CN108192106A - A kind of synthesis of coordination polymer containing F and its application in lithium ion battery negative material - Google Patents
A kind of synthesis of coordination polymer containing F and its application in lithium ion battery negative material Download PDFInfo
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- CN108192106A CN108192106A CN201711469139.0A CN201711469139A CN108192106A CN 108192106 A CN108192106 A CN 108192106A CN 201711469139 A CN201711469139 A CN 201711469139A CN 108192106 A CN108192106 A CN 108192106A
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Abstract
A kind of synthesis of coordination polymer containing F and its application in lithium ion battery negative material.Coordination polymer chemical formula is [Co (tfbdc) (EtOH)2]n, wherein tfbdc2‑For tetrafluoro terephthaldehyde's acid ion；Preparation method is by cabaltous nitrate hexahydrate, and tetrafluoro terephthalic acid (TPA) is added in absolute ethyl alcohol, and hydro-thermal reaction obtains target product；Electrode slice is can be made into, is assembled into CR2032 lithium ion button shape cells in negative material.The present invention can be directly used as lithium ion battery negative material by synthesizing a kind of coordination polymer containing F.Complex synthetic method is simple, and raw material is cheap and easy to get, and yield is high, and characterization is convenient.The negative material being prepared has good chemical property.When charging and discharging currents density is 100mA/g, the specific capacity of complex maintains 865mAh/g after recycling 60 times.Multiplying power also embodies good stability and excellent chemical property when testing.
Description
Technical field
The present invention relates to battery technology fields, and in particular to a kind of coordination polymer material containing F with good stability
Synthesis, negative electrode of lithium ion battery and preparation method of lithium ion battery.
Background technology
Lithium ion battery be after nickel oxygen, a kind of mechanism of new electrochemical power sources to grow up after nickel-cadmium cell, have high voltage,
High-energy, the features such as small, internal resistance is small, self discharge is small, have extended cycle life, memory-less effect, it is referred to as " environmentally protective electricity
Source ".With reference to the development of present society and the requirement of novel electric appliance, lithium ion battery is according to high-energy density and high capacitive property
And as an important directions of new energy research work, to its research work also just in progress like a raging fire.Lithium ion
The performance of battery depends primarily on the structure and performance of inside battery material.These inside battery materials include negative material, electricity
Xie Zhi, diaphragm and positive electrode etc..Wherein the selection of positive and negative electrode material directly determines the performance and price of lithium ion battery.Cause
The research of this cheap, high performance positive and negative electrode material is always the emphasis of lithium ion battery industry development.Ideal lithium-ion electric
Pond negative material should be able to accommodate a large amount of Li+, there is higher ionic conductivity and electronic conductivity and good steady
It is qualitative etc..Existing negative material is difficult to meet above-mentioned requirements simultaneously, therefore, researches and develops chemical property preferably novel cathode material
Material and the research hotspot for being modified always lithium ion battery negative material field to having material.
Coordination polymer is that a kind of had by metal ion or metal cluster with organic ligand by what self assembly mode was formed
Machine inorganic hybrid material, because its adjustable changeable chemical constitution and excellent performance have obtained people and widely paid close attention to.In gas
Body stores and separation, and catalysis, fluorescence is magnetic, proton conduction, and drug delivery etc. is all widely used.In terms of electrochemistry,
The advantages that coordination polymer synthetic method is simple, at low cost, and metal and ligand are all potential storage lithium sites makes it successfully should
For lithium ion battery.Meanwhile crystallographic characteristics also largely ensure that structural stability, improve following for battery
Ring performance, therefore, it has become more potential electrode materials.But the complex reported at present is applied to lithium ion battery battery
During the material of pole, poorly conductive and specific capacity it is low be the practical critical issue of limitation input.Solve the problems, such as these to electrode material
Development have important impetus.
Invention content
Present invention aim to address existing complex electrode material there are the problem of poorly conductive and low specific capacity, carry
For a kind of simple, the at low cost coordination polymer containing F of synthesis, and it is applied to lithium ion battery as cell negative electrode material.
Due to F-With very strong electronegativity, it is easier and Li+With reference to, therefore the complex can effectively overcome at present
Coordination polymer is applied to the shortcomings that specific capacity existing for lithium ion battery is low and stability is poor.
