CN107665993B - Synthesis of coordination polymer and application of coordination polymer in lithium ion battery cathode material - Google Patents
Synthesis of coordination polymer and application of coordination polymer in lithium ion battery cathode material Download PDFInfo
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- H01M10/0422—Cells or battery with cylindrical casing
- H01M10/0427—Button cells
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- H—ELECTRICITY
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- 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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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/137—Electrodes based on electro-active polymers
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Abstract
The invention discloses a synthesis of coordination polymer and application thereof in lithium ion battery cathode material, wherein the chemical formula of the coordination polymer is [ Ni (PBIM) (OH-BDC)]n(in the formula, n is a natural number from 1 to infinity), wherein PBIM is 2,2 '-pyridyl benzimidazole, OH-BDC is 5-hydroxyisophthalic acid, the preparation method of the complex is that nickel acetate tetrahydrate, 2,2' -pyridyl benzimidazole, 5-hydroxyisophthalic acid and triethylamine are added into a mixed solution of water and methanol, and a target product complex [ Ni (PBIM) (OH-BDC) is obtained through a hydrothermal reaction]n(ii) a Can be used in the negative electrode material of the lithium ion battery. The invention has the advantages that: the obtained complex has the advantages of simple synthesis method, easily obtained raw materials, easy operation, mild reaction conditions, high yield, low cost and good stability of the product, and can be directly used in a lithium battery cathode material to show good electrochemical performance.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to synthesis of a coordination polymer material with good stability, a lithium ion battery cathode and a lithium ion battery preparation method.
Background
Along with the development of economic society, the demand for efficient clean energy is urgent, and lithium ion batteries are advanced energy storage devices, have the outstanding advantages of light weight, small volume, portability, high working voltage, high specific energy, small self-discharge, long cycle life, high safety, no memory effect, no environmental pollution and the like, become small and light-weight ideal power supplies for electronic devices such as cameras, mobile phones, notebook computers, portable measuring instruments and the like, and are also the preferred power supplies for high-energy power batteries of automobiles in the future. The lithium ion battery consists of a positive electrode, a negative electrode, an electrolyte and a diaphragm. Because the anode and cathode materials are the key for determining the performance of the battery, the commercial anode material taking graphene as the leading factor cannot meet the requirements of the current society for energy sources due to the problems of low theoretical capacity and safety. The search for stable electrode materials with high capacity and low discharge voltage plateau is the current research hotspot. However, although many oxides, sulfides, phosphides and the like are researched at present, the oxides, sulfides, phosphides and the like have certain advantages in specific capacity and cycle performance, the huge volume expansion generated in the charging and discharging process is a bottleneck limiting the development of the oxides, sulfides, phosphides and the like.
The coordination polymer (complex for short) is an organic-inorganic hybrid material, and has structural diversity due to the selectivity of the assembled metal ions and organic ligands, and has wide application in various fields such as gas adsorption separation, catalysis, magnetism, fluorescence and the like due to rich functional groups and open metal sites. In the field of electrochemistry, complex materials and derivatives thereof are also receiving increasing attention. The complex is directly applied to the lithium ion battery, the synthesis method is simple, and due to the structural diversity of the complex, metal and ligand are potential lithium extraction sites and become a focus of attention. However, the direct application of the complex reported at present to lithium ion batteries mainly faces the problems of poor solubility and low specific capacity of materials. Overcoming these problems is greatly helpful in driving the development of electrode materials.
Disclosure of Invention
The first objective of the present invention is to provide a method for preparing a coordination polymer applied to a negative electrode material of a lithium ion battery, aiming at the above technical analysis, so as to solve the problems of poor solubility and low specific capacity existing in the current application in the battery.
A second object of the present invention is to provide an electrode sheet using the above negative electrode material.
The third purpose of the invention is to provide a lithium ion battery using the negative electrode material electrode plate.
The invention is realized by the following technical scheme:
a method for synthesizing a novel complex comprises the following steps:
step (1): complex [ Ni (PBIM) (OH-BDC)]n(wherein n is a natural number of 1 to positive infinity).
