CN107665993A - A kind of synthesis of coordination polymer and its application in lithium ion battery negative material - Google Patents
A kind of synthesis of coordination polymer and its application in lithium ion battery negative 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
- H01—ELECTRIC ELEMENTS
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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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Abstract
The invention discloses a kind of synthesis of coordination polymer and its application in lithium ion battery negative material, the chemical formula of the complex is [Ni (PBIM) (OH BDC)]n(in formula：N arrives just infinite natural number for 1), wherein PBIM is 2,2' pyridine radicals benzimidazoles, OH BDC are 5 Hydroxy M Phthalic Acids, the preparation method of complex is to be hydrated nickel acetate, 2,2' pyridine radicals benzimidazoles by four, 5 Hydroxy M Phthalic Acids and triethylamine are added in water and methanol mixed solution, and target product complex [Ni (PBIM) (OH BDC)] is obtained through hydro-thermal reactionn；It can be used in lithium ion battery negative material.It is an advantage of the invention that：Obtained complex synthetic method is simple, and raw material is easy to get, easily operated, reaction condition is gentle, yield is high, cost is low, and product has preferable stability, is directly used in lithium cell cathode material, shows good chemical property.
Description
Technical field
The present invention relates to cell art, and in particular to a kind of conjunction of the coordination polymer material with good stability
Into negative electrode of lithium ion battery and preparation method of lithium ion battery.
Background technology
With the development of economy and society, also extremely urgent for the demand of the high-efficiency cleaning energy, lithium ion battery is as first
Enter energy storage device, because of its light weight, small volume, be easy to carry, operating voltage is high, and bigger than energy, self discharge is small, cycle life
It is long, safe, memory-less effect, outstanding advantages of non-environmental-pollution, turn into video camera, mobile phone, notebook computer with
And the ideal source of the electronic installation miniaturization such as Portable Measurement Instrument, and the first choice of future automobile high-energy power battery
Power supply.Lithium ion battery is by positive pole, negative pole, electrolyte and barrier film composition.Because positive and negative pole material is the pass of decision battery performance
Key, and using graphene be leading commercialization negative material because theoretical capacity is low and safety issue, can not meet current
Demand of the society to the energy.Seek with high power capacity, the electrode material of the stabilization of low discharge voltage platform is current research heat
Point.And more oxide is studied at present, and sulfide, phosphide etc., although having in specific capacity and cycle performance certain excellent
Gesture, but caused huge volumetric expansion is to limit the bottleneck of its development in charge and discharge process.
Coordination polymer (abbreviation complex) is a kind of organic-inorganic hybrid material, due to the metal ion of assembling and organic
The alternative of part and show structure diversity, because its abundant functional group and open metallic site are in gas absorption point
All it is widely used from, catalysis, magnetic, the various fields such as fluorescence.In electrochemical field, complex material and its derivative also by
To increasing concern.Complex is directly applied into lithium ion battery, synthetic method is simple, and due to complex in itself
Structure diversity, metal and part are all potential removal lithium embedded sites and turn into focus.But in the cooperation reported at present
It is the dissolubility difference of material and the problems such as specific capacity is low that thing, which directly applies to mainly faced in lithium ion battery,.Overcome these
Problem is very helpful to the development for promoting electrode material.
The content of the invention
First purpose of the present invention is to be directed to above technical Analysis, there is provided one kind is applied to lithium ion battery negative material
Coordination polymer preparation method, solve the problems, such as to be applied at present present in battery dissolubility difference and specific capacity be low.
Second object of the present invention is to provide a kind of electrode slice using above-mentioned negative material.
Third object of the present invention is to provide a kind of lithium ion battery using above-mentioned negative material electrode slice.
The present invention is achieved by the following technical solutions：
First, a kind of synthetic method of new complex, comprises the following steps：
Step (1)：Complex [Ni (PBIM) (OH-BDC)]n(in formula：N is 1 to arrive just infinite natural number) synthesis.
Four hydration nickel acetates are weighed, 2,2'- pyridine radicals benzimidazoles, 5- Hydroxy M Phthalic Acids and triethylamine are dissolved in body
Product is than being 1:It is well mixed to obtain mixed liquor in the mixed solution of 3 first alcohol and water, it is placed in 23mL sealing stainless steel cauldrons
In, it is heated to 120 degrees Celsius and reacts 3 days, reaction is down to room temperature after terminating, and obtains complex crystal.Refer in Fig. 1 present invention
The synthetic reaction block diagram of complex.