Technical scheme of the present invention：
A kind of coordination polymer containing F, chemical formula are [Co (tfbdc) (EtOH)2]n, in formula：N be 1 to it is just infinite from
So number, tfbdc2-For tetrafluoro terephthaldehyde's acid ion；The coordination polymer is by Co2+Ion and organic ligand tfbdc2-By matching
Position key forms two-dimensional layered structure；The Co of a crystallography independence is included in minimum asymmetric cell2+, a tfbdc2-Ligand
With the ethanol molecule of two coordinations；Adjacent Co2+Pass through tfbdc between ion2-Ligand bridging is into two-dimension plane structure.
A kind of synthetic method of the coordination polymer containing F, includes the following steps：
1) cabaltous nitrate hexahydrate Co (NO are weighed3)2·6H2O and tetrafluoro terephthalic acid (TPA) (H2Tfbdc) it is dissolved in anhydrous second
In alcohol, mixed liquor is obtained after stirring；
2) above-mentioned mixed liquor is placed in autoclave and is heated to 80-100 degrees Celsius, heating reaction 2-4 days, reaction is tied
Room temperature is down to after beam, it is the coordination polymer containing F that purple powder bulk crystals, which are obtained by filtration,；
Cabaltous nitrate hexahydrate Co (NO in mixed liquor described in step 13)2·6H2O and tetrafluoro terephthalic acid (TPA) (H2tfbdc)
Molar ratio is (1-3):1；The amount ratio of cabaltous nitrate hexahydrate and absolute ethyl alcohol is (0.05-0.2) mmol：(2-6)mL.
A kind of application of coordination polymer containing F as negative material in lithium ion battery is prepared, specific method are：Match
Position polymer 60 degrees Celsius of dryings 5 hours first in vacuum drying oven.Then according to 7:2:1 mass ratio weighs polycomplexation respectively
Object, Ketjen black and Kynoar are closed, the uniform pulp of ground and mixed after N-Methyl pyrrolidone is added in, is coated on copper foil,
The drying 12 hours of 60 degrees Celsius of vacuum, is cut into the circle of 12 millimeters of diameter as negative plate；Obtained round negative plate is with lithium
Piece is used as to electrode, and 2400 films of Celgard are diaphragm, and 1mol/L hexafluoros close lithium phosphate (LiPF6) ethylene carbonate (EC)/
Diethyl carbonate (DEC) solution is electrolyte, and the volume ratio of wherein ethylene carbonate (EC) and diethyl carbonate (DEC) is 1:1,
It is assembled into CR2032 lithium ion button shape cells.
Assembled lithium ion battery is tested on blue electric battery test system.Temperature is room temperature during test, permanent
Voltage range in current charge-discharge electrical testing is 0.01-3V.The coordination polymer is tested respectively as negative electrode of lithium ion battery material
During material, current density is 100mA g-1Under constant current charge-discharge performance and cycle performance and high current density be 500mA
g-1Under cycle performance.It is respectively 100,200,500,1000,2000mA g in current density-1When high rate performance.
It is an advantage of the invention that：
By synthesizing a kind of coordination polymer containing F, and it is directly used as lithium ion battery negative material.Complex synthesizes
Method is simple, and raw material is cheap and easy to get, and yield is high, and characterization is convenient.In addition, more traditional lithium ion battery negative material (stone
Ink), the negative material being prepared is due to F-With very strong electronegativity, it is easier and Li+With reference to good electrification
Learn performance.When charging and discharging currents density is 100mA/g, the specific capacity of the complex maintains 865mAh/ after recycling 60 times
g.Good stability and excellent chemical property are also embodied when multiplying power is tested.
Description of the drawings
Fig. 1 is the synthetic reaction block diagram of complex in the present invention.
Fig. 2 and Fig. 3 is the structural analysis figure of complex in the present invention, wherein：Fig. 2 is the coordination context diagram of metal Co, often
A Co is hexa-coordinate；Fig. 3 passes through ligand bridging, the two-dimensional layered structure of formation for metal Co.
Fig. 4 is the X-ray diffractogram of complex in the present invention.