Weighing nickel acetate tetrahydrate, 2,2 '-pyridyl benzimidazole, 5-hydroxyisophthalic acid and triethylamine, dissolving the nickel acetate tetrahydrate, the 2,2' -pyridyl benzimidazole, the 5-hydroxyisophthalic acid and the triethylamine in a mixed solution of methanol and water in a volume ratio of 1:3, uniformly mixing to obtain a mixed solution, placing the mixed solution in a 23mL sealed stainless steel reaction kettle, heating to 120 ℃, reacting for 3 days, and cooling to room temperature after the reaction is finished to obtain a complex crystal. FIG. 1 shows the steps of the synthesis of the complex of the present invention.
Wherein the molar ratio of nickel acetate tetrahydrate, 2' -pyridylbenzimidazole, 5-hydroxyisophthalic acid and triethylamine is 5: 1: 2: 1; the volume ratio of methanol to water is 1: 3.
and (2) putting the crystals in the reaction kettle in the step (1) on a glass sheet, selecting transparent crack-free crystals with the size of 0.3X 0.5mm under a microscope, measuring on a Supernova type X-ray single crystal diffractometer, and using Mo-K α ray monochromated by a graphite monochromator
Is a source of incident radiation, in
The diffraction points were collected by scanning, their coordinates and their anisotropic parameters were corrected by the least squares method, the position of the hydrogen atoms was obtained by theoretical hydrogenation, and all calculations were performed using the SHELXL-97 and SHELXL-97 packages. The final molecular formula of the compound was determined by single crystal diffraction data analysis in combination with elemental analysis, thermogravimetric analysis, and Olex-2 software. The results show that: the structural formula of the metal-organic framework material is [ Ni (PBIM) (OH-BDC)]n(wherein n is a natural number of 1 to plus infinity), wherein PBIM is 2,2' -pyridylbenzimidazole and OH-BDC is 5-hydroxyisophthalic acid, belonging to the monoclinic system, space group P21N, unit cell parameter of
α γ 90 °, β 96.123(4 °), unit cell volume is
Z＝4，Dc＝1.649g/cm3Wherein each metal Ni is hexa-coordinatedThe structure is respectively coordinated with two nitrogens from 2,2' -pyridyl benzimidazole and four oxygens from two 5-hydroxyisophthalic acids, the complex presents a one-dimensional zigzag chain structure, and the chains are connected into a three-dimensional structure through weak interaction of hydrogen bonds. FIG. 3 is an X-ray diffraction pattern of a plurality of samples after the operation of step 1, which illustrates that the diffraction patterns of the plurality of samples synthesized are consistent with the X-ray diffraction pattern of the simulated samples, thereby illustrating that the purity of the synthesized complex is high.
II, complex [ Ni (PBIM) (OH-BDC)]nApplication of negative electrode material in preparation of electrode plate
And (2) drying the complex crystal prepared in the step (1) in a vacuum oven at 60 ℃ for 8 hours. Then weighing the dried complex [ Ni (PBIM) (OH-BDC) in a mass ratio of 6:3:1]nGrinding and uniformly mixing a conductive agent (ketjen black) and a binder (polyvinylidene fluoride), mixing into slurry by using a solvent (N-methylpyrrolidone), coating the slurry on a copper foil, drying for 12 hours at the temperature of 80 ℃ in vacuum, and slicing to obtain the round electrode plate. The specific operation is to select an MSK-T10 manual slicer with the mold diameter of 12mm to slice the obtained electrode slice to obtain a circular electrode slice, and weighing the electrode slice for later use.
Application of electrode plate made of negative electrode material in preparation of lithium ion battery
Using lithium plate as counter electrode, Celgard 2400 membrane as diaphragm, 1mol/L lithium hexafluorophosphate (LiPF)6) The lithium ion button cell is an electrolyte, wherein Ethylene Carbonate (EC) and diethyl carbonate (DEC) in volume ratio are used as solvents, a weighed circular electrode plate is used as a negative electrode to assemble the lithium ion button cell, and the cell model is CR 2032.
And (3) electrochemical performance testing: the temperature is room temperature, the voltage range in constant current charge and discharge test is 0.01-3V, the number of charge and discharge cycles in cycle performance test is 150, and the current density is 100mAg-1The multiplying power performance test respectively tests that the current density is 50mA g-1，100mA g-1，200mA g-1，500mA g-1，1000mA g-1，50mA g-1Constant current charge and discharge were performed, and the number of cycles was 10 at each magnification.