Wherein four are hydrated the mol ratio of nickel acetates, 2,2'- pyridine radicals benzimidazole, 5- Hydroxy M Phthalic Acids and triethylamine
For 5：1：2：1；The volume ratio of first alcohol and water is 1：3.
Step (2)：It on sheet glass, selecting size is under the microscope 0.3*0.5* to take in step 1 in reactor crystal
The crystal of the transparent flawlesses of 0.5mm, measured on Supernova type X ray single crystal diffractometers, using by graphite monochromatic
The Mo-K alpha rays of device monochromatizationFor Incident Irradiation Source, withScan mode collects point diffraction, by minimum
Their coordinate and its anisotropic parameters of square law amendment, the position of hydrogen atom are obtained by theory hydrogenation, and all calculating makes
Carried out with SHELXL-97 and SHELXL-97 program bags.With reference to elementary analysis, thermogravimetric analysis, and Olex-2 softwares carry out data
Single crystal diffraction data analysis, to determine the final molecular formula of the compound.As a result show：The knot of the metal-organic framework materials
Structure formula is [Ni (PBIM) (OH-BDC)]n(in formula：N arrives just infinite natural number for 1), wherein PBIM is 2,2'- pyridine radicals benzene
And imidazoles, OH-BDC are 5- Hydroxy M Phthalic Acids, belong to monoclinic system, space group P21/ n, cell parameter areα=γ=90 °, β=96.123 (4) °, unit cell volume areZ=4, Dc=1.649g/cm3, wherein each W metal is hexa-coordinate structure, respectively with from 2,2'-
Two nitrogen of pyridine radicals benzimidazole and four oxygen coordination on two 5- Hydroxy M Phthalic Acids, complex show one
The word chain structure of dimension, interchain connect into three-dimensional structure by hydrogen bond weak interaction.Fig. 3 is big after the operation of step 1
Sample X-ray diffractogram is measured, illustrating the X-ray diffractogram of the diffraction pattern and the sample by simulation of the substantial amounts of sample of synthesis is
Consistent, thus illustrate that the complex purity of synthesis is higher.
2nd, complex [Ni (PBIM) (OH-BDC)]nAs application of the negative material in electrode slice is prepared
The complex crystal 60 degrees Celsius of dryings in vacuum drying oven prepared in step (1) are taken, are dried 8 hours.Then with
6:3:1 mass ratio weighs dried complex [Ni (PBIM) (OH-BDC)]n, conductive agent (ketjen black) and bond
Agent (Kynoar) ground and mixed is uniform, is tuned into pulpous state with solvent (1-METHYLPYRROLIDONE), is coated on copper foil, vacuum 80 is taken the photograph
Family name's degree is dried 12 hours, and section obtains circular electric pole piece.Concrete operations are to choose the MSK-T10 that mould diameter is 12mm to cut manually
Piece machine cuts into slices obtained electrode slice to obtain circular pole piece, and it is standby to weigh.
3rd, the application using above-mentioned negative material electrode slice in lithium ion battery preparation
Using lithium piece, 1mol/L hexafluoro closes lithium phosphate (LiPF for electrode, the films of Celgard 2400 are barrier film6) it is electricity
Xie Zhi, volume ratio ethylene carbonate (EC):Diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, with the circular electric weighed
Pole piece is that negative pole assembles lithium ion button shape cell, battery size CR2032.
Electrochemical property test：Temperature is room temperature during test, and the voltage range in constant current charge-discharge test is 0.01-
3V, charge and discharge cycles number is 150 times in cycle performance test, current density 100mAg-1, surveyed respectively in high rate performance test
It is 50mA g to have tried in current density-1, 100mA g-1, 200mA g-1, 500mA g-1, 1000mA g-1, 50mA g-1Lower progress
Constant current charge-discharge, and cycle-index is 10 times under each multiplying power.
