CN104916829A - Nitrogen-doped porous nanometer carbon-tin composite lithium ion battery negative electrode material and preparation method thereof - Google Patents
Nitrogen-doped porous nanometer carbon-tin composite lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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- CN104916829A CN104916829A CN201510184373.3A CN201510184373A CN104916829A CN 104916829 A CN104916829 A CN 104916829A CN 201510184373 A CN201510184373 A CN 201510184373A CN 104916829 A CN104916829 A CN 104916829A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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- 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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The invention relates to a nitrogen-doped porous nanometer carbon-tin composite lithium ion battery negative electrode material and a preparation method thereof, and belongs to the technical filed of lithium ion battery electrode materials. The specific capacity, the rate performance and the cycle performances of carbon-tin composite lithium ion batteries in the prior art are further improved in the invention. The method comprises the following steps: reacting an ethanol and water mixed solution of K2SnO3 under high temperature conditions, centrifuging the obtained product, and drying to obtain SnO2 white powder; adding the SnO2 white powder into water to form a suspension, adding a surfactant, a polymerization monomer and an initiator into the suspension, and carrying out a polymerization reaction under violent stirring conditions to obtain a black SnO2/polymer composite material; and mixing the black SnO2/polymer composite material with potassium hydroxide, reacting in oxygen-free atmosphere under high temperature conditions, and reacting the obtained reaction product with hydrochloric acid to obtain the nitrogen-doped porous nanometer carbon-tin composite lithium ion battery negative electrode material. The negative electrode material is characterized in that carbon is coated on the surface of a nanometer tin particle to form a carbon layer, and nitrogen is distributed in the carbon layer; and nanometer apertures are distributed in the carbon layer.
Description
Technical field
The present invention relates to a kind of nitrating porous nano carbon tin composite lithium ion battery cathode material and preparation method thereof, this composite lithium ion battery cathode material has the feature that specific capacity is large, good cycle, high rate performance are high simultaneously, belongs to technical field of lithium ion battery electrode.
Background technology
Volume is little, lightweight owing to having for lithium ion battery, energy density is large, good cycling stability, self discharge are little, memory-less effect, the outstanding advantage such as safe and reliable, pollution-free, capacity becomes power lithium-ion battery at the lithium ion battery of more than 3Ah, becomes the important a member in power source.
Existing commercial Li-ion battery negative material is graphite material, and the carbon good conductive effect in the electrodes of this material use, make electrode have higher high rate performance, but its Theoretical Mass specific capacity only has 375mAh g
-1, so low specific discharge capacity cannot meet with lithium ion battery the designing requirement of the various devices being the energy.In the prior art, developed in addition but not yet business-like non-carbon lithium ion battery negative material, as micron order, nanoscale tin particles., although tin has up to 992mAh g
-1theoretical Mass specific capacity, but, tin there will be in charge and discharge process expansion rate up to 300% violent volumetric expansion, cause negative plates tin particles coating shedding, nanoscale tin particles tin material being made uniform granularity also only make it have alleviate occur because of expansion efflorescence, Fragmentation Phenomena ability, therefore, the cycle performance of this electrode material is still unsatisfactory.
Given this, prior art proposes a kind of carbon tin composite lithium ion battery cathode material, it is characterized in that, at nanoscale tin particles coated with carbon bed, its effect is under the prerequisite of specific discharge capacity relatively improving negative material, the existence of carbon coating layer can stop the reunion of active material tin, prevent the change in volume of tin negative pole material to a certain extent, and then improve the cycle performance of lithium ion battery, simultaneously, due to the satisfactory electrical conductivity of carbon, improve electric conductivity and the chemical property of this carbon tin composite lithium ion battery cathode material, and then improve high rate performance and the cycle performance of lithium ion battery.But these effects of the program are very limited.So specific capacity of negative electrode material of lithium ion battery, high rate performance and cycle performance still await further raising.
