CN210006820U - lithium ion battery anode structure with doping and cladding double modification - Google Patents

lithium ion battery anode structure with doping and cladding double modification Download PDF

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CN210006820U
CN210006820U CN201920344550.3U CN201920344550U CN210006820U CN 210006820 U CN210006820 U CN 210006820U CN 201920344550 U CN201920344550 U CN 201920344550U CN 210006820 U CN210006820 U CN 210006820U
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active material
lithium ion
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张晨
白莹
郁彩艳
赵慧玲
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Henan University
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Abstract

The utility model provides an lithium ion battery anode structure with doping and two decorations of cladding, including the structure of lithium ion battery cathode active material body, doping metal ion, coating and having the pinning effect, doping metal ion forms the cladding thing at the doping in-process, and the cladding thing constitutes the coating, and the coating reunion is outside cathode active material is originally the utility model discloses with the two kinds of modification means to lithium ion battery cathode material of body doping and surface coating through step annealing realization cathode material metal ion doping and the two decoration effects of corresponding metallic element compound surface cladding, the event can reach from interior to exterior stability lithium ion battery cathode active material's body structure and surface structure, compromise inside body structure and surface protection structure's compatibility to improve the whole dynamics action that lithium ion battery cathode active material transported the diffusion at electrochemistry cyclic process ion.

Description

lithium ion battery anode structure with doping and cladding double modification
Technical Field
The utility model relates to a lithium ion battery cathode material field, concretely relates to lithium ion battery cathode structure that have doping and two decorations of cladding.
Background
The method comprises the steps of selecting doping ions with the radius similar to that of metal cations contained in the positive active material to replace the metal ions in the positive active material, mainly comprising transition metal ion doping, aliovalent element doping, rare earth element doping, heavy element doping and the like, in the coating modification, selecting a coating material according to the characteristics and modification purposes of different coating materials, mainly comprising metal oxides, fluorides, phosphates, fast ion conductors and the like, along with the deepening of the modification research of the lithium ion positive active material, the related research of improving the positive active performance by adopting a doping and coating double modification means also gradually appears, but the current research of doping and coating double modification is limited in a two-step annealing treatment method, the surface of the positive active material is directly treated by adopting a annealing step treatment method, the surface of the doping and coating double modification means has the effect of improving the surface of the positive active material, and the electrochemical active material has the problem of improving the surface stability of the positive active material in the early stage of the anode active material preparation process, but the electrochemical active material has the defect that the electrochemical active material has the cycle effect of improving the surface of the anode active material in the anode active material prepared by adopting the two-cycle annealing treatment method, so that the anode active material has the defect that the cycle effect of improving the anode active material, and the cathode active material has the anode active material prepared by adopting the anode active material in the cycle treatment method of the anode active material in the early stage of improving the anode active material preparation process, and the anode active material preparation method of the anode active material in the anode active material.
The utility model provides an mix the in-process from two modification structures of cladding modified lithium ion battery positive pole active material altogether, improve its electrochemistry circulation performance's advantage at positive pole active material bulk doping metal ion in order to exert, form the coating simultaneously on its surface in order to keep positive pole active material body surface structure's stability and durability in electrochemistry circulation process, thereby step realizes the two modification effect of metal ion bulk doping and its compound surface cladding, this structure is prepared by step annealing processing method, compromise bulk doping and surface cladding's two modification advantages, effectively strengthen lithium ion positive pole active material's whole electricity transport characteristic.
SUMMERY OF THE UTILITY MODEL
The utility model provides an lithium ion battery anode structure who has doping and two decorations of cladding and pinning effect, this structure has realized that inside body phase doping metallic element improves the electrochemical properties of anodal active material body to form the coating of protection anodal active material body structure simultaneously on its surface.
Realize the technical scheme of the utility model is that:
lithium ion battery anode structures with doping and cladding double modification and pinning effects, including lithium ion battery anode active material body, doping metal ion, cladding layer and structure body with pinning effect.