Fig. 5 is constant current charge-discharge figure when complex is as lithium ion battery negative material in the present invention.
Fig. 6 is charge and discharge cycles figure when complex is as lithium ion battery negative material in the present invention.
Fig. 7 is high rate performance figure when complex is as lithium ion battery negative material in the present invention.
Fig. 8 is the charge and discharge cycles figure under high current when complex is as lithium ion battery negative material in the present invention.
Specific embodiment
First, the coordination polymer containing F, chemical formula are [Co (tfbdc) (EtOH)2]n, in formula：N is 1 to just infinite nature
Number, tfbdc2-For tetrafluoro terephthaldehyde's acid ion；The coordination polymer is by Co2+Ion is formed with organic ligand by coordinate bond
Two-dimensional layered structure, wherein organic ligand are tetrafluoro terephthalic acid (TPA)；A crystallography independence is included in minimum asymmetric cell
Co2+, a tfbdc2-Ligand and the ethanol molecule of two coordinations；Adjacent Co2+Pass through tfbdc between ion2-Ligand bridging
Into two-dimension plane structure.
2nd, the synthetic method of the coordination polymer containing F, referring to Fig. 1, specific synthetic method is as follows：
Embodiment 1：
1) cabaltous nitrate hexahydrate Co (NO are weighed3)2·6H2O (29.0mg, 0.1mmol), tetrafluoro terephthalic acid (TPA)
(H2Tfbdc) (11.9mg, 0.05mmol) is dissolved in 4mL absolute ethyl alcohols, and mixed liquor is obtained after stirring evenly；
2) above-mentioned mixed liquor be placed in 25mL autoclaves be heated to 90 degrees Celsius react 3 days, be down to after reaction
Room temperature, it is the coordination polymer containing F that purple powder bulk crystals, which are obtained by filtration,.
Embodiment 2：
1) cabaltous nitrate hexahydrate Co (NO are weighed3)2·6H2O (14.5mg, 0.05mmol), tetrafluoro terephthalic acid (TPA)
(H2Tfbdc) (11.9mg, 0.05mmol) is dissolved in 2mL absolute ethyl alcohols, and mixed liquor is obtained after stirring evenly；
2) above-mentioned mixed liquor be placed in 25mL autoclaves be heated to 80 degrees Celsius react 2 days, be down to after reaction
Room temperature, it is the coordination polymer containing F that purple powder bulk crystals, which are obtained by filtration,.
Embodiment 3：
1) cabaltous nitrate hexahydrate Co (NO are weighed3)2·6H2O (43.5mg, 0.15mmol), tetrafluoro terephthalic acid (TPA)
(H2Tfbdc) (11.9mg, 0.05mmol) is dissolved in 6mL absolute ethyl alcohols, and mixed liquor is obtained after stirring evenly；
2) above-mentioned mixed liquor be placed in 25mL autoclaves be heated to 100 degrees Celsius react 4 days, be down to after reaction
Room temperature, it is the coordination polymer containing F that purple powder bulk crystals, which are obtained by filtration,.
3rd, the structure determination of the coordination polymer for containing F：
The crystal that two embodiment 1 of above-mentioned steps obtains is taken to select suitable crystal under the microscope on glass slide,
It is tested on Supernova type X ray single crystal diffractometers, with the Mo-K alpha rays Jing Guo graphite monochromator monochromatizationFor Incident Irradiation Source, withScan mode collects point diffraction, by their coordinate of least square refinement
And its anisotropic parameters, the position of hydrogen atom are obtained by theory plus hydrogen, all calculating uses SHELXL-97 and SHELXL-
97 program bags carry out.Crystallographic structural analysis is carried out according to Olex-2 softwares, with reference to elemental analysis, thermogravimetric analysis is final to determine to be somebody's turn to do
The structural formula of complex is [Co (tfbdc) (EtOH)2]n(H2Tfbdc is tetrafluoro terephthalic acid (TPA)).The complex belongs to monocline
Crystallographic system, space group P21/ n, cell parameter are α=γ=
90 °, β=103.106 (6) °, unit cell volume isZ=2, Dc=1.742g/cm3.The coordination polymer is by Co2+
Ion forms two-dimensional layered structure with organic ligand by coordinate bond, and wherein organic ligand is tetrafluoro terephthalic acid (TPA)；Minimum is not
The Co of a crystallography independence is included in symmetrical cell2+, a tfbdc2-Ligand and the ethanol molecule of two coordinations；Adjacent
Co2+Pass through tfbdc between ion2-Ligand bridging is into two-dimension plane structure.Structure chart is to utilize Diamond Software on Drawing.Fig. 2
It is the coordination context diagram of the central metal cobalt of complex in the present invention；3 be the two-dimensional layered structure figure of complex.