Summary of the invention
In order to improve the specific capacity of carbon tin composite lithium ion cell, high rate performance and cycle performance further, we have invented a kind of nitrating porous nano carbon tin composite lithium ion battery cathode material and preparation method thereof.
The nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method of the present invention is characterized in that, (a) K
2snO
3ethanol and water mixed solution react under the high temperature conditions, after product is centrifugal, drying, obtain SnO
2white powder, from the described SnO of microcosmic
2white powder is SnO
2nano particle; B () is by SnO
2white powder is added to the water formation suspension-turbid liquid, surfactant softex kw or cetyl benzenesulfonic acid sodium, polymerization single polymerization monomer pyrroles or aniline, initiator ammonium persulfate is added in described suspension-turbid liquid, polymerization reaction take place under intense agitation, obtains black SnO
2/ polymer composites, from the described black SnO of microcosmic
2/ polymer composites is by the SnO of polymer overmold
2nano particle; C () is by described SnO
2/ polymer composites mixes with potassium hydroxide, reacts under non-oxygen atmosphere and under hot conditions, will obtain end product nitrating porous nano carbon tin composite lithium ion battery cathode material after product and hydrochloric acid reaction.
The nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention, at nanoscale tin particles coated with carbon, forms carbon-coating, it is characterized in that, in described carbon-coating, be scattered with nitrogen; Nano grade pore is distributed with in described carbon-coating.
Details are as follows for its technique effect of the present invention.
In (a) step, nanoscale SnO is obtained in the nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method of the present invention
2particle.Obtain by the SnO of polymer overmold in (b) step
2nano particle, described polymer will become nitrogen, carbon donor.In (c) step, at high temperature described polymer separates out carbon, nitrogen, forms nitrating carbon-coating, and one of effect of described carbon-coating prevents SnO under high temperature
2the reunion of nano particle, keeps high dispersion; Non-oxygen atmosphere avoids the oxidation of nitrogen, if non-oxygen atmosphere is formed by nitrogen, can also mix more nitrogen in carbon-coating; A part of carbon generation priming reaction in potassium hydroxide and carbon-coating forms nanometer porous carbon-coating, and hydrochloric acid is removed described activation reaction product potash, potassium oxide, simple substance potassium and neutralized excessive potassium hydroxide; A part of carbon in addition in carbon-coating is by SnO
2be reduced to simple substance tin, make the further porous of carbon-coating simultaneously; Form the kamash alloy of another carbon tin complex form at carbon, tin contact layer, make carbon-coating and nanoscale tin particles strong bonded.So far end product black nitrating porous nano carbon tin composite lithium ion battery cathode material is obtained.
Furtherly, the formation of nanometer porous structure can embed more lithium ion, further increases the specific capacity of nano-sized carbon tin composite lithium ion battery cathode material; Its effect of mixing of nitrogen shows in the following areas:
1, after nitrating, nitrogen replaces carbon, and enter in carbon lattice structure, carbon-coating can be made to produce a large amount of defects and avtive spot, these defects and avtive spot can catch lithium ion, thus improves the embedded quantity of lithium ion, and therefore the specific capacity of negative pole is improved;
2, nitrogen element can also change the Cloud Distribution in carbon-coating around carbon atom, makes the carbon-coating of nitrating possess more excellent electric conductivity and more stable chemical property compared to the carbon-coating of non-nitrating, and then improves high rate performance and the cycle performance of negative pole.
Choosing of negative material is depended in the raising of specific capacity, as prior art and the present invention choose tin, and the form of negative material, as the nanoscale tin particles in prior art and the present invention; Also has the special process of carbon-coating, as nitrating of the present invention forms defect and avtive spot; Also have the present invention to introduce nanometer porous structure and improve specific capacity further.
The raising of the conductivity of negative pole is depended in the raising of high rate performance; As prior art and the present invention choose the good carbon of conduction, and by carbon-coating clad nano level tin particles, nitrating of the present invention improves the conductivity of carbon-coating further.