The doped metal ions form a coating in the doping process, the coating forms a coating layer, and the coating layer is agglomerated outside the positive active material body.
or more kinds of doped metal ions are selected to meet the requirement that the difference between the radius of the doped element ions and the radius of the transition metal ions in the positive active material is larger, so that continuous solid solution is avoided being formed, saturated doping can be easily achieved in the positive active material body, the crystal structure of the active material body is kept, or more kinds of cladding materials can be formed on the surface of the positive active material body in situ, and the double-modified positive active material is obtained.
The chemical components of the or more coatings formed in situ on the surface of the positive active material body by doping metal ions are determined by the annealing temperature and the annealing atmosphere adopted in the preparation process, the selected doping element M and the anions and cations in the positive active material body, and finally the lithium ion battery positive active material with the doping and coating double-modification effects is formed through the steps of annealing treatment.
The structure body with the pinning effect is arranged in the interface of the cladding layer, and the structure body with the pinning effect is formed by the aggregation of the doped metal and the cladding.
The anode active material body is LiCoO with a layered structure2、LiNiO2、LiCoxNi1-xO2、LiCoxNiyMnzO2、xLi2MnO3·(1-x)LiMO2And derivatives thereof, wherein 0<x<1、0<y<1、0<z<1. x + y + z =1, M is Mn, Ni, Co; olivine structured LiFePO4And derivatives thereof; spinel-structured LiMn2O4、LiMn1.5Ni0.5O4And derivatives thereof.
The doped metal ions are or more of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
The utility model is prepared by the following method:
1. the method comprises the steps of preparing a pretreatment product of a lithium ion battery positive active material with a self-coated double-modification structure in a doping process by adopting a sol-gel method, then annealing for steps to prepare a final product of the lithium ion battery positive active material with the self-coated double-modification structure in the doping process, specifically, weighing a precursor of a transition metal element, a lithium salt and a precursor of a doping metal element M with a content of in a certain proportion in the positive material according to a stoichiometric ratio, selecting a chelating agent, dissolving the chelating agent in deionized water, mixing and stirring the precursor solutions uniformly, evaporating the mixture into gel, putting the gel into a drying box, fully drying the gel into xerogel at a certain temperature of , pre-annealing at a temperature range of 400-600 ℃, taking out the gel, uniformly grinding to obtain the pretreatment product of the self-coated lithium ion battery positive active material with the double-modification structure in the doping process, then calcining at a set annealing temperature and an annealing atmosphere, naturally cooling, cleaning, drying and grinding to prepare the final product of the self-coated double-modification lithium ion battery positive active material in the doping process.
2. Weighing a precursor of a transition metal element, a lithium salt and a precursor of a doping metal element M with a content in a certain proportion in the positive electrode material according to a stoichiometric ratio, fully and mechanically mixing and ball-milling in a ball mill, calcining at a set annealing temperature and in an annealing atmosphere, naturally cooling, cleaning, drying and grinding to obtain the self-coated double-modified positive electrode active material of the lithium ion battery in the doping process.
The beneficial effects of the utility model are that the preparation process of this anodal active material structure is first with the bulk phase doping, accomplish the whole back that dopes of anodal material body, step are being possessed the anodal active material body surface that the bulk phase adulterated by the doping material and form the cladding shell layer, that is, realize anodal material metal ion doping and the two kinds of modification means to lithium ion battery anodal material of surface cladding through step annealing with the bulk phase doping, so can reach from inside to outside and stabilize anodal active material's of lithium ion battery bulk phase structure and surface structure, compromise the compatibility of inside body structure and surface protection structure, thereby improve the whole dynamic behavior of anodal active material of lithium ion battery ion transport diffusion in electrochemical cycle process, optimize the purpose of security performance in the anodal active material working process simultaneously.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only the embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of the present invention.
