CN109742361A - A kind of preparation method and application of compound anode material of lithium-ion battery - Google Patents
A kind of preparation method and application of compound anode material of lithium-ion battery Download PDFInfo
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- CN109742361A CN109742361A CN201910016708.9A CN201910016708A CN109742361A CN 109742361 A CN109742361 A CN 109742361A CN 201910016708 A CN201910016708 A CN 201910016708A CN 109742361 A CN109742361 A CN 109742361A
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- selenide
- chlorella
- stannous
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- ion battery
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of preparation method and application of compound anode material of lithium-ion battery.It is matched according to material quality part, weighs 1-2 mass parts chlorella and 1 mass parts pink salt is add to deionized water, be centrifuged after magnetic agitation, dried in baking oven after sediment washing, obtain jade-green solid sample；Solid sample is ground to powder, then is mixed with 4-12 mass parts selenium powder, calcining in corundum boat is put into and obtains the derivative carbon complex of stannic selenide-stannous selenide-chlorella；Copper foil over-assemble will be coated in after stannic selenide-stannous selenide-chlorella composition and the super P carbon of conductive agent, binder CMC mixed grinding into button-type battery.After measured, when voltage is 0.01-3.0 V, high current density 1A/g after charge and discharge cycles 600 times, specific capacity is stablized in 300 mAh/g or more, and capacity retention ratio is up to 85.7%.Raw material sources are extensive, low in cost, can be mass-produced, and meet environmental requirement.
Description
Technical field
The invention belongs to sodium-ion battery Material Field more particularly to a kind of stannic selenides-with long cycle life characteristics
Stannous selenide-chlorella constitutes the preparation method and application of compound anode material of lithium-ion battery.
Background technique
In secondary energy sources storage system, lithium ion battery is received significant attention, and high speed development, we live in
Locate visible (portable electronic products, communication apparatus, electric car etc.).However consider the finiteness of metal lithium resource, a large amount of lithiums
Consumption made lithium resource increasingly deficient, only solely rely on lithium ion battery and be unable to satisfy the mankind to following need
It asks.And have the metallic sodium of the same clan of similar physics and chemical property with lithium, reserves more horn of plenty, and energy storage mechnism is similar, because
This sodium-ion battery is most to be expected to replace one of the battery of lithium ion battery applications in we live.
However because sodium ion has the atomic radius bigger than lithium ion, existing major part lithium ion battery is negative
The all unsuitable storage sodium of pole material, is primarily due to the problems such as interlamellar spacing is small, and dynamics is slow.Therefore finding has specific capacity
It is high, can stable/embedding sodium electrode material have great importance.And stannic selenide and stannous selenide have special stratiform knot
Structure has very high storage sodium theoretical capacity (780mAh g-1), there is preferable storage sodium characteristic.However, stannic selenide and stannous selenide
When storing up sodium, volume expansion is huge (expansion rate close to 300%), and electric conductivity is poor, and conventional method of modifying is complex carbon material
Improve its electric conductivity, and part inhibits its huge volume expansion.The invention patent is stored using stannic selenide and stannous selenide
Current potential difference when sodium allows them alternately to react with sodium ion, it is swollen to effectively inhibit volume of electrode material during storing up sodium
It is swollen.When stannous selenide is reacted with sodium ion, stannic selenide does not react with sodium ion；When stannic selenide is reacted with sodium ion,
Sodium ion is reacted stannous selenide, therefore realizes " from buffering effect " of system during storing up sodium, can effectively be subtracted
The problems such as slow volume expansion bring material dusting, structure collapses, to realize the long circulation life stability of composite material.
The present invention is by preparing selenizing as presoma carbon source, adsorbent and nano-reactor using biomass chlorella
The derivative carbon complex of tin-stannous selenide-chlorella.It is compared difference with conventional method and is: 1, chlorella is from eutrophy
Green alga in the water body of change, it is from a wealth of sources, and turn waste into wealth, sustainable development and Green Development are more met as carbon source
Strategy；2, chlorella is as algal biomass, is rich in various functional groups and protein in vivo, can be with adsorbing metal ions and in situ
Nitrogen P elements, the electric conductivity of its modified derived carbon are provided；3, chlorella is used as special nano-reactor in the method, can be with
Effectively stannic selenide-stannous selenide nanoparticle is prevented to reunite；4, stannic selenide-selenium is constructed by biomass absorbent and one-step calcination method
Change stannous material, method is simple, and process is short, has the prospect of large-scale production；5, sodium is stored using stannic selenide and stannous selenide
When current potential difference, allow them alternately react with sodium ion, construct stannic selenide-stannous selenide from buffer system, effectively inhibit electric
Volume expansion of pole material during storing up sodium；And the result shows that, which has excellent storage sodium
Can, there is application prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of, and stannic selenide-stannous selenide-chlorella with long cycle life characteristics spreads out
The preparation method and application of raw carbon complex anode material of lithium-ion battery, simple process, strong operability, raw material sources are wide
It is general, it is low in cost, it can be mass-produced, meet environmental requirement.