The form of negative material is depended in the raising of cycle performance, and as the nanoscale tin particles in prior art and the present invention, and coated carbon-coating stops nanometer tin particle agglomeration, alleviates efflorescence, Fragmentation Phenomena; And chemical property, as carbon-coating nitrating of the present invention improves chemical property; Also have the present invention to introduce loose structure and stop expansion further, improve cycle performance.
Its technique effect of the present invention can be verified by lower testing result.
As shown in Figure 1, schemed from the SEM of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention, this negative material is Nanoparticulate.
As shown in Figure 2, the existence of known nitrogen is schemed by a width XPS of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention.
As shown in Figure 3, the existence of known carbon is schemed by another width XPS of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention.
As shown in Figure 4, the existence of known tin is schemed by the another width XPS of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention.
As shown in Figure 5, the XRD figure of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention further illustrates the existence of crystalline state tin.
As shown in Figure 6, under the current density of 0.1A/g, initial charge specific capacity, specific discharge capacity maximum are respectively 994.4mAh/g, 2311.6mAh/g, shown in curve as up in solid line in figure, descending curve; 200th time charge specific capacity, specific discharge capacity maximum still can reach 745mAh/g, 780mAh/g respectively, shown in curve as up in dotted line in figure, descending curve, this measured result illustrates that the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention is under the prerequisite with very high specific capacity, has good cycle performance simultaneously.
As shown in Figure 7, under the current density of 0.1A/g, circulation 250 circle still keeps the specific discharge capacity of more than 677mAh/g, and remain coulombic efficiency CE (the coulombic efficiency of more than 95%, refer to the ratio of discharge capacity of the cell and charging capacity in same cyclic process), illustrate that the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention has good cycle performance again.
As shown in Figure 8, experienced by the circulation of 60 circles, still can discharge under the current density of 5A/g (Current Density) and keep the specific capacity of 180mAh/g, not only show excellent high rate performance, also good cycle performance is shown, as seen from the figure, when discharging with the current density of 0.1A/g more afterwards, specific capacity still can return to initial value.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention.Fig. 2 ~ Fig. 4 is that three width XPS of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention scheme; Fig. 2 is simultaneously as Figure of abstract.Fig. 5 is the XRD figure of the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention.Fig. 6 be adopt the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention to make lithium ion battery negative first and the 200th charging, electric discharge specific discharge capacity change curve.Fig. 7 is the lithium ion battery negative specific discharge capacity, the coulombic efficiency change curve in successively charge and discharge cycles that adopt the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention to make.Fig. 8 is the lithium ion battery negative current density and the specific discharge capacity graph of relation in successively charge and discharge cycles that adopt the nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention to make.
Embodiment
Its embodiment of nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method of the present invention is as follows.
(a) K
2snO
3ethanol and water mixed solution under the high temperature conditions in reaction kettle for reaction, product is centrifugal, washing, after drying, obtain SnO
2white powder, from the described SnO of microcosmic
2white powder is SnO
2nano particle.At K
2snO
3ethanol and water mixed solution in, K
2snO
3concentration be 0.02 ~ 0.03mol/L, the volume ratio of ethanol and water is (2 ~ 4): (4 ~ 6).Described high temperature is 190 ~ 210 DEG C, and the reaction time is 11 ~ 13 hours.
B () is by SnO
2white powder is added to the water forms suspension-turbid liquid after ultrasonic disperse, surfactant softex kw or cetyl benzenesulfonic acid sodium, polymerization single polymerization monomer pyrroles or aniline, initiator ammonium persulfate is added in described suspension-turbid liquid, polymerization reaction take place under intense agitation, obtains black SnO
2/ polymer composites, from the described black SnO of microcosmic
2/ polymer composites is by the SnO of polymer overmold
2nano particle.Described polymeric reaction temperature is 0 ~ 5 DEG C, and polymerization reaction time is 22 ~ 26 hours.