FIG. 2 shows a prepared lithium ion battery positive electrode active material Y with a self-coated double-modification structure in a doping process2O3@LiCo0.99Y0.01O2And LiCo having only a bulk-doped single-modification structure0.995Y0.005O2And Y having only a surface-coated single-modified structure2O3@LiCoO2Bulk LiCoO with original positive electrode active material2Electrochemical long cycle curve of (2). The results show that Y with self-coating double modified structure is coated during doping2O3@LiCo0.99Y0.01O2Has optimal cycle stability.
Fig. 3 shows XRD test patterns of the positive electrode material Y @ LCO with bulk doping and surface coating double modification structure at different atomic ratio (Y/Co) contents (0.0 at.%, 0.5 at.%, 1.0at.%, 1.5 at.%, 2.0 at.%). The results showed that the positive electrode active material LiCoO was retained in the material before and after modification2The bulk crystal structure of (1) has a Y ion doping content higher than 1.0at.% and then Y appears2O3And the main peak (003) shifts to a low angle as the doping content increases, indicating LiCoO2After doping with the metal ions Y having a large ion radius, the (003) interplanar spacing becomes large.
Fig. 4 is a graph of the content of different doped Y metal ions and the variation trend of the lattice constant, which is plotted after the quantitative calculation of the XRD measurement result. The results show that LiCoO is added with the doping content of Y metal ions2The lattice constant a of the anode active material body is basically kept unchanged, the lattice constant c and the ratio c/a of the lattice constant c to the lattice constant c are increased, and the fact that Y metal ions can enter LiCoO through doping is quantitatively and intuitively proved2Bulk phase and increases the (003) interplanar spacing.
FIG. 5 shows lithium ion battery positive electrode active materials (Y gold) with self-coating double modification in doping processGenus ion content 1.5 at.%)). FIG. a shows the prepared bulk phase doping and surface coating double-modified Y2O3@LiCoO2An SEM (scanning electron microscope) morphology graph of the positive electrode active material shows that product particles are uniform and the size of the product particles is 1-3 mu m; panel b is an EDS spectrum collected in an SEM test showing that the product particles contain Co, Y elements; and the graphs c and d are Mapping graphs of Co and Y elements collected in the SEM test, respectively, and show that the Co and Y elements are uniformly distributed in the prepared product.
FIG. 6 LiCoO, a positive electrode active material for lithium ion batteries2And (4) characterization results of the TEM before modification and the TEM after double modification. Panel a is unmodified LiCoO2A TEM image of the positive active material body; FIG. b is the HRTEM result of the dashed area in FIG. a, wherein the interplanar spacings are marked and the layered structure LiCoO in a standard card library2(003) The interplanar spacing is , and the figure c shows that the prepared bulk phase doping and surface coating double-modified lithium ion battery anode active material Y0.005O0.0075@LiCo0.99Y0.01O2Shows bulk doped LiCo0.99Y0.01O2The surface of the main body material is covered with a coating; FIG. d is the HRTEM result of the dashed line region of FIG. c, in which the noted interplanar spacings correspond to Y, respectively2O3The (400) and (222) interplanar spacings of (A) and (B), the presence of a surface coating layer is verified, and the XRD curve shows Y2O3The diffraction peak phase is .
Detailed Description
The technical solution in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of , but not all embodiments.
As shown in fig. 1, lithium ion battery positive electrode structures with doping and cladding double modification and pinning effects comprise a lithium ion battery positive electrode active material body 1, a doping metal ion 2, a cladding layer 3 and a structural body 4 with pinning effects.
The doped metal ions 2 form a coating in the doping process, the coating forms a coating layer 3, and the coating layer 3 is agglomerated outside the positive active material body 1.
The structural body 4 with the pinning effect is arranged in the interface of the coating layer 3, and the structural body 4 with the pinning effect is formed by the aggregation of the doped metal and the coating.