The advantages of the present invention：
(1) compared with traditional lithium ion battery negative material (graphite), using the complex that the present invention synthesizes as electricity
Battery prepared by pond negative material, improves a lot in terms of specific capacity, is 100mAg in current density-1When, by 150
Secondary charge and discharge cycles, specific capacity is still in 1021mAhg-1。
(2) battery prepared by the present invention improves a lot in stability, is 100mAg in current density-1When, pass through
150 charge and discharge cycles, capability retention 84.21%, its specific capacity can be stablized in 1021mAhg-1Left and right.Show good
Good chemical property, and in 500mAg-1When, circulate 150 weeks, capacity is in 600mAhg-1Left and right simultaneously keeps stable, simultaneously
Coulombic efficiency is up to 99%, embodies the good cycle performance of material.High rate performance test similarly proves complex of the present invention
Electrochemical stability.
Brief description of the drawings
Fig. 1 is the synthetic reaction block diagram of complex in the present invention；
Fig. 2 is the structural analysis figure of complex in the present invention：
(a) coordination context diagram of Ni metals；Each Ni is hexa-coordinate；
(b) Ni metals form one-dimensional metallic bond by part bridging；
(c) interchain is connected by hydrogen bond, forms three-dimensional accumulation graph；
Fig. 3 is sample X-ray diffractogram；
Fig. 4 is the constant current charge-discharge figure of lithium ion battery prepared by the lithium cell cathode material of the present invention；
Fig. 5 is the charge and discharge cycles figure of lithium ion battery prepared by the lithium cell cathode material of the present invention；
Fig. 6 is the high rate performance figure of lithium ion battery prepared by the lithium cell cathode material of the present invention.
Embodiment
Further to illustrate the present invention to reach technological means and its technique effect that predetermined goal of the invention is taken, with
Under in conjunction with the embodiments and accompanying drawing, to a kind of preparation using complex as the lithium ion battery negative material of template proposed by the present invention
The embodiment of method illustrates.
Embodiment 1, complex [Ni (PBIM) (OH-BDC)]nSynthesis.
(1) referring to Fig. 1, it is the synthetic reaction block diagram of complex in the present invention.
Weigh four hydration nickel acetates (Ni (OAc)2·4H2O) (0.5mmol), 2,2'- pyridine radicals benzimidazoles (PBIM)
(0.1mmol), 5- Hydroxy M Phthalic Acids (OH-BDC) (0.2mmol), triethylamine (0.1mmol) are dissolved in 2mL methanol and 6mL
In water, 120 degrees Celsius are heated in reactor and is reacted 3 days, reaction is down to room temperature after terminating, and obtains complex crystal.
(2) it on sheet glass, selecting size is under the microscope 0.3*0.5*0.5mm to take in step 1 in reactor crystal
Transparent flawless regular shape crystal, measured on Supernova type X ray single crystal diffractometers, using by graphite list
The Mo-K alpha rays of color device monochromatizationFor Incident Irradiation Source, withScan mode collects point diffraction, by most
Their coordinate and its anisotropic parameters of small square law amendment, the position of hydrogen atom are obtained by theory hydrogenation, all calculating
Carried out using SHELXL-97 and SHELXL-97 program bags.With reference to elementary analysis, thermogravimetric analysis, and Olex-2 softwares enter line number
According to single crystal diffraction data analysis, to determine the final molecular formula of the compound.As a result show：The metal-organic framework materials
Structural formula is [Ni (PBIM) (OH-BDC)]n, wherein PBIM is 2,2'- pyridine radicals benzimidazoles, and OH-BDC is 5- hydroxyl isophthalic
Dioctyl phthalate, (in formula：N arrives just infinite natural number for 1).Belong to monoclinic system, space group P21/ n, cell parameter areα=γ=90 °, β=96.123 (4) °, unit cell volume
ForZ=4, Dc=1.649g/cm3.Wherein each W metal is hexa-coordinate structure, respectively with from 2,
Two nitrogen of 2'- pyridine radicals benzimidazoles and four oxygen coordination on two 5- Hydroxy M Phthalic Acids, complex are presented
Go out one-dimensional word chain structure, interchain connects into three-dimensional structure by hydrogen bond weak interaction.Tied using Diamond softwares
Composition is drawn, as shown in Fig. 2 (a) is [Ni (PBIM) (OH-BDC)] of the invention in figurenThe coordination environment of metallic nickel in material
Figure；(b) be material in the present invention one-dimensional word chain figure；(c) it is that the three-dimensional that material is formed by hydrogen bond accumulation in the present invention is tied
Composition.
