CN109369924A - A kind of synthesis of tinbase coordination polymer and its application in lithium ion battery negative material - Google Patents
A kind of synthesis of tinbase coordination polymer and its application in lithium ion battery negative material Download PDFInfo
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- CN109369924A CN109369924A CN201811105136.3A CN201811105136A CN109369924A CN 109369924 A CN109369924 A CN 109369924A CN 201811105136 A CN201811105136 A CN 201811105136A CN 109369924 A CN109369924 A CN 109369924A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- H01M4/608—Polymers containing aromatic main chain polymers containing heterocyclic rings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a kind of synthesis of tinbase coordination polymer and its application in lithium ion battery negative material, the chemical formula of the coordination polymer is [Sn (HDPA)]nIn formula: n is 1 to just infinite natural number, and HDPA is 2,6 cinchomeronic acid of 4- hydroxyl.Preparation method is that stannous sulfate and 2,6 cinchomeronic acid of 4- hydroxyl are added in the aqueous solution of KOH, obtains target product through hydro-thermal reaction.The present invention has synthesized a kind of tinbase coordination polymer, and is directly applied to lithium ion battery negative material.The invention has the advantages that the tinbase coordination polymer synthetic method is simple, the raw material yield that is easy to get is high, at low cost.It is directly used in lithium cell cathode material, can effectively solve the problem of tin-based material is decayed in charge and discharge process because of cycle performance caused by volume expansion, and show good chemical property.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparation technical fields, and in particular to a kind of novel tinbase polycomplexation
Close the synthesis of object, anode plate for lithium ionic cell and lithium ion battery.
Background technique
Lithium ion battery is a kind of accumulator for being shifted between battery plus-negative plate with lithium ion and battery being made to complete charge and discharge
Outstanding advantages of part, it is small in size with light weight, easy to carry, is now widely used for every field.With New energy electric
The rapid development and popularization of automobile, tradition using graphite as the lithium ion battery of cathode because its lower capacity cannot meet reality again
Border application, this just has the negative electrode material of high specific energy and safety to design synthesis, and more stringent requirements are proposed.
Tin-based composites are because of its theoretical specific capacity (stannous oxide (SnO), tin oxide (SnO with higher2) and tin list
The theoretical capacity of matter (Sn) is respectively 875mAh g-1, 782mAh g-1With 990mAh g-1), lower charging/discharging voltage platform,
It is the research hotspot currently as lithium ion battery negative material.But such material in charge and discharge process since alloying is deposited
It will lead to the decline of material circulation performance in caused huge volume expansion, and then influence whole chemical property.At present
People synthesize a series of materials also by the design of various approach and are used to optimize solution existing issue, and there are mainly two types of methods: (1) will
Tin-based material nanosizing, such as synthesis nano wire, nanometer rods, nanosphere etc.；(2) by tin-based material and other materials such as carbon or
Some inert materials not reacted with lithium etc. are compound.However, these solutions theoretically cannot all completely eliminate by
In the existing volume expansion of charge and discharge, moreover, the preparation process of these materials is usually all more complicated, cost is also relatively
It is high.Therefore, design and development is a kind of cheap, and the tin base cathode material with good circulation stability is still urgently to solve at present
Certainly the problem of.
Coordination polymer is a kind of organic-inorganic hybrid material formed with metal node and organic ligand bridging, because
Synthetic method is simple, at low cost and attract attention convenient for operation, and is widely used in magnetism, fluorescence, the fields such as catalysis.At present
The existing report that coordination polymer is much directly applied to battery electrode material, the combination of metal node and organic ligand is not only
More storage lithium sites can be provided, material is more likely solved the problems, such as in terms of volume expansion, to show good storage
Lithium performance.However, gone back metallic tin as the report that node constructs coordination polymer at present seldom, tinbase coordination polymer is straight
It scoops out and also rarely has report for battery material.
Summary of the invention
The first purpose of this invention is analyzed for the above technology, is provided a kind of using divalent metal tin as the coordination of node
The preparation method of polymer, the coordination polymer yield by this method preparation is high, and raw material is cheap and easy to get, can solve current tinbase
The cost and yield issues of material expensive.
A second object of the present invention is to provide a kind of negative electrode of lithium ion battery electrode slices using above-mentioned material.The coordination
Polymer has capacity high as lithium ion battery negative material, the advantages of having extended cycle life, and can effectively solve tin-based material
The problem of volume expansion.
Third object of the present invention is to provide a kind of lithium ion batteries of negative electrode material electrode slice using above-mentioned preparation.