The invention has the advantages and beneficial effects that:
(1) compared with the traditional lithium ion battery cathode material (graphite), the battery prepared by adopting the complex synthesized by the invention as the battery cathode material has greatly improved specific capacity and 100 mA-g current density-1The specific capacity is still 1021mAh g after 150 times of charge-discharge circulation-1。
(2) The battery prepared by the invention has greatly improved stability and the current density is 100 mA.g-1When the lithium ion battery is charged and discharged for 150 times, the capacity retention rate is 84.21 percent, and the specific capacity can be stabilized at 1021mAh g-1Left and right. Shows good electrochemical performance and is 500mA · g-1Circulating for 150 weeks, and the capacity is 600mAh g-1Left and right, and keeps stable, and simultaneously the coulombic efficiency reaches up to 99 percent, which reflects the good cycle performance of the material. The rate performance test also proves the electrochemical stability of the complex of the invention.
Drawings
FIG. 1 is a diagram of the reaction steps for the synthesis of a complex according to the present invention;
FIG. 2 is a diagram of structural analysis of the complex of the present invention:
(a) a coordination environment diagram of Ni metal; each Ni is hexa-coordinate;
(b) the Ni metal is bridged through a ligand to form a one-dimensional metal chain;
(c) the chains are connected through hydrogen bonds to form a three-dimensional stacking diagram;
FIG. 3 is an X-ray diffraction pattern of a sample;
FIG. 4 is a constant current charge-discharge diagram of a lithium ion battery prepared from the negative electrode material of the lithium battery of the present invention;
FIG. 5 is a charge-discharge cycle diagram of a lithium ion battery prepared from the negative electrode material for a lithium battery of the present invention;
FIG. 6 is a graph of rate performance of a lithium ion battery prepared from the lithium battery negative electrode material of the present invention.
Detailed Description
In order to further clarify the technical means and technical effects adopted by the present invention to achieve the predetermined objects, a specific embodiment of the method for preparing a complex-templated lithium ion battery negative electrode material according to the present invention is described below with reference to the following examples and drawings.
Example 1 Complex [ Ni (PBIM) (OH-BDC)]nAnd (4) synthesizing.
(1) Please refer to fig. 1, which is a diagram illustrating the steps of the synthesis reaction of the complex of the present invention.
Weighing Nickel acetate tetrahydrate (Ni (OAc)2·4H2O) (0.5mmol), 2,2' -Pyridyl Benzimidazole (PBIM) (0.1mmol), 5-hydroxyisophthalic acid (OH-BDC) (0.2mmol) and triethylamine (0.1mmol) are dissolved in 2mL of methanol and 6mL of water, the mixture is heated to 120 ℃ in a reaction kettle for reaction for 3 days, and the temperature is reduced to room temperature after the reaction is finished, thus obtaining complex crystals.
(2) Taking the crystals in the reaction kettle in the step 1, placing the crystals on a glass sheet, selecting transparent crack-free regular crystals with the size of 0.3X 0.5mm under a microscope, measuring on a Supernova type X-ray single crystal diffractometer, and using Mo-K α ray monochromated by a graphite monochromator
Is a source of incident radiation, in
The diffraction points were collected by scanning, their coordinates and their anisotropic parameters were corrected by the least squares method, the position of the hydrogen atoms was obtained by theoretical hydrogenation, and all calculations were performed using the SHELXL-97 and SHELXL-97 packages. The final molecular formula of the compound was determined by single crystal diffraction data analysis in combination with elemental analysis, thermogravimetric analysis, and Olex-2 software. The results show that: the structural formula of the metal-organic framework material is [ Ni (PBIM) (OH-BDC)]nWherein PBIM is 2,2' -pyridyl benzimidazole, OH-BDC is 5-hydroxyisophthalic acid, (wherein n is a natural number from 1 to positive infinity). Belonging to the monoclinic system, space group P21N, unit cell parameter of
α＝γ＝90°，β96.123(4) ° unit cell volume
Z＝4，Dc＝1.649g/cm3. Wherein each metal Ni is in a six-coordination structure and is respectively coordinated with two nitrogen from 2,2' -pyridyl benzimidazole and four oxygen from two 5-hydroxyisophthalic acid, the complex presents a one-dimensional zigzag chain structure, and the chains are connected into a three-dimensional structure through weak interaction of hydrogen bonds. The structure diagram is drawn by using Diamond software, as shown in FIG. 2, wherein (a) is [ Ni (PBIM) (OH-BDC) of the present invention]nThe coordination environment diagram of metallic nickel in the material; (b) is a one-dimensional zigzag pattern of the material of the invention; (c) is a three-dimensional structure diagram of the material of the present invention, which is formed by stacking hydrogen bonds.