4th, the characterization of coordination polymer purity：
Complex, which is largely collected, according to 1 the method for embodiment obtains purple powder crystal.For further characterization synthesis cooperation
The purity of object, we test the x-ray diffraction pattern of complex.Referring to Fig. 4, it can be seen from the figure that is synthesized is a large amount of
The diffraction pattern of sample shows the complex purity of synthesis with being consistent by the X-ray diffractogram that crystal data is simulated
It is higher.
5th, the preparation of electrode slice：
Complex is used to prepare lithium ion cell electrode as lithium ion battery negative material the present invention also provides a kind of
The method of piece.It comprises the concrete steps that, takes the purple powder crystal collected in step 4 60 degrees Celsius of dryings 5 hours in vacuum drying oven.
According to 7:2:1 mass ratio weighs complex 56mg, Ketjen black 16mg and Kynoar 8mg respectively, adds in N- methylpyrroles
The uniform pulp of ground and mixed, is coated on copper foil after alkanone, and the drying 12 hours of 60 degrees Celsius of vacuum is cut into 12 millimeters of diameter
Circular electric pole piece.
6th, lithium ion battery assembles:
The present invention also provides a kind of lithium ion batteries assembled using complex as lithium ion battery negative material.With
Lithium piece is used as to electrode, and 2400 films of Celgard are diaphragm, and 1mol/L hexafluoros close lithium phosphate (LiPF6) ethylene carbonate
(EC)/diethyl carbonate (DEC) (volume ratio 1:1) solution is electrolyte, using the electrode slice obtained in above-mentioned step 5 as cathode
It is assembled into CR2032 lithium ion button shape cells.
7th, battery performance test：
Assembled lithium ion battery is tested on blue electric battery test system.Test temperature is room temperature, permanent electricity
It is 0.01-3V to flow the voltage range in charge-discharge test, and charge and discharge cycles number is 60 times in cycle performance test, current density
For 100mAg-1, it is 100,200,500,1000,2000,100mA g that high rate performance test has chosen current density respectively-1Under into
Row constant current charge-discharge is recycled 10 times under each multiplying power.
Referring to Fig. 5, be constant current charge-discharge figure when complex is as lithium ion battery negative material in the present invention, from
It can be seen from the figure that when the complex is as lithium ion battery negative material, has than relatively low charge and discharge platform, shows good
Good charge-discharge performance is 100mAg in current density-1When, discharge capacity is 2142mAhg for the first time-1, first week charging appearance
It measures as 711mAhg-1.By 60 charge and discharge cycles, specific capacity can be stablized in 865mAhg-1Left and right, coulombic efficiency compared with
Height shows good cyclical stability.Please refer to Fig. 6.Fig. 7 be complex as lithium ion battery negative material when multiplying power
Performance map.It is respectively respectively to recycle 10 weeks under 100,200,500,1000,2000mA/g in current density, capability value respectively may be about
893,758,597,503,431mAh/g.When current density returns to 100mA/g, the capacity of battery substantially may return to initially
Value illustrates that the complex has good cyclical stability and high rate performance under high current, as negative electrode of lithium ion battery
Great potentiality are shown in terms of material.
Referring to Fig. 8, be when complex is as lithium ion battery negative material in the present invention in high current 100mA/g
Charge and discharge cycles figure, it can be seen from the figure that when the complex is as lithium ion battery negative material, in high current 500mA
g-1When, it recycles 100 weeks, capacity is in 400mAhg-1Left and right, and keeps stable, embodies complex cyclical stability, possess compared with
Good application prospect.