Technical solution of the present invention:
It is a kind of using Bivalent Tin as the coordination polymer of metal node, chemical formula be [Sn (HDPA)]n, in formula: n is 1 to just
Infinite natural number, HDPA are 2,6 cinchomeronic acid of 4- hydroxyl；The coordination polymer is by Sn2+Ion passes through with organic ligand HDPA
Coordinate bond forms one-dimensional catenary structure；It include an independent Sn of crystal in minimum asymmetric cell2+, a HDPA ligand；Phase
Adjacent Sn2+By ligand bridging at one-dimensional chain between ion, one-dimensional chain forms hydrogen bond with carboxyl oxygen by the hydrogen on HDPA ligand,
And then connect into a tridimensional network.
It is a kind of using Bivalent Tin as the preparation method of the coordination polymer of metal node, steps are as follows:
Stannous sulfate (SnSO is weighed according to the ratio that molar ratio is 1:14) and 2,6 cinchomeronic acid of 4- hydroxyl (HDPA) be placed in
In reaction kettle, then the aqueous solution of KOH is added into reaction kettle, the amount ratio of stannous sulfate and KOH aqueous solution is (0.05-0.15)
Mmol:(5-15 the concentration of) mL, KOH aqueous solution is 0.5-1mol L-1.Above-mentioned be uniformly mixed is obtained into mixed liquor, sealing is placed in
Heating reaction 72-96 hours, are down to room temperature after reaction in 150-160 degrees Celsius of baking oven, filter, and use 50mL distilled water respectively
Washing 3 times obtains colourless acicular crystal, as coordination polymer of the Bivalent Tin for metal node, the yield based on Sn
It is 77~85%.
A kind of preparation of the electrode slice applied to negative electrode of lithium ion battery
The coordination polymer crystal that above-mentioned preparation method is synthesized is dry in 60-80 degrees Celsius of vacuum drying oven, dries
It is 6-8- hours dry.Then coordination polymer, conductive agent (ketjen black), binder are weighed with the mass ratio of 6:3:1
(PVDF), ground and mixed is uniform, is tuned into pulpous state with solvent (NMP), is coated on copper foil, 80-100 degrees Celsius of vacuum dry 12-14
Hour, slice obtains circular electric pole piece.
A kind of preparation of fastening lithium ionic cell
It is used as using lithium piece to electrode, 2400 film of Celgard is diaphragm, 1mol L-1Hexafluoro close lithium phosphate (LiPF6)
For electrolyte, volume ratio ethylene carbonate (EC): diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, with above-mentioned preparation
Circular electric pole piece be negative pole assembling lithium ion button shape cell, battery size CR2032.
The advantages of the present invention:
1. a kind of novel tinbase coordination polymer is prepared；
2. the coordination polymer directly applies to lithium ion battery negative material, tin-based material charge and discharge can be effectively controlled
Volume expansion in electric process, to reach good cyclical stability；
3. the preparation method is simple, easily it is mass produced.
Detailed description of the invention
Fig. 1 is [Sn (HDPA)]nThe structural unit figure of crystal；
Fig. 2 is [Sn (HDPA)]nCrystal one-dimensional catenary structure figure；
Fig. 3 is [Sn (HDPA)]nThe interchain of crystal is connected by hydrogen bond, forms three-dimensional accumulation graph；
Fig. 4 is [Sn (HDPA)]nThe X-ray powder diffraction spectrogram of crystal；
Fig. 5 is [Sn (HDPA)]nThe lithium ion battery of cathode is prepared in 200mA g-1Lithium under the conditions of constant current charge-discharge from
The constant current charge-discharge figure of sub- battery；
Fig. 6 is [Sn (HDPA)]nThe lithium ion battery of cathode is prepared in 200mA g-1Lithium under the conditions of constant current charge-discharge from
The charge and discharge cycles figure of sub- battery；
Fig. 7 is [Sn (HDPA)]nThe lithium ion battery of cathode is prepared in 500mA g-1Lithium under the conditions of constant current charge-discharge from
The charge and discharge cycles figure of sub- battery；
Fig. 8 is [Sn (HDPA)]nPrepare the high rate performance figure of the lithium ion battery of cathode.
Specific embodiment
It is of the invention to reach the technological means and its technical effect that predetermined goal of the invention is taken further to illustrate, with
Under in conjunction with the embodiments and attached drawing, to proposed by the present invention a kind of using complex as the preparation of the lithium ion battery negative material of template
The specific embodiment of method is illustrated, and detailed description are as follows:
It is one, a kind of using two tin as the coordination polymer of metal node,
Chemical formula is [Sn (HDPA)]n, in formula: n is 1 to arrive just infinite natural number, and HDPA is 2,6 pyridine two of 4- hydroxyl
Acid；The coordination polymer is by Sn2+Ion forms one-dimensional catenary structure by coordinate bond with organic ligand HDPA；It is minimum asymmetric single
It include an independent Sn of crystal in member2+, a HDPA ligand；Adjacent Sn2+By ligand bridging at one-dimensional between ion
Chain, one-dimensional chain connect into a tridimensional network by the hydrogen and carboxyl oxygen formation hydrogen bond on HDPA ligand.