(3) the light green color web crystal that collection step (1) obtains, referring to Fig. 3, being the pure of further characterization synthetic material
Degree, we test the x-ray diffraction pattern of complex.It can be seen that the diffraction pattern and warp of the substantial amounts of sample of synthesis
It is consistent to cross the X-ray diffractogram of the sample of simulation, and the purity of compound is higher.
Embodiment 2, complex [Ni (PBIM) (OH-BDC)]nAs application of the negative material in lithium ion battery preparation
(4) the complex crystal 60 degrees Celsius of dryings in vacuum drying oven prepared in step (1) are taken, are dried 8 hours.Then
With 6:3:1 mass ratio weighs dried complex [Ni (PBIM) (OH-BDC)]n, conductive agent (ketjen black) and viscous
It is uniform to tie agent (Kynoar) ground and mixed, is tuned into pulpous state with solvent (1-METHYLPYRROLIDONE), is coated on copper foil, vacuum 80
Degree Celsius dry 12 hours, obtain electrode slice.Choosing die size a diameter of 12mm MSK-T10 hand microtomes will obtain
Electrode slice cuts into slices to obtain circular electric pole piece, and it is standby to weigh.
(5) using lithium piece, 1mol/L hexafluoro closes lithium phosphate (LiPF for electrode, the films of Celgard 2400 are barrier film6)
For electrolyte, volume ratio ethylene carbonate (EC):Diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, with step (4)
Obtained circular electric pole piece is that negative pole assembles lithium ion button shape cell, battery size CR2032.
(6) electrochemical property test：
Referring to Fig. 4, the constant current charge-discharge figure of lithium ion battery prepared by the lithium cell cathode material that it is the present invention,
It can be seen that this material as lithium ion battery negative material, shows good charge-discharge performance, it is close in electric current
Spend for 100mAg-1When, discharge capacity is 2989mAhg first-1, first all charging capacitys are 1241mAhg-1.It is close in electric current
Spend for 100mAg-1When, by 150 charge and discharge cycles, its specific capacity can be stablized in 1021mAhg-1Left and right, coulombic efficiency
It is higher, show good chemical property.And in 500mAg-1When, circulate 150 weeks, capacity is in 600mAhg-1Left and right,
And keep stable and embody the good cycle performance of material, refer to Fig. 5.
(7) referring to Fig. 6, the high rate performance figure of lithium ion battery prepared by the lithium cell cathode material that it is the present invention.
It can be seen that it is 50mA g in current density-1, 100mA g-1, 200mA g-1, 500mA g-1, 1000mA g-1Under enter
Row constant current charge-discharge, and cycle-index is 10 times under each multiplying power.Under different current densities, its capability value difference average out to
1225,1043,942,778,572,284mAhg-1, when current density returns to 50mA g-1When, capacity is still up to 1286mAh
g-1, show the good high rate performance of material.
Claims (4)
- A kind of 1. coordination polymer [Ni (PBIM) (OH-BDC)]nPreparation method, it is characterised in that comprise the following steps：Step (1)：Synthetic compound：Nickel acetate, 2,2'- pyridine radicals benzimidazole, 5- Hydroxy M Phthalic Acids and triethylamine are hydrated by four to press It is 5 according to mol ratio：1：2：1 is dissolved in volume ratio as 1：It is well mixed in the mixed solution of 3 first alcohol and water, obtains mixed liquor, Mixed liquor is placed in sealing stainless steel cauldron, 120 degrees Celsius is heated to and reacts 3 days, reaction is down to room temperature after terminating, and obtains Complex crystal；Step (2)：The complex crystal that step (1) obtains is taken to be measured on monocrystalline instrument on sheet glass, obtain number of crystals According to using the progress data analysis of Olex-2 softwares, parsing crystal structure, chemical formula is [Ni (PBIM) (OH-BDC)]n, in formula：n Just infinite natural number is arrived for 1, structure chart drafting is carried out using Diamond softwares；Wherein PBIM is 2,2'- pyridine radicals benzo miaows Azoles, OH-BDC are 5- Hydroxy M Phthalic Acids.