(3) The greenish stripe crystals from step (1) were collected and referring to fig. 3, to further characterize the purity of the synthesized material, we tested the X-ray diffraction pattern of the complex. As can be seen from the figure, the diffraction patterns of a large number of synthesized samples are consistent with the X-ray diffraction patterns of simulated samples, and the purity of the compound is higher.
Example 2 Complex [ Ni (PBIM) (OH-BDC)]nApplication of negative electrode material in preparation of lithium ion battery
(4) And (2) drying the complex crystal prepared in the step (1) in a vacuum oven at 60 ℃ for 8 hours. Then weighing the dried complex [ Ni (PBIM) (OH-BDC) in a mass ratio of 6:3:1]nGrinding and uniformly mixing a conductive agent (ketjen black) and a binder (polyvinylidene fluoride), mixing into slurry by using a solvent (N-methylpyrrolidone), coating the slurry on a copper foil, and drying for 12 hours at the temperature of 80 ℃ in vacuum to obtain the electrode plate. And (4) selecting an MSK-T10 manual slicer with the mould size and the diameter of 12mm, slicing the obtained electrode slice to obtain a circular electrode slice, and weighing for later use.
(5) Using lithium plate as counter electrode, Celgard 2400 membrane as diaphragm, 1mol/L lithium hexafluorophosphate (LiPF)6) Assembling the lithium ion button cell by taking the circular electrode plate obtained in the step (4) as a negative electrode and taking Ethylene Carbonate (EC) and diethyl carbonate (DEC) as a solvent in a volume ratio as electrolyteAnd the battery model is CR 2032.
(6) And (3) electrochemical performance testing:
referring to fig. 4, it is a constant current charge-discharge diagram of a lithium ion battery prepared from the negative electrode material of the lithium battery of the present invention, and it can be seen from the diagram that the material as the negative electrode material of the lithium ion battery shows good charge-discharge performance with a current density of 100mA · g-1The first discharge capacity was 2989mAh g-1The first cycle charge capacity is 1241mAh g-1. At a current density of 100mA g-1The specific capacity can be stabilized at 1021mAh g after 150 times of charge-discharge circulation-1And the coulombic efficiency is higher, and the electrochemical performance is good. And at 500mA · g-1Circulating for 150 weeks, and the capacity is 600mAh g-1And the good cycle performance of the material is stably embodied, please refer to fig. 5.
(7) Please refer to fig. 6, which is a rate performance diagram of a lithium ion battery prepared from the negative electrode material of the lithium battery of the present invention. As can be seen from the graph, at a current density of 50mA g-1，100mA g-1，200mA g-1，500mA g-1，1000mA g-1Constant current charge and discharge were performed, and the number of cycles was 10 at each magnification. Under different current densities, the capacity values are respectively 1225, 1043, 942, 778, 572 and 284 mAh.g on average-1When the current density returns to 50mA g-1The capacity is still as high as 1286mAh g-1And the good rate performance of the material is shown.
Claims (4)
1. Coordination polymer [ Ni (PBIM) (OH-BDC)]nThe preparation method is characterized by comprising the following steps:
step (1): synthesizing a complex: nickel acetate tetrahydrate, 2' -pyridyl benzimidazole, 5-hydroxyisophthalic acid and triethylamine are mixed according to a molar ratio of 5: 1: 2: 1 is dissolved in a solvent with the volume ratio of 1:3, uniformly mixing the mixed solution of methanol and water to obtain a mixed solution, placing the mixed solution in a sealed stainless steel reaction kettle, heating to 120 ℃, reacting for 3 days, and cooling to room temperature after the reaction is finished to obtain a complex crystal;
step (2): taking the complex crystal obtained in the step (1) on a glass sheet, measuring on a single crystal instrument to obtain crystal data, analyzing the data by using Olex-2 software, and analyzing the crystal structure, wherein the chemical formula is [ Ni (PBIM) (OH-BDC)]nIn the formula: n is a natural number from 1 to infinity, and drawing a structure diagram by utilizing Diamond software; wherein PBIM is 2,2' -pyridyl benzimidazole, OH-BDC is 5-hydroxyisophthalic acid.