C () is by described SnO
2/ polymer composites mixes with potassium hydroxide, reacts under non-oxygen atmosphere and under hot conditions, will obtain end product nitrating porous nano carbon tin composite lithium ion battery cathode material after product and hydrochloric acid reaction.The concentration of described potassium hydroxide solution is 7mol/L.SnO
2the hybrid mode of/polymer composites and potassium hydroxide is by SnO
2/ polymer composites joins in potassium hydroxide solution, then to containing SnO
2the potassium hydroxide solution of/polymer composites mixes, filter, dry process, obtains SnO
2the solid mixt that/polymer composites and potassium hydroxide highly mix each other.Described non-oxygen atmosphere is formed by nitrogen, or is formed by inert gas, as argon gas.Described hot conditions is 800 ~ 820 DEG C, 2 ~ 2.5 hours time.Described product and hydrochloric acid reaction refer to be removed potash, potassium oxide, simple substance potassium with hydrochloric acid and neutralizes the reaction of excessive potassium hydroxide.
One embodiment of the present of invention are as described below.
(1) 0.1943g K is taken
2snO
33H
2o and 0.15g urea is dissolved in 9.375mL ethanol and 15.625mL deionized water mixed solution, and adding of urea is conducive to SnO
2the formation of nano particle, join after prepared solution is mixed in 50mL reactor, be then placed in baking oven and react 12 hours at 200 DEG C of temperature, after reaction terminates, product is centrifugal, washing, last in vacuum drying oven at 60 DEG C of temperature dry 12 hours, obtain SnO
2white powder.
(2) SnO described in 0.15g is taken
2white powder, ultrasonic disperse forms suspension-turbid liquid in the round-bottomed flask that 100mL deionized water is housed, 0.5g softex kw, 1.37g ammonium persulfate is added successively to described suspension-turbid liquid, then round-bottomed flask is placed in 0 DEG C of ice bath, stir and add 0.83mL pyrroles after 30 minutes, complete the preparation of polymerization reaction reactant liquor, after vigorous stirring reacts 24 hours, suction filtration is carried out to reacted solution, use deionized water cyclic washing, last in vacuum drying oven at 60 DEG C of temperature dry 6 hours, obtain black SnO
2/ polymer composites.
(3) 0.4g black SnO is taken
2/ polymer composites, being scattered in 20mL concentration is in the potassium hydroxide solution of 7mol/L, and stirring at room temperature is suction filtration after 24 hours, obtains black solid content, described black solid content is placed in vacuum drying oven at 70 DEG C of temperature dry 6 hours, obtains SnO
2the solid mixt that/polymer composites and potassium hydroxide highly mix each other, described solid mixt is put into tube furnace, be filled with nitrogen and form non-oxygen atmosphere, described tube furnace is warming up to 800 DEG C with the heating rate of 5 DEG C/min, be incubated 2 hours, described polymer carbonization during this period, a part of carbon occurs to react as follows with contiguous potassium hydroxide:
4KOH+C＝K
2CO
3+K
2O+2H
2
And:
6KOH+2C→2K
2CO
3+2K+3H
2
Some carbon reduction SnO
2maintain nitrogen protection; be cooled to room temperature, obtain calcined product, described collection calcined product is placed in 20mL deionized water; regulate the deionized water solution being dissolved with calcined product to neutral with 8% hydrochloric acid; remove potash, potassium oxide, simple substance potassium and neutralize excessive potassium hydroxide, suction filtration obtains solid content, uses deionized water cyclic washing; last in vacuum drying oven at 60 DEG C of temperature dry 6 hours, obtain black end product nitrating porous nano carbon tin composite lithium ion battery cathode material.