To achieve the above object, the present invention adopts the following technical scheme:
The present invention prepares the derivative carbon complex of stannic selenide-stannous selenide-chlorella using simple one-step calcination method.Its
Specific step is as follows:
1) material quality part matches
Pink salt 1
Chlorella 1-2
Selenium powder 4-12；
2) it prepares
It is matched according to material quality part, the chlorella and pink salt for weighing certain mass are add to deionized water, and magnetic force stirs
It mixes 12-24h and obtains mixture；
Gained sediment is dried in 60-80 DEG C of baking oven, obtained after deionized water washing by precipitating after mixture centrifugation
To jade-green solid sample；
Obtained jade-green solid sample is ground to powder, then is mixed with selenium powder, is put into corundum boat,
H2Calcining 4-5 hours is carried out for 400-700 DEG C in/Ar (5%/95%) atmosphere tube type furnace, obtains black solid sample, as selenizing
The derivative carbon complex of tin-stannous selenide-chlorella；
3) it applies
By the derivative carbon complex of stannic selenide-stannous selenide prepared by the present invention-chlorella according to 8:1:1 mass ratio with lead
After the super P carbon of electric agent, binder CMC mixed grinding uniformly after be coated on copper foil and be used as working electrode, metallic sodium piece is to electricity
Pole and reference electrode, the NaPF of 1mol/L6/ DIGLYME is that electrolyte is assembled into 2025 type button-type batteries.After measured, in electricity
When pressure is 0.01-3.0V, high current density 1A/g after charge and discharge cycles 600 times, specific capacity is stablized in 300mAh/g or more, capacity
Conservation rate is up to 85.7%.
Above-mentioned steps, the chlorella have abundant as the algal biomass in eutrophication water, cell wall
Functional group, the ability with stronger adsorbing metal salt, can be used as environmentally protective nano-reactor；Using chlorella as charcoal
Presoma, the derived carbon made of high-temperature calcination pyrolysis are agraphitic carbon, have N and P Heteroatom doping abundant.
The pink salt is stannous chloride, stannic chloride, stannous sulfate, STANNOUS SULPHATE CRYSTALLINE；
The derivative carbon complex of the stannic selenide-stannous selenide-chlorella has stannic selenide and stannous selenide two phase structure；
The chlorella derived carbon is agraphitic carbon, has N and P Heteroatom doping abundant.
Remarkable advantage of the invention is:
1) green alga of the chlorella used in the present invention in the water body of eutrophication, it is from a wealth of sources, and turn waste into wealth.
Chlorella functions as presoma carbon source, adsorbent and nano-reactor, and carbon is converted in calcination process and limits selenium
Change tin-stannous selenide nanoparticle to reunite, to obtain the derivative carbon complex of stannic selenide-stannous selenide-chlorella.
2) chlorella used in the present invention is dexterously used as nano-reactor, tin source can be adsorbed, so that stannic selenide-selenizing
The derivative carbon complex of stannous-chlorella has stannic selenide-stannous selenide two phase structure, and has special layer structure.It utilizes
Current potential difference when stannic selenide and stannous selenide storage sodium, allows them alternately to react with sodium ion, constructs stannic selenide-stannous selenide
From buffer system, effectively inhibit volume expansion of electrode material during storing up sodium.
3) the chlorella derived carbon used in the present invention functions as carrier, rises to the stannic selenide-stannous selenide
To the buffer function, the electric conductivity of increase material and the infiltration for being conducive to electrolyte of auxiliary.On the one hand, chlorella derived carbon and selenium
Change tin-stannous selenide buffer system to provide for stannic selenide-stannous selenide particle volume expansion and contraction during de-/embedding sodium
Certain free space.On the other hand, the chlorella derived carbon of rich N, P doping is conducive to the diffusion of electrolyte, helps
In raising electron conductivity, and few layer selenizing molybdenum structure can be effectively fixed, further increase its and store up sodium performance.
4) the derivative carbon complex of stannic selenide-stannous selenide of the invention-chlorella is that a kind of completely new sodium-ion battery is negative
Pole, the derivative carbon complex of stannic selenide-stannous selenide that the embodiment of the present invention 1 obtains-chlorella are applied to sodium-ion battery cathode
In, voltage be 0.01-3.0V, high current density 1A/g when charge and discharge cycles 600 times after, specific capacity stablize 300mAh/g with
On, capacity retention ratio is up to 85.7%.