The positive active material body 1 is LiCoO with a layered structure2、LiNiO2、LiCoxNi1-xO2、LiCoxNiyMnzO2、xLi2MnO3·(1-x)LiMO2And derivatives thereof, wherein 0<x<1、0<y<1、0<z<1. x + y + z =1, M is Mn, Ni, Co; olivine structured LiFePO4And derivatives thereof; spinel-structured LiMn2O4、LiMn1.5Ni0.5O4And derivatives thereof.
The doped metal ions 2 are or more of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
The lithium battery with the structure is prepared by a sol-gel method and a high-temperature solid phase method, and the specific embodiment is as follows:
example 1
In this embodiment lithium ion battery anode structures with doping and cladding double modification and pinning effects, the lithium ion battery anode active material body 1 is LiCoO2The doped metal ion 2 is Y, the coating layer 3 is Y2O3The structure 4 having the pinning effect is a cladding Y2O3And bulk Y doping.
The preparation method comprises the following specific steps:
the modified lithium ion battery positive active material body is LiCoO2The self-coating co-modified double-modified positive active material in the doping process can be written as LiαCoβMγOδ@LixCoyMzO2Wherein 0 is not more than α<0.1，0≤β<0.1，0<γ<0.1，0<δ≤0.3，0.9<x≤1，0.9<y<1，0<z<0.1，0<Gamma + z is less than or equal to 0.1, or more coatings are formed on the surface of the double modified element M, if M is a rare earth element Y, LiCoO subjected to bulk phase doping and surface coating double modification is adopted2Different coatings such as LiYO will be formed at different annealing temperatures2Or Y2O3. Specifically, setting the annealing temperature higher than 900 ℃, surface LiYO can be obtained2Double modified LiCoO coated with bulk phase Y doping2Positive electrode active material, named Li0.005Y0.005O0.01@Li0.995Co0.99Y0.01O2Setting an annealing temperature below 900 ℃ will form a surface Y2O3Double modified LiCoO coated with bulk phase Y doping2Positive electrode active material designated as Y0.005O0.0075@LiCo0.99Y0.01O2。
Preparation of surface coating Y2O3Double modified LiCoO doped with bulk phase Y2Positive electrode active material Y0.005O0.01@LiCo0.99Y0.01O2The method comprises the specific implementation steps of weighing quantitative lithium nitrate, cobalt nitrate, yttrium nitrate and citric acid according to the proportion of 1.1:0.985:0.015:3.15, respectively dissolving in deionized water, then uniformly mixing, continuously stirring the mixed solution at 80 ℃ for 8h to form sol, then presintering in a muffle furnace at 500 ℃ for 6h, cooling, taking out, fully grinding uniformly, then annealing at 750 ℃ in an air atmosphere for 12h, naturally cooling to room temperature to obtain the self-coated double-modified positive electrode active material Y in the doping process0.005O0.01@LiCo0.99Y0.01O2。
Example 2
In this embodiment lithium ion battery anode structures with doping and cladding double modification and pinning effects, the lithium ion battery anode active material body 1 is LiCoO2Y is the doped metal ion 2, and LiYO is the coating layer 32The structure 4 having the pinning effect is coated LiYO2And bulk phase Y doping double modification.
Preparation of surface-coated LiYO2Double modified LiCoO doped with bulk phase Y2Positive electrode active material Li0.005Y0.005O0.01@Li0.995Co0.99Y0.01O2The method comprises the specific implementation steps of weighing quantitative lithium nitrate, cobalt nitrate, yttrium nitrate and citric acid according to the molar ratio of 1.2:0.985:0.015:3.15, respectively dissolving in ultrapure water, uniformly mixing, continuously stirring the mixed solution at 80 ℃ for reaction for 10 hours to form sol, drying in a drying box at 120 ℃ for 12 hours, uniformly grinding the obtained dried gel, presintering in a muffle furnace at 600 ℃ for 24 hours, cooling, taking out, fully grinding uniformly, annealing at 900 ℃ for 24 hours in an air atmosphere, naturally cooling to room temperature, and obtaining the self-coated and double-modified positive electrode active material Li in the doping process0.005Y0.005O0.01@Li0.995Co0.99Y0.01O2。
Example 3
In this embodiment lithium ion battery anode structures with doping and cladding double modification and pinning effects, the lithium ion battery anode active material body 1 is LiCoO2The doped metal ion 2 is La, the coating layer 3 is LaCoO3The structure 4 with pinning effect is coated LaCoO3And bulk La doping double modification.
