CN108550840A - Three-dimensional netted carbon embeds antimony-containing alloy kalium ion battery negative material and preparation method - Google Patents
Three-dimensional netted carbon embeds antimony-containing alloy kalium ion battery negative material and preparation method Download PDFInfo
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- CN108550840A CN108550840A CN201810465819.3A CN201810465819A CN108550840A CN 108550840 A CN108550840 A CN 108550840A CN 201810465819 A CN201810465819 A CN 201810465819A CN 108550840 A CN108550840 A CN 108550840A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
Three-dimensional netted carbon embeds antimony-containing alloy kalium ion battery negative material, including the thin carbon layer of tridimensional network and antimony-containing alloy particle, the antimony-containing alloy particle are uniformly embedded among thin carbon layer；The preparation method of the material is：1) NaCl, the ionic compound of formation antimony-containing alloy and carbon source is soluble in water, mixed solution is made in 3 12h of stirring；2) mixed solution freezing, drying are removed into moisture removal to keep the cubic structure of NaCl；3) above-mentioned object is put into crucible, be heat-treated under a reducing atmosphere, carbon source and carbon is made to turn to carbon simple substance, metal ion is reduced into metal simple-substance, and metal simple-substance is assembled to form alloy；4) it is washed with deionized and removes NaCl, then dry to obtain product, the material capacity is high, good cycle, high rate performance is excellent, has stable charge and discharge platform, solve that cubical expansivity existing for metallic antimony negative material is big, cycle and the bad problem of high rate performance.
Description
Technical field
The invention belongs to kalium ion battery negative material technical fields, and in particular to a kind of embedded antimony base conjunction of three-dimensional netted carbon
Golden kalium ion battery negative material and preparation method.
Background technology
With the fast development of new energy, electric vehicle and intelligent grid so that limited lithium resource (0.0017wt.%)
The problem of being difficult to meet demand is increasingly prominent.Therefore, developing low-cost, high safety, the long-life, can fast charging and discharging newcooperative medical system
It is imperative to learn power supply system.Recent studies suggest that kalium ion battery has many advantages outstanding.With height ratio capacity, height
The positive and negative pole material of voltage difference and good embedding potassium/de- potassium stability is the necessary item for realizing high specific energy, long-life kalium ion battery
Part.The main problem that kalium ion battery is faced is to find suitable electrode material.
It is mainly carbon material to study more negative material at present, but its theoretical capacity (KC8, 279mAh/g) and low, it is only logical
It is difficult to greatly improve to cross modified or optimization preparation process, cannot be satisfied the requirement of extensive energy-storage battery.Therefore, novel height is researched and developed
Specific capacity non-carbon negative material becomes research emphasis and hot spot, and it is anti-that with potassium alloying can occur for many metals and semiconductor
It answers.Such as phosphorus base, tinbase, antimony base, transition metal oxide.As novel anode material, wherein it is prominent that antimony sill stores up potassium capacity
Go out, theoretical embedding potassium capacity is 660mAh/g, moreover, there is Sb the layer structure of fold, the space availability ratio of atom packing to reach
39%, contribute to K+In the migration of interlayer；Sb has higher conductivity (2.5 × 10 simultaneously-4S/cm), the biography of electronics can be promoted
Defeated and transfer, these properties are conducive to its alloying reaction.The deintercalation potassium process of antimony also has flat electrochemical reaction flat
Platform can provide highly stable operating voltage.As potential negative material, metallic antimony becomes the heat of concern and research increasingly
Point.But there are serious problems for simple substance antimony, and cubical expansivity is big during charge and discharge cycles, and easy dusting causes active antimony base material
Material falls off from collector, causes capacity attenuation fast.It is exactly that metallic antimony is active/nonactive with other that one kind, which being efficiently modified method,
Metal combines and forms alloy, such as SnSb, Cu2Sb、CoSb3、Zn4Sb3And NiSb2Deng cycle performance can then significantly improve, main
Reason is wanted to be that the active component of different embedding potassium current potentials or inert component can react the volume change of phase by buffering to inhibit electricity
Pole expands, and increases the ductility of material, to reach raising electrode cycle life；Another method be it is compound with carbon, in addition to
Increase other than electric conductivity, cushioning effect can also be played to alloy volume change；Another relatively conventional method is nanometer
Change, reduces crystallite dimension.