5) the derivative carbon complex of stannic selenide-stannous selenide-chlorella is a kind of good anode material of lithium-ion battery, this
Invention provides a kind of method for preparing the derivative carbon complex of stannic selenide-stannous selenide-chlorella, preparation process letter for the first time
Single, equipment is easy to get, and strong operability, raw material sources are extensive, low in cost, can mass production, meet environmental requirement.
Detailed description of the invention
Fig. 1 is the XRD diagram of the derivative carbon complex of the resulting stannic selenide-stannous selenide of embodiment 1-chlorella.
Fig. 2 is the SEM figure of the derivative carbon complex of the resulting stannic selenide-stannous selenide of embodiment 1-chlorella.
Fig. 3 is that the derivative carbon complex of the resulting stannic selenide-stannous selenide of embodiment 1-chlorella is negative as sodium-ion battery
The charging and discharging curve figure when material of pole under 100mA/g current density.
Fig. 4 is that the derivative carbon complex of the resulting stannic selenide-stannous selenide of embodiment 1-chlorella is negative as sodium-ion battery
Long-life cycle performance figure when the material of pole under 1A/g current density.
Specific embodiment
Embodiment 1
1) 4g chlorella is weighed respectively and 2g stannous chloride is added in 0.4L deionized water, it, will after centrifugation after stirring 12h
Washing of precipitate is placed in 60 DEG C of baking oven and dries；
2) light green solid obtained by step 1) is ground to powder, is mixed with the selenium powder of 12g, in H2/ Ar (5%/95%)
It is calcined 4 hours for 400 DEG C in atmosphere tube type furnace, collects black solid sample, as stannic selenide-stannous selenide-chlorella derived carbon
Compound；
The derivative carbon complex of stannic selenide-stannous selenide of above-mentioned preparation-chlorella is subjected to XRD, obtains stannic selenide-selenizing
The XRD diagram of the derivative carbon complex of stannous-chlorella, as shown in Figure 1.From fig. 1, it can be seen that the material that synthesis obtains is stannic selenide-selenium
Change the mixed phase of stannous two-phase, diffraction maximum position and stannic selenide-stannous selenide standard diagram (JCPDS, 089-3197；
JCPDS, 048-1224) match.
The derivative carbon complex of stannic selenide-stannous selenide of above-mentioned preparation-chlorella is scanned by scanning electron microscope, obtains selenium
Change the SEM figure of the derivative carbon complex of tin-stannous selenide-chlorella, as shown in Figure 2.The compound is irregular as shown in Figure 2
Sphere, carbon derived from chlorella are chondritic, and surface is made of stannic selenide-stannous selenide of sheet；
Using the derivative carbon complex of stannic selenide-stannous selenide manufactured in the present embodiment-chlorella: the super P carbon of conductive agent: viscous
Agent CMC is tied according to electrode of working equably is coated on copper foil after mass percent 80:10:10 mixed grinding, metallic sodium piece is
To electrode and reference electrode, the NaPF of 1mol/L6/ DIGLYME is that electrolyte is assembled into button cell；All assemblings are in inertia
It is carried out in atmosphere glove box.Under 100mA/g and 1A/g current density, it is tested respectively and stores up sodium performance, result such as Fig. 3 institute
Show.Fig. 3 is charging and discharging curve of the material under 100mA/g current density, and as can be seen from Figure 3 the electrode material is for the first time
After electric discharge, charging and discharging curve repeatability is preferable, illustrates it with good cyclical stability.As shown in Figure 4, stannic selenide-selenium
When changing the derivative carbon complex of stannous-chlorella as anode material of lithium-ion battery, shows excellent long circulation life and stablize
Property, in the case where voltage is 0.01-3.0V, in high current density 1A/g, 600 specific capacities of charge and discharge cycles are stablized in 300mAh/g,
Capacity retention ratio is up to 85.7%.Therefore, the derivative carbon complex of stannic selenide-stannous selenide-chlorella has long circulation life special
Property, it is environmentally friendly high-performance anode material of lithium-ion battery, has a good application prospect.
Embodiment 2
1) 4g chlorella is weighed respectively and 4g stannic chloride is added in 0.5L deionized water, after stirring 12h, will be sunk after centrifugation
Washing of forming sediment, which is placed in 60 DEG C of baking oven, dries；
2) light green solid obtained by step 1) is ground to powder, is mixed with the selenium powder of 20g, in H2/ Ar (5%/95%)
It is calcined 4 hours for 700 DEG C in atmosphere tube type furnace, collects black solid sample, as stannic selenide-stannous selenide-chlorella derived carbon
Compound；
Using the derivative carbon complex of stannic selenide-stannous selenide manufactured in the present embodiment-chlorella: the super P carbon of conductive agent: viscous
Agent CMC is tied according to electrode of working equably is coated on copper foil after mass percent 80:10:10 mixed grinding, metallic sodium piece is
To electrode and reference electrode, the NaPF of 1mol/L6/ DIGLYME is that electrolyte is assembled into button cell；All assemblings are in inertia
It is carried out in atmosphere glove box.