Two, the present invention in tinbase coordination polymer preparation
Embodiment 1:
(1) stannous sulfate (SnSO of 0.05mmol is weighed4) and 0.05mmol 2,6 cinchomeronic acid (HDPA) of 4- hydroxyl
It is placed in reaction kettle, in the 0.5mol L that 5mL is added thereto-1KOH aqueous solution, mixed above-mentioned
Liquid.
(2) sealing of above-mentioned mixed liquor is placed in heating reaction 96 hours in 150 degrees Celsius of baking ovens, is down to room after reaction
Temperature, filtering are distilled water washing 3 times with 50mL respectively, obtain colourless acicular crystal, and the yield based on Sn is 77%.
Embodiment 2:
(1) stannous sulfate (SnSO of 0.1mmol is weighed4) and 2,6 cinchomeronic acid (HDPA) of 4- hydroxyl of 0.1mmol set
In reaction kettle, in the 0.75mol L that 10mL is added thereto-1KOH aqueous solution, mixed above-mentioned
Liquid.
(2) sealing of above-mentioned mixed liquor is placed in heating reaction 96 hours in 150 degrees Celsius of baking ovens, is down to room after reaction
Temperature, filtering are distilled water washing 3 times with 50mL respectively, obtain colourless acicular crystal, and the yield based on Sn is 80%.
Embodiment 3:
(1) stannous sulfate (SnSO of 0.15mmol is weighed4) and 0.15mmol 2,6 cinchomeronic acid (HDPA) of 4- hydroxyl
It is placed in reaction kettle, in the 1.0mol L that 15mL is added thereto-1KOH aqueous solution, mixed above-mentioned
Liquid.
(2) sealing of above-mentioned mixed liquor is placed in heating reaction 72 hours in 160 degrees Celsius of baking ovens, is down to room after reaction
Temperature, filtering are distilled water washing 3 times with 50mL respectively, obtain colourless acicular crystal, and the yield based on Sn is 85%.
Three, the present invention in coordination polymer structure determination
Crystal structure is measured by Supernova type X-ray single crystal diffractometer, using by graphite monochromator monochromatization
Mo-K alpha rayFor Incident Irradiation Source, point diffraction is collected with ω-φ scanning mode, is repaired by least square method
The position of just their coordinate and its anisotropic parameters, hydrogen atom is obtained by theory plus hydrogen, and all calculating uses SHELXL-
97 and SHELXL-97 program bag carries out.The result shows that: the structural formula of the coordination polymer is [Sn (HDPA)]n.Belong to orthorhombic
System, space group Pna21, cell parameter isα=β=γ=
90 °, unit cell volume is Z=4, Dc=2.581mg/mm3.The coordination polymer is by Sn2+Ion is matched with organic
Body forms one-dimensional catenary structure by coordinate bond, and wherein organic ligand is 2,6 pyridinedicarboxylic acid of 4- hydroxyl；Minimum asymmetric cell
In include an independent Sn of crystallography2+, a HDPA.Adjacent Sn2+By ligand bridging at one-dimensional chain knot between ion
Structure.One-dimensional chain connects into a tridimensional network by the hydrogen and carboxyl oxygen formation hydrogen bond on HDPA ligand.Structure chart
It is to utilize Diamond Software on Drawing.Fig. 1 is the coordination context diagram of the central metal Sn of coordination polymer in the present invention；Fig. 2 is to match
The one-dimensional catenary structure figure of position polymer；Fig. 3 is the accumulation graph that coordination polymer is formed in three-dimensional space by hydrogen bond.
Four, the purity of coordination polymer characterizes in the present invention
The coordination polymer collected according to preparation method in specific implementation step two.Referring to Fig. 4, for preparing matches
Position polymer powder diffraction spectrum with by crystal data simulate come X-ray map be consistent, show synthesize match
Position polymer purity is very high.
Five, lithium ion battery negative material electrode slice is prepared using above-mentioned coordination polymer
Obtained crystal will largely be collected and dry 60 degrees Celsius in a vacuum drying oven, dried 8 hours.Then with 6:3:1
Mass ratio weigh coordination polymer, conductive agent (ketjen black), binder (PVDF) ground and mixed is uniform, uses solvent
(NMP) it is tuned into pulpous state, is coated on copper foil, 80 degrees Celsius of vacuum drying 12 hours, slice obtains round pole piece.