Invention content
The object of the present invention is to provide a kind of three-dimensional netted carbon to embed antimony-containing alloy kalium ion battery negative material and preparation
Method, obtained composite negative pole material capacity is high, and good cycle, high rate performance is excellent, has stable charge and discharge platform, solution
Cubical expansivity existing for metallic antimony negative material of having determined is big, cycle and the bad problem of high rate performance.
The technical solution that the present invention takes is：
Three-dimensional netted carbon embeds antimony-containing alloy kalium ion battery negative material, includes the thin carbon layer and antimony of tridimensional network
Based alloy particle, the antimony-containing alloy particle are uniformly embedded among thin carbon layer.
Further, the antimony-containing alloy particle size is 5nm~100nm, is selected from binary antimony-based compounds Fe-Sb, Ta-
One of Sb, Bi-Sb, Sn-Sb, Ni-Sb, Cu-Sb, Co-Sb, Mg-Sb, Mn-Sb, Zn-Sb, Zr-Sb, Ti-Sb, V-Sb or ternary
One of antimony-based compounds Cu-Sn-Sb, Fe-Ni-Sb.
Further, the thickness of the thin carbon layer is 1~3nm.
Three-dimensional netted carbon embeds the preparation method of antimony-containing alloy kalium ion battery negative material, includes the following steps：
(1) it will be dissolved in deionized water as the NaCl of template, the ionic compound of formation antimony-containing alloy and carbon source, magnetic
Mixed solution is made in power stirring 3-12h, wherein the molar ratio of antimony ion and carbon source contained in ionic compound is 1:10~1:
500, the molar ratio with NaCl is 1:100~1:500；
(2) mixed solution made from step (1) is freezed, is placed into freeze drier after freezing reality completely ,-
Vacuum drying removes moisture removal to keep the cubic structure of NaCl, before then collecting dried object as under the conditions of 70 DEG C to -10 DEG C
Drive body；
(3) presoma made from step (2) is put into crucible, is placed under reducibility gas atmosphere in tube furnace at heat
Reason, makes carbon source and carbon turn to carbon simple substance, metal ion is reduced into metal simple-substance, and metal simple-substance is assembled to form alloy, in the process
In, inert gas 30-60min is passed through with the flow of 50-500ml/min first into tube furnace, to exclude air, according still further to hydrogen
Gas and inert gas 250:100~100:200 flow-rate ratio is passed through hydrogen and inert gas, and with 5 DEG C/min~10 DEG C/min
Rate be warming up to 550 DEG C~750 DEG C, keep the temperature cooled to room temperature after 2h~5h；
(4) product of step (3) is taken out from tube furnace, is washed, filtered repeatedly with deionized water, until thoroughly removes
NaCl；The mixture of washes clean is dried under conditions of 60~80 DEG C in baking oven again and is embedded to get to three-dimensional netted carbon
Antimony-containing alloy material.
Further, the carbon source is one or more of citric acid, sucrose, Victoria C, glucose, starch.
Further, the inert gas is one or more of nitrogen, argon gas or helium.
Beneficial effects of the present invention：
The present invention combines method of three kinds of improvement simple substance antimonies as negative material described in background technology, the cathode of preparation
Material has the following advantages：(1) there is larger specific surface area and a large amount of active site；(2) there is continuous network,
It can ensure that materials conductive contact is good, the diffusion path of potassium ion can be shortened；(3) since alloying pellet surface is wrapped in thin layer
Carbon, can slow down agglomeration traits, and the space of pore structure can also be used to alleviate the volume that material occurs in cycle charge-discharge swollen
Swollen problem.
Using template, preparation process is easy to operate, safety and low production cost, and antimony-containing alloy is with nano-scale particle
Form be uniformly embedded in carbon-coating, around there is carbon-coating package to increase the stability of alloy structure, so, pass through antimony-containing alloy
High carbon material is compound with chemical stability, it is made to have both high power capacity and high conductivity, and cycle and high rate performance are excellent.