(4) described end product nitrating porous nano carbon tin composite lithium ion battery cathode material, Kynoar (PVDF) and conductive carbon black are mixed according to mass ratio 8:1:1, then add 1-METHYLPYRROLIDONE to size mixing, be coated in copper foil current collector, again using lithium sheet as to electrode, take concentration as the LiPF of 1mol/L
6eC/DEC mixed liquor be electrolyte, wherein the volume ratio of EC:DEC is 1:1, with Celgard2400 polypropylene film for barrier film, button cell assembling is completed in glove box, this half-cell charge and discharge cycles 250 under the current density of 0.1A/g encloses the specific capacity that still can keep more than 677mAh/g, as shown in Figure 6, Figure 7, and has excellent high rate performance and cycle performance, the specific capacity of 180mAh/g is still kept, as shown in Figure 8 under the current density of 5A/g.
The nitrating porous nano carbon tin composite lithium ion battery cathode material of the present invention, at nanoscale tin particles coated with carbon, forms carbon-coating.Nitrogen is scattered with in described carbon-coating; In described carbon-coating, be distributed with nano grade pore, described nano grade pore comprises micropore and mesoporous.
Claims (7)
1. a nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method, is characterized in that, (a) K
2snO
3ethanol and water mixed solution react under the high temperature conditions, after product is centrifugal, drying, obtain SnO
2white powder, from the described SnO of microcosmic
2white powder is SnO
2nano particle; B () is by SnO
2white powder is added to the water formation suspension-turbid liquid, surfactant softex kw or cetyl benzenesulfonic acid sodium, polymerization single polymerization monomer pyrroles or aniline, initiator ammonium persulfate is added in described suspension-turbid liquid, polymerization reaction take place under intense agitation, obtains black SnO
2/ polymer composites, from the described black SnO of microcosmic
2/ polymer composites is by the SnO of polymer overmold
2nano particle; C () is by described SnO
2/ polymer composites mixes with potassium hydroxide, reacts under non-oxygen atmosphere and under hot conditions, will obtain end product nitrating porous nano carbon tin composite lithium ion battery cathode material after product and hydrochloric acid reaction.
2. nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method according to claim 1, is characterized in that, at K
2snO
3ethanol and water mixed solution in, K
2snO
3concentration be 0.02 ~ 0.03mol/L, the volume ratio of ethanol and water is (2 ~ 4): (4 ~ 6); Described high temperature is 190 ~ 210 DEG C, and the reaction time is 11 ~ 13 hours.
3. nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method according to claim 1, it is characterized in that, described polymeric reaction temperature is 0 ~ 5 DEG C, and polymerization reaction time is 22 ~ 26 hours.
4. nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method according to claim 1, it is characterized in that, the concentration of described potassium hydroxide solution is 7mol/L; SnO
2the hybrid mode of/polymer composites and potassium hydroxide is by SnO
2/ polymer composites joins in potassium hydroxide solution, then to containing SnO
2the potassium hydroxide solution of/polymer composites mixes, filter, dry process, obtains SnO
2the solid mixt that/polymer composites and potassium hydroxide highly mix each other; Described non-oxygen atmosphere is formed by nitrogen, or is formed by inert gas; Described hot conditions is 800 ~ 820 DEG C, 2 ~ 2.5 hours time; Described product and hydrochloric acid reaction refer to be removed potash, potassium oxide, simple substance potassium with hydrochloric acid and neutralizes the reaction of excessive potassium hydroxide.
5. nitrating porous nano carbon tin composite lithium ion battery cathode material preparation method according to claim 1, is characterized in that, by described SnO
2when/polymer composites mixes with potassium hydroxide, also add urea.
6. a nitrating porous nano carbon tin composite lithium ion battery cathode material, at nanoscale tin particles coated with carbon, forms carbon-coating, it is characterized in that, in described carbon-coating, be scattered with nitrogen; Nano grade pore is distributed with in described carbon-coating.
7. nitrating porous nano carbon tin composite lithium ion battery cathode material according to claim 6, is characterized in that, described nano grade pore comprises micropore and mesoporous.
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