- 2. according to the synthetic method of the coordination polymer described in claim 1, it is characterised in that the step (2) it is specific Operation is as follows：It on sheet glass, selecting size is under the microscope 0.3*0.5* to take the complex crystal obtained in step 1 The crystal of the transparent flawless regular shapes of 0.5mm, measured on Supernova type X ray single crystal diffractometers, use process Graphite monochromator monochromatizationMo-K alpha rays be Incident Irradiation Source, withScan mode collects point diffraction, By least square refinement coordinate and its anisotropic parameters, the position of hydrogen atom is obtained by theory hydrogenation, all calculating Carried out using SHELXL-97 and SHELXL-97 program bags；With reference to elementary analysis, thermogravimetric analysis, and Olex-2 softwares enter line number According to single crystal diffraction data analysis, to determine the final molecular formula of the compound, the results showed that:The metal-organic framework materials Structural formula is [Ni (PBIM) (OH-BDC)]n, belong to monoclinic system, space group P21/n, cell parameter isα=γ=90 °, β=96.123 (4) °, unit cell volume areZ=4, Dc=1.649g/cm3, wherein each W metal is hexa-coordinate structure, respectively with from 2,2'- Two nitrogen of pyridine radicals benzimidazole and four oxygen coordination on two 5- Hydroxy M Phthalic Acids, complex show one The word chain structure of dimension, interchain connect into three-dimensional structure by hydrogen bond weak interaction.
- 3. the complex [Ni (PBIM) (OH-BDC)] of claim 1 methods described synthesisnElectrode slice is being prepared as negative material In application, it is characterised in that comprise the following steps：Weigh the complex crystal [Ni of claim 1 methods described synthesis (PBIM)(OH-BDC)]n60 degrees Celsius of dryings in vacuum drying oven, dry 8 hours；With 6:3:1 mass ratio weighs above-mentioned baking Complex after dry, conductive agent ketjen black and binding agent Kynoar ground and mixed are uniform, with Solvents N-methyl pyrrole Pyrrolidone is tuned into pulpous state, is coated on copper foil, the drying 12 hours of 80 degrees Celsius of vacuum, and section obtains circular electric pole piece；It is applied to lithium In ion battery cathode material.
- 4. the application of electrode slice prepared by claim 3 in lithium ion battery preparation, it is characterised in that comprise the following steps： Using lithium piece, 1mol/L hexafluoro closes lithium phosphate (LiPF for electrode, the films of Celgard 2400 are barrier film6) it is electrolyte, body Product is than ethylene carbonate (EC):Diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, with the electrode slice of claim 2 preparation Lithium ion button shape cell, battery size CR2032 are assembled for negative pole.
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Cited By (8)
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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 |
| CN108933237A (en) * | 2018-06-01 | 2018-12-04 | 南开大学 | A kind of preparation method and application of anode material for lithium-ion batteries |
| CN109273714A (en) * | 2018-09-21 | 2019-01-25 | 南开大学 | A kind of preparation and application of the metal-organic framework material with excellent storage lithium performance |
| CN109273715A (en) * | 2018-09-21 | 2019-01-25 | 南开大学 | A kind of preparation method of the coordination polymer based on 2,6- pyridinedicarboxylic acid and its application in lithium ion battery |
| 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 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108933237A (en) * | 2018-06-01 | 2018-12-04 | 南开大学 | A kind of preparation method and application of anode material for lithium-ion batteries |
| CN108933237B (en) * | 2018-06-01 | 2021-01-15 | 南开大学 | Preparation method and application of lithium ion battery positive electrode material |
| CN109273714A (en) * | 2018-09-21 | 2019-01-25 | 南开大学 | A kind of preparation and application of the metal-organic framework material with excellent storage lithium performance |
| CN109273715A (en) * | 2018-09-21 | 2019-01-25 | 南开大学 | A kind of preparation method of the coordination polymer based on 2,6- pyridinedicarboxylic acid and its application in lithium ion battery |
| 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 |
| CN110554011A (en) * | 2019-08-22 | 2019-12-10 | 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 |
| 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 |
| CN112745512A (en) * | 2021-02-07 | 2021-05-04 | 河南农业大学 | Copper metal-organic framework material based on metal copper and preparation method and application thereof |
| CN113336802A (en) * | 2021-05-31 | 2021-09-03 | 苏州大学 | Organic sulfur molecule based on nickel-mercaptobenzimidazole coordination compound, and preparation method 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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