2. The process for preparing a coordination polymer according to claim 1, wherein said step (2) is specifically performed by: placing the complex crystals obtained in step 1 on a glass slide, selecting transparent crystals with a regular shape and no cracks with a size of 0.3 × 0.5mm under a microscope, measuring on a Supernova X-ray single crystal diffractometer, and monochromating with a graphite monochromator
Is taken as an incident radiation source, so that Mo-K α rays are taken as an incident radiation source
Collecting diffraction points in a scanning mode, correcting coordinates and anisotropic parameters thereof by a least square method, obtaining the position of a hydrogen atom by theoretical hydrogenation, and completing all analysis and refinement by a SHELXL-97 program; the final molecular formula of the coordination polymer is determined by combining element analysis, thermogravimetric analysis and data single crystal diffraction data analysis of Olex-2 software, and the result shows that the structural formula of the coordination polymer material is [ Ni (PBIM) (OH-BDC)]nBelonging to the monoclinic system, space group P21/n, cell parameter is
α γ 90 °, β 96.123(4 °), unit cell volume is
Z＝4，Dc＝1.649g/cm3Wherein each metal is NiBoth are hexa-coordination structures, and are respectively coordinated with two nitrogen from 2,2' -pyridyl benzimidazole and four oxygen from two 5-hydroxyisophthalic acid, the complex presents a one-dimensional zigzag chain structure, and the chains are connected into a three-dimensional structure through weak interaction of hydrogen bonds.
3. The complex [ Ni (PBIM) (OH-BDC) synthesized by the method of claim 1]nThe application of the material as a negative electrode material in preparing an electrode plate is characterized by comprising the following steps: weighing the complex crystal [ Ni (PBIM) (OH-BDC) synthesized by the method of claim 1]nDrying in a vacuum oven at 60 ℃ for 8 hours; weighing the dried complex, a conductive agent ketjen black and a binder polyvinylidene fluoride according to a mass ratio of 6:3:1, grinding and mixing uniformly, mixing into a slurry by using a solvent N-methyl pyrrolidone, coating the slurry on a copper foil, drying for 12 hours at a vacuum temperature of 80 ℃, and slicing to obtain a circular electrode slice; the method is applied to the negative electrode material of the lithium ion battery.
4. The use of the electrode sheet prepared according to claim 3 in the preparation of a lithium ion battery, characterized by comprising the steps of: using lithium plate as counter electrode, Celgard 2400 membrane as diaphragm, 1mol/L lithium hexafluorophosphate (LiPF)6) The lithium ion button cell is assembled by taking the electrode plate prepared in the claim 3 as a negative electrode and taking Ethylene Carbonate (EC) and diethyl carbonate (DEC) as the electrolyte with the volume ratio of 1:1 as a solvent, and the cell model is CR 2032.
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| CN108666573A (en) * | 2018-04-23 | 2018-10-16 | 曲靖师范学院 | A kind of preparation method of titanium-based MOF lithium ion battery negative materials |
| CN108933237B (en) * | 2018-06-01 | 2021-01-15 | 南开大学 | Preparation method and application of lithium ion battery positive electrode material |
| CN109273714B (en) * | 2018-09-21 | 2021-03-26 | 南开大学 | Preparation and application of metal organic framework material with excellent lithium storage performance |
| CN109273715B (en) * | 2018-09-21 | 2020-08-04 | 南开大学 | Preparation method of coordination polymer based on 2, 6-dipicolinic acid and application of coordination polymer in lithium ion battery |
| CN110554011B (en) * | 2019-08-22 | 2020-12-18 | 武汉大学 | Visual water fluorescence microsensor based on dual-response lanthanide MOF, water determination pipe device, water visualization determination device and application thereof |
| CN110527107A (en) * | 2019-08-27 | 2019-12-03 | 深圳大学 | A kind of orderly two-dimentional electroconductive molecule monolayer array preparation method and photoelectric device |
| CN112745512B (en) * | 2021-02-07 | 2022-06-07 | 河南农业大学 | Copper metal-organic framework material based on metal copper and application thereof |
| CN113336802B (en) * | 2021-05-31 | 2022-05-17 | 苏州大学 | Organic sulfur molecule based on nickel-mercaptobenzimidazole coordination compound, and preparation method and application thereof |
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