Embodiment 3
1) 10g chlorella is weighed respectively and 5g stannous sulfate is added in 0.8L deionized water, after stirring for 24 hours, after centrifugation
Washing of precipitate is placed in 80 DEG C of baking oven and is dried；
2) light green solid obtained by step 1) is ground to powder, is mixed with the selenium powder of 60g, in H2/ Ar (5%/95%)
It is calcined 5 hours for 600 DEG C in atmosphere tube type furnace, collects black solid sample, as stannic selenide-stannous selenide-chlorella derived carbon
Compound；
Using the derivative carbon complex of stannic selenide-stannous selenide manufactured in the present embodiment-chlorella: the super P carbon of conductive agent: viscous
Agent CMC is tied according to electrode of working equably is coated on copper foil after mass percent 80:10:10 mixed grinding, metallic sodium piece is
To electrode and reference electrode, the NaPF of 1mol/L6/ DIGLYME is that electrolyte is assembled into button cell；All assemblings are in inertia
It is carried out in atmosphere glove box.
Embodiment 4
1) 5g chlorella is weighed respectively and 5g stannous chloride is added in 0.5L deionized water, it, will after centrifugation after stirring for 24 hours
Washing of precipitate is placed in 70 DEG C of baking oven and dries；
2) light green solid obtained by step 1) is ground to powder, is mixed with the selenium powder of 40g, in H2/ Ar (5%/95%)
It is calcined 4.5 hours for 500 DEG C in atmosphere tube type furnace, collects black solid sample, as stannic selenide-stannous selenide-chlorella is derivative
Carbon complex；
Using the derivative carbon complex of stannic selenide-stannous selenide manufactured in the present embodiment-chlorella: the super P carbon of conductive agent: viscous
Agent CMC is tied according to electrode of working equably is coated on copper foil after mass percent 80:10:10 mixed grinding, metallic sodium piece is
To electrode and reference electrode, the NaPF of 1mol/L6/ DIGLYME is that electrolyte is assembled into button cell；All assemblings are in inertia
It is carried out in atmosphere glove box.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (8)
1. a kind of preparation method of compound anode material of lithium-ion battery, includes the following steps:
1) material quality part matches
Pink salt 1
Chlorella 1-2
Selenium powder 4-12；
2) it prepares
It is matched according to material quality part, the chlorella and pink salt for weighing certain mass are add to deionized water, and magnetic agitation obtains
To mixture；
Gained sediment is dried in an oven, obtained jade-green solid after deionized water washing by precipitating after mixture centrifugation
Body sample；
Obtained jade-green solid sample is ground to powder, then is mixed with selenium powder, is put into corundum boat, 5%/
95% H2It is calcined in/Ar atmosphere tube type furnace, obtains black solid sample, as stannic selenide-stannous selenide-chlorella spreads out
Raw carbon complex.
2. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
The pink salt stated is stannous chloride, stannic chloride, stannous sulfate, STANNOUS SULPHATE CRYSTALLINE.
3. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
The derivative carbon complex of the stannic selenide-stannous selenide stated-chlorella has stannic selenide and stannous selenide two phase structure.
4. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
The magnetic agitation stated, mixing time 12-24h.
5. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
It is dried in the baking oven stated, drying temperature is at 60-80 DEG C.
6. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
The drying stated, drying temperature is at 60-80 DEG C.
7. a kind of preparation method of compound anode material of lithium-ion battery according to claim 1, it is characterised in that institute
The calcining stated, calcination temperature are calcined 4-5 hours at 400-700 DEG C.
8. a kind of application of compound anode material of lithium-ion battery, it is characterised in that stannic selenide-stannous selenide-chlorella spreads out
Raw carbon complex is coated in copper according to uniformly rear after the mass ratio and the super P carbon of conductive agent, binder CMC mixed grinding of 8:1:1
Working electrode is used as on foil, metallic sodium piece is to electrode and reference electrode, the NaPF of 1mol/L6/ DIGLYME is electrolyte assembling
At button-type battery.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111924873A (en) * | 2020-07-31 | 2020-11-13 | 广东凯金新能源科技股份有限公司 | Novel sodium-ion battery negative electrode material and preparation method thereof |
| CN113036102A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Molybdenum selenide composite carbonized common sowthistle herb flower crown hair electrode material for sodium ion battery |
| CN113823784A (en) * | 2021-08-25 | 2021-12-21 | 福建师范大学 | Preparation method and application of tin selenide-selenium-doped polyacrylonitrile compound sodium ion battery cathode material with long cycle life |
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| CN113823784A (en) * | 2021-08-25 | 2021-12-21 | 福建师范大学 | Preparation method and application of tin selenide-selenium-doped polyacrylonitrile compound sodium ion battery cathode material with long cycle life |
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