Six, lithium ion battery is assembled using the negative electrode material electrode slice of above-mentioned preparation
It is used as using lithium piece to electrode, 2400 film of Celgard is diaphragm, 1mol L-1Hexafluoro close lithium phosphate (LiPF6)
For electrolyte, volume ratio ethylene carbonate (EC): diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, is with round pole piece
Cathode assembles lithium ion button shape cell, battery size CR2032.
Seven, performance of lithium ion battery is tested
Referring to Fig. 5, it is the constant current charge-discharge of the lithium ion battery prepared by lithium cell cathode material of the invention
Figure, it can be seen from the figure that the coordination polymer when as lithium ion battery negative material, shows good charge and discharge electrical property
Can, it is 200mA g in current density-1When, discharge capacity is 2065mAh g for the first time-1, first week charging capacity is 1021mAh g-1。
Referring to Fig. 6, being 200mA g in current density-1When, by 180 charge and discharge cycles, specific capacity can be stablized in 732mAh
g-1Left and right, coulombic efficiency is higher, shows good chemical property.And in 500mA g-1When, it recycles 500 weeks, capacity exists
560mAh g-1Left and right, and keep stablizing and embody the good cycle performance of material, please refer to Fig. 7.
Referring to Fig. 8, it is the high rate performance figure of the lithium ion battery of lithium cell cathode material preparation of the invention.From figure
In as can be seen that current density be 100mA g-1, 200mA g-1, 500mA g-1, 1000mA g-1, 2000mA g-1Lower progress
Constant current charge-discharge, and cycle-index is 10 times under each multiplying power.Under different current densities, capability value distinguishes average out to
890,760,942,590,423,305mAh g-1, when current density returns to 100mA g-1When, capacity is still up to 914mAh g-1,
Show the good high rate performance of material.
Claims (4)
1. a kind of tinbase coordination polymer, it is characterised in that chemical formula is [Sn (HDPA)]n, in formula: n is 1 to arrive just infinite nature
Number, HDPA are 2,6 cinchomeronic acid of 4- hydroxyl；The coordination polymer is by Sn2+Ion is formed with organic ligand HDPA by coordinate bond
One-dimensional catenary structure；It include an independent Sn of crystal in minimum asymmetric cell2+, a HDPA ligand；Adjacent Sn2+From
By ligand bridging at one-dimensional chain between son, one-dimensional chain is connected by the hydrogen and carboxyl oxygen formation hydrogen bond on HDPA ligand
At a tridimensional network.
2. a kind of preparation method of tinbase coordination polymer described in claim 1, characterized by comprising: be according to molar ratio
The ratio of 1:1 weighs stannous sulfate (SnSO4) and 2,6 cinchomeronic acid (HDPA) of 4- hydroxyl be placed in reaction kettle, then to reaction kettle
The amount ratio of the middle aqueous solution that KOH is added, stannous sulfate and KOH aqueous solution is (0.05-0.15) mmol:(5-15) mL, KOH water
The concentration of solution is 0.5-1mol L-1；Above-mentioned be uniformly mixed is obtained into mixed liquor, sealing is placed in 150-160 degrees Celsius of baking oven
Heating reaction 72-96 hours, is down to room temperature after reaction, filters, and is distilled water washing 3 times with 50mL respectively, obtains colourless needle
The coordination polymer that shape crystal, the as Bivalent Tin are metal node, the yield based on Sn are 77~81%.
3. a kind of application of tinbase coordination polymer described in claim 1 in lithium ion battery negative material, feature exist
In: the tinbase coordination polymer is directly used as lithium ion battery negative material and assembles lithium ion battery, specific method is:
Coordination polymer is dry first in 60-80 degrees Celsius of vacuum drying oven, dries 6-8- hours；Then according to the mass ratio of 6:3:1
Coordination polymer is weighed, conductive agent (ketjenblack), binder (PVDF), ground and mixed is uniform, with Solvents N-methyl pyrroles
Alkanone is tuned into pulpous state, is coated on copper foil, and 80-100 degrees Celsius of vacuum 12-14 hours dry, and slice obtains circular electric pole piece.
4. application according to claim 3, which is characterized in that the assembling lithium ion battery is, using lithium piece conduct pair
Electrode, 2400 film of Celgard are diaphragm, and the hexafluoro of 1mol/L closes lithium phosphate (LiPF6) it is electrolyte, volume ratio ethylene carbonate
Ester (EC): diethyl carbonate (DEC)=1:1 is the electrolyte of solvent, is negative pole group with circular electric pole piece prepared by claim 3
Fill lithium ion button shape cell, battery size CR2032.
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Application publication date: 20190222 |