Preparing doped -body-coated La by steps of high-temperature solid-phase method0.195Co0.0195O0.0585@LiCo0.995La0.005O2Weighing mass lithium carbonate, cobaltosic oxide and lanthanum nitrate according to the stoichiometric ratio of 1: 0.8: 0.2, mixing and ball-milling in a ball mill, calcining at 1100 ℃ for 4h, naturally cooling, taking out, cleaning, drying and grinding to obtain the double-modified La0.195Co0.0195O0.0585@LiCo0.995La0.005O2And (3) a positive electrode material.
Example 4
The present embodiment has dopingAnd a lithium ion battery anode structure with coating double modification and pinning effects, wherein the lithium ion battery anode active material body 1 is LiCoO2Ce is doped with metal ions 2, CeO is coated layer 32The structural body 4 with pinning effect is coated with CeO2And bulk Ce doping double modification.
high-temperature solid-phase method for preparing doping-coated -formed Ce0.005O0.02@LiCo0.99Ce0.005O2And (3) a positive electrode material.
mass parts of lithium nitrate, cobalt nitrate and cerium nitrate are weighed according to the stoichiometric ratio of 1: 0.99: 005, mixed and ball-milled in a ball mill, calcined at 650 ℃ for 24 hours, and taken out after natural cooling, cleaned, dried and ground to obtain double-modified Ce0.005O0.02@LiCo0.99Ce0.005O2And (3) a positive electrode material.
Example 5
In this embodiment lithium ion battery anode structures with doping and cladding double modification and pinning effects, the lithium ion battery anode active material body 1 is Li [ Li0.2Mn0.56Ni0.17Co0.07]O2The doped metal ion 2 is Y, the coating layer 3 is Y2O3The structure 4 having the pinning effect is a cladding Y2O3And bulk phase Y doping double modification.
Different from example 1, the selection of the host material for coating doping co-modification, this time Y is prepared2O3Lithium-rich Li [ Li ] with double modification of cladding and Y doping0.2Mn0.56Ni0.17Co0.07]O2And (3) a positive electrode material.
The precursor is weighed by dissolving lithium acetate, manganese acetate, yttrium nitrate, nickel acetate, cobalt acetate and citric acid in a molar ratio of 1.1:0.545:0.015:0.17:0.07:3.15 in an ethylene glycol solution, mixing and stirring uniformly, continuously stirring at 120 ℃ for 24 hours to form sol, drying at 150 ℃ in a drying box for 18 hours, pre-sintering the obtained dried gel at 500 ℃ in a muffle furnace for 6 hours, grinding uniformly, annealing the dried gel at 900 ℃ in an air atmosphere for 12 hours, and naturally coolingCooling to room temperature to obtain Y2O3Coated Li [ Li ]0.2Mn0.55Y0.01Ni0.17Co0.07]O2A material. LaCoO can be obtained by similarly changing the precursor of the doping element3Coated lithium-rich Li [ Li ]0.2Mn0.555La0.005Ni0.17Co0.07]O2And (3) a positive electrode material.
Example 6
In this embodiment lithium ion battery anode structures with doping and cladding double-modification and pinning effects, the lithium ion battery anode active material body 1 is LiNi0.5Mn1.5O4The doped metal ion 2 is Y, the coating layer 3 is Y2O3The structure 4 having the pinning effect is a cladding Y2O3And bulk phase Y doping double modification.