Claims (4)
1. a kind of coordination polymer containing F, which is characterized in that chemical formula is [Co (tfbdc) (EtOH)2]n, in formula：N is for 1 to just
Infinite natural number, tfbdc2-For tetrafluoro terephthaldehyde's acid ion；The coordination polymer is by Co2+Ion and organic ligand
tfbdc2-Two-dimensional layered structure is formed by coordinate bond；The Co of a crystallography independence is included in minimum asymmetric cell2+, one
A tfbdc2-Ligand and the ethanol molecule of two coordinations；Adjacent Co2+Pass through tfbdc between ion2-Ligand bridging is flat into two dimension
Face structure.
2. a kind of synthetic method of the coordination polymer containing F as described in claim 1, it is characterised in that include the following steps：
1) cabaltous nitrate hexahydrate Co (NO are weighed3)2·6H2O and tetrafluoro terephthalic acid (TPA) (H2Tfbdc it) is dissolved in absolute ethyl alcohol,
Mixed liquor is obtained after stirring；
2) above-mentioned mixed liquor is placed in autoclave and is heated to 80-100 degrees Celsius, heat reaction 2-4 days, after reaction
Room temperature is down to, it is the coordination polymer containing F that purple powder bulk crystals, which are obtained by filtration,.
3. the synthetic method of the coordination polymer according to claim 2 containing F, it is characterised in that：Six in the mixed liquor
Nitric hydrate cobalt Co (NO3)2·6H2O and tetrafluoro terephthalic acid (TPA) (H2Tfbdc) molar ratio is (1-3):1；Cabaltous nitrate hexahydrate
Amount ratio with absolute ethyl alcohol is (0.05-0.2) mmol：(2-6)mL.
4. a kind of application of the coordination polymer containing F as negative material in lithium ion battery is prepared as described in claim 1,
It is characterized in that：The coordination polymer containing F is directly used as lithium ion battery negative material, specific method is：Coordination polymer
60 degrees Celsius of dryings 5 hours first in vacuum drying oven；Then according to 7:2:1 mass ratio weighs the coordination polymerization containing F respectively
Object, Ketjen black and Kynoar add in the uniform pulp of ground and mixed after N-Methyl pyrrolidone, are coated on copper foil, very
Empty 60 degrees Celsius of dryings 12 hours are cut into the circular electric pole piece of 12 millimeters of diameter；By the use of lithium piece as to electrode, Celgard
2400 films are diaphragm, and 1mol/L hexafluoros close lithium phosphate (LiPF6) ethylene carbonate (EC)/diethyl carbonate (DEC) solution be
The volume ratio of electrolyte, wherein ethylene carbonate (EC) and diethyl carbonate (DEC) is 1:1, using obtained electrode slice as cathode
It is assembled into CR2032 lithium ion button shape cells.
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| CN109369924A (en) * | 2018-09-21 | 2019-02-22 | 南开大学 | A kind of synthesis of tinbase coordination polymer and its application in lithium ion battery negative material |
| CN109873157A (en) * | 2019-01-26 | 2019-06-11 | 南京理工大学 | Co for lithium ion battery2(BDC)2Ted negative electrode material |
| CN114516964A (en) * | 2020-11-19 | 2022-05-20 | 国家纳米科学中心 | Octafluorobiphenyl-containing material as well as preparation method and application thereof |
| GB2617144A (en) * | 2022-03-30 | 2023-10-04 | Nicholas Huw Cartwright | Method and apparatus for synthesizing two-dimensional materials |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109369924A (en) * | 2018-09-21 | 2019-02-22 | 南开大学 | A kind of synthesis of tinbase coordination polymer and its application in lithium ion battery negative material |
| CN109873157A (en) * | 2019-01-26 | 2019-06-11 | 南京理工大学 | Co for lithium ion battery2(BDC)2Ted negative electrode material |
| CN114516964A (en) * | 2020-11-19 | 2022-05-20 | 国家纳米科学中心 | Octafluorobiphenyl-containing material as well as preparation method and application thereof |
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| GB2617144A (en) * | 2022-03-30 | 2023-10-04 | Nicholas Huw Cartwright | Method and apparatus for synthesizing two-dimensional materials |
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