chromic nitrate Cr (NO 3) 3In the aqueous solution, after stirring a period of time, with Cr 3+With PO 4 3-Mol ratio be 1: 1 ammonium dihydrogen phosphate NH 4H 2PO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 110 ℃, and then in 400 ℃ of sintering.Shell chromium phosphate CrPO in the gained combination electrode material 4Account for the LiMn2O4 LiMn that the kernel acetylacetone,2,4-pentanedione was handled 2O 41% of mass ratio.
Embodiment 5 kernels are LiFePO4 LiFePO 4, shell is manganese phosphate Mn (PO 4) 2Combination electrode material
With LiFePO4 LiFePO 4Attritive powder is dispersed in manganese nitrate Mn (NO 3) 6In the aqueous solution, after stirring a period of time, with Mn 6+With PO 4 3-Mol ratio be 2: 1 ammonium dihydrogen phosphate NH 4H 2PO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 120 ℃, and then in 500 ℃ of sintering.Shell manganese phosphate Mn (PO in the gained combination electrode material 4) 2Account for kernel LiFePO4 LiFePO 43% of mass ratio.
Embodiment 6 kernels are lithium titanate Li 4Ti 5O 12, shell is cobalt phosphate CoPO 4Combination electrode material
With lithium titanate Li 4Ti 5O 12Attritive powder is dispersed in cobalt nitrate Co (NO 3) 3In the aqueous solution, after stirring a period of time, with Co 3+With PO 4 3-Mol ratio be 1: 1 diammonium hydrogen phosphate (NH 4) 2HPO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 130 ℃, and then in 550 ℃ of sintering.Shell cobalt phosphate CoPO in the gained combination electrode material 4Account for kernel lithium titanate Li 4Ti 5O 127% of mass ratio.
Embodiment 7 kernels are composite material 0.5Li 2MnO 30.5LiMn 0.4Ni 0.4Co 0.2O 2, shell is the phosphoric acid nickel 3(PO 4) 2Combination electrode material
With composite material 0.5Li 2MnO 30.5LiMn 0.4Ni 0.4Co 0.2O 2Attritive powder is dispersed in nitric acid nickel (NO 3) 2In the aqueous solution, after stirring a period of time, with Ni 2+With PO 4 3-Mol ratio be 1.5: 1 diammonium hydrogen phosphate (NH 4) 2HPO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry down at 140 ℃.Shell nickel phosphate Ni in the gained combination electrode material 3(PO 4) 2Account for kernel composite material 0.5Li 2MnO 30.5LiMn 0.4Ni 0.4Co 0.2O 215% of mass ratio.
Embodiment 8 kernels are the composite material 0.3Li that acetylacetone,2,4-pentanedione was handled 2MnO 30.7LiMn 2O 4, shell is cupric phosphate Cu 3(PO 4) 2Combination electrode material
The composite material 0.3Li that acetylacetone,2,4-pentanedione was handled 2MnO 30.7LiMn 2O 4Attritive powder is dispersed in copper chloride CuCl 2In the aqueous solution, after stirring a period of time, with Cu 2+With PO 4 3-Mol ratio be 1.5: 1 diammonium hydrogen phosphate (NH 4) HPO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 150 ℃, and then in 700 ℃ of sintering.Shell cupric phosphate Cu in the gained combination electrode material 3(PO 4) 2Account for the composite material 0.3Li that the kernel acetylacetone,2,4-pentanedione was handled 2MnO 30.7LiMn 2O 420% of mass ratio.
Embodiment 9 kernels are composite material 0.7Li 2MnO 30.3Li 4Mn 5O 9, shell is trbasic zinc phosphate Zn 3(PO 4) 2Combination electrode material
With composite material 0.7Li 2MnO 30.3Li 4Mn 5O 9Attritive powder is dispersed in zinc nitrate Zn (NO 3) 2In the aqueous solution, after stirring a period of time, with Zn 2+With PO 4 3-Mol ratio be 1.5: 1 diammonium hydrogen phosphate (NH 4) 2HPO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 150 ℃, and then in 750 ℃ of sintering.Shell trbasic zinc phosphate Zn in the gained combination electrode material 3(PO 4) 2Account for kernel composite material 0.7Li 2MnO 30.3Li 4Mn 5O 925% of mass ratio.
Embodiment 10 kernels are composite material 0.8Li 2MnO 30.2Li 4Mn 5O 12, shell is trbasic zinc phosphate Zn 3(PO 4) 2Combination electrode material
With composite material 0.8Li 2MnO 30.2Li 4Mn 5O 12Attritive powder is dispersed in zinc nitrate Zn (NO 3) 2In the aqueous solution, after stirring a period of time, with Zn 2+With PO 4 3-Mol ratio be 1.5: 1 diammonium hydrogen phosphate (NH 4) 2HPO 4The aqueous solution slowly adds above-mentioned suspension-turbid liquid, and after reaction and ageing a period of time, the product that obtains refilters separation, and products therefrom is dry under 150 ℃, and then in 800 ℃ of sintering.Shell trbasic zinc phosphate Zn in the gained combination electrode material 3(PO 4) 2Account for the multiple composite material 0.8Li of kernel 2MnO 30.2Li 4Mn 5O 1230% of mass ratio.
The mass ratio of kernel and shell does not limit, but preferred shell accounts for the mass percent 0.01%～30% of kernel.Kernel element doping and surface modification are used to improve the chemical property of kernel, optional wide range, for example doped chemical can be selected a kind of among Li, F, Mg, Al, Ti, V, Cr, Fe, Co, Ni, Mn, Cu, Zn, Cl, the I etc. or more than one, the mol ratio that doped chemical accounts for former kernel is 0.01～0.5, and surface modification can adopt organic substance surface treatment and the surface coated mode of inorganic matter, the organic substance surface treatment has acetylacetone,2,4-pentanedione, polythiophene etc., and the inorganic surfaces coating can be selected Al 2O 3, ZnO, TiO 2Deng, above-mentioned doped chemical and surface modification are just enumerated, and should not be construed limitation of the present invention, and every material that improves the kernel chemical property that can be used in all can.

Claims (3)

1. the lithium ion battery composite cathode material that coats of a transition metal phosphate is with LiMn2O4 LiMn 2O 4, lithium nickelate LiNiO 2, LiFePO4 LiFePO 4, lithium titanate Li 4Ti 5O 12, lithium-rich anode material bLi 2MnO 3(1-b) LiMO 2, a kind of in 0＜b＜1 perhaps carries out element doping or/and the composite material of surface modification gained is a kernel to above-mentioned any one material, is shell with the transition metal phosphate, wherein, and LiMO 2Be LiCo xNi yMn zO 2, x+y+z=1 or LiMn2O4 LiMn 2O 4Or Li 4Mn 5O 9Or Li 4Mn 5O 12
2. lithium ion battery composite cathode material according to claim 1 is characterized in that described transition metal phosphate is expressed as A aPO 4, 0＜a＜2 wherein, A is any one among Ti, V, Cr, Mn, Fe, Co, Ni, Cu and the Zn.
3. lithium ion battery composite cathode material according to claim 1 and 2 is characterized in that, the mass percent that described coating layer accounts for kernel is 0.01%～30%.
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Application publication date: 20101013