Different from example 5, the selection of the host material for coating doping co-modification, this time Y is prepared2O3Coated and Y-doped double-modified LiNi0.5Mn1.5O4Spinel cathode material.
quantitative lithium nitrate, manganese acetate, yttrium nitrate, nickel acetate and citric acid are weighed according to the molar ratio of 1.1:1.485:0.015:0.5:3.1, dissolved in ultrapure water, uniformly mixed and stirred, the pH value is adjusted to 7 by using ammonia water, sol is formed by continuously stirring at 80 ℃ for 8h, then dried at 120 ℃ for 14h, the obtained dried gel is presintered in a muffle furnace at 500 ℃ for 6h, uniformly ground, finally annealed at 800 ℃ for 14h in air atmosphere, and naturally cooled to room temperature to obtain Y2O3Coated LiNi0.5Mn1.4Y0.01O4Spinel cathode material. Similarly, the precursor of the doping element is changed to obtain CeO2Coated LiNi0.5Mn1.495Ce0.005O4Spinel cathode material.
Example 7
In this embodiment lithium ion battery anode structures with doping and cladding double-modification and pinning effects, the lithium ion battery anode active material body 1 is LiFePO4 Doping metal ionsSeed 2 is Y, and coating layer 3 is Y2O3The structure 4 having the pinning effect is a cladding Y2O3And bulk phase Y doping double modification.
Different from example 6 in the selection of the host material for cladding doping co-modification, Y was prepared this time2O3Coated LiFe0.99Y0.01PO4Weighing quantitative lithium carbonate, ferrous salt, ammonium dihydrogen phosphate and yttrium nitrate as raw materials according to the molar ratio of 1.1:0.985:1:0.015, calcining for 10h in argon at 900 ℃, and cooling to normal temperature to obtain Y2O3Coated LiFe0.99Y0.01PO4A material.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (2)

  1. The lithium ion battery anode structure with doping and coating double modifications is characterized by comprising a lithium ion battery anode active material body (1), doping metal ions (2), a coating layer (3) and a structural body (4) with a pinning effect, wherein the doping metal ions (2) form a coating in the doping process, the coating layer (3) is formed by the coating, the coating layer (3) is aggregated outside the anode active material body (1), the structural body (4) with the pinning effect is arranged in the interface of the coating layer (3), and the structural body (4) with the pinning effect is formed by aggregation of the doping metal and the coating.
  2. 2. The lithium ion battery positive electrode structure with doping and coating double modification of claim 1, wherein: the positive active material body (1) is LiCoO with a layered structure2、LiNiO2、LiCoxNi1-xO2、LiCoxNiyMnzO2、xLi2MnO3·(1-x)LiMO2And itDerivatives of formula (I) wherein 0<x<1、0<y<1、0<z<1. x + y + z =1, M is Mn, Ni, Co; olivine structured LiFePO4And derivatives thereof; spinel-structured LiMn2O4、LiMn1.5Ni0.5O4And derivatives thereof.
CN201920344550.3U 2019-03-19 2019-03-19 lithium ion battery anode structure with doping and cladding double modification Active CN210006820U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113394401A (en) * 2021-06-25 2021-09-14 浙江帕瓦新能源股份有限公司 Halide fast ion conductor modified anode material and preparation method thereof
CN114068925A (en) * 2020-07-30 2022-02-18 宝山钢铁股份有限公司 Lanthanum-containing perovskite type oxide surface modified positive electrode material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114068925A (en) * 2020-07-30 2022-02-18 宝山钢铁股份有限公司 Lanthanum-containing perovskite type oxide surface modified positive electrode material and preparation method thereof
CN113394401A (en) * 2021-06-25 2021-09-14 浙江帕瓦新能源股份有限公司 Halide fast ion conductor modified anode material and preparation method thereof

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