Description of the drawings
Fig. 1 is that the three-dimensional netted carbon of 1 gained of embodiment embeds the SEM figures of Cu-Sb materials；
Fig. 2 is that the three-dimensional netted carbon of 1 gained of embodiment embeds the XRD spectrum of Cu-Sb materials；
Fig. 3 is that the three-dimensional netted carbon of 1 gained of embodiment embeds the charge-discharge performance figure of Cu-Sb materials；
Fig. 4 is that the three-dimensional netted carbon of 2 gained of embodiment embeds the SEM figures of Co-Sb materials；
Fig. 5 is that the three-dimensional netted carbon of 2 gained of embodiment embeds the XRD spectrum of Co-Sb materials；
Fig. 6 is that the three-dimensional netted carbon of 2 gained of embodiment embeds the charge-discharge performance figure of Co-Sb materials；
Fig. 7 is that the three-dimensional netted carbon of 3 gained of embodiment embeds the SEM figures of Bi-Sb materials；
Fig. 8 is that the three-dimensional netted carbon of 3 gained of embodiment embeds the XRD spectrum of Bi-Sb materials；
Fig. 9 is that the three-dimensional netted carbon of 3 gained of embodiment embeds the charge-discharge performance figure of Bi-Sb materials.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Embodiment 1
1) C of 2.5g is weighed6H8O7·H2Cu (the NO of the NaCl of O, 20.7g, 0.2156g3)2·3H2O, 0.2035g's
SbCl3, it is dissolved in 75mL water, magnetic agitation 12h.
2) solution after stirring evenly moves into surface plate, covers preservative film, is put into refrigerator and freezes, will after for 24 hours
The material that build-ups ice takes out, and is put into freeze drier, is freeze-dried at -50 DEG C to being completely dried.
3) powder after drying is taken out, puts into crucible, is heat-treated in tube furnace.It is passed through argon with 200ml/min
For gas 30min to exclude air, then using hydrogen as carrier gas, hydrogen is 250 with argon flow amount ratio：100, with the heating speed of 6 DEG C/min
Rate keeps the temperature 3h, cooled to room temperature to 680 DEG C, and the whole process to room temperature since heating is passed through gas always.
4) powder after taking-up washed repeatedly with deionized water, filtered, until NaCl is completely removed.By the powder of washes clean
Body is put into baking oven dries at 80 DEG C, and tridimensional network can be obtained by, which being ground after drying, embeds Cu2The carbon composite of Sb, it is interior
Embedding Cu2Sb diameters are 30nm or so, and the length of side of each mesh is about 600nm.
Freeze-drying makes NaCl other than keeping its cubic structure, and the surfaces NaCl are uniform with metal ion solution by citric acid
Package, in high-temperature heat treatment process, citric acid carbonization forms alloy quilt at the thin layer carbon for being wrapped in the surfaces NaCl, metal ion
Be wrapped in carbon-coating, be washed with deionized water NaCl masterplates later, target product retain NaCl hole and its around it is equably thin
The alloying pellet of layer carbon and carbon-coating package.
Nanoscale Cu as can be seen from Figure 12Sb is dispersed in three-dimensional carbon structure, hole shape rule, close circle, and carbon
Net is connected with each other, and integrality is good；Carbon-coating surface has no metallic particles, and metallic particles is all embedded in inside carbon-coating, and particle ruler
Very little very little, within the scope of 10-20nm；Fig. 2 is XRD spectrum, and comparison finds that the diffracting spectrum of sample almost coincide with standard diagram,
It can prove that the material of synthesis is Cu2Sb。
Embodiment 2
1) C of 2.5g is weighed6H8O7·H2The SbCl of the NaCl of O, 20.7g, 0.2035g3, the Co (NO of 0.2610g3)2·
2H2O is dissolved in 75mL water, magnetic agitation 12h.
2) solution after stirring evenly moves into surface plate, covers preservative film, is put into refrigerator and freezes, will after for 24 hours
Freeze real material to take out, be put into freeze drier, is freeze-dried at -50 DEG C to being completely dried.
3) powder after drying is taken out, puts into crucible, is heat-treated in tube furnace.It is passed through argon with 200ml/min
For gas 30min to exclude air, then using hydrogen as carrier gas, hydrogen is 250 with argon flow amount ratio：100, with the heating speed of 8 DEG C/min
Rate keeps the temperature 3h, cooled to room temperature to 720 DEG C.
4) powder after taking-up washed repeatedly with deionized water, filtered, until NaCl is completely removed.By the powder of washes clean
Body is put into baking oven dries at 80 DEG C, and the compound potassium ion electricity of carbon that tridimensional network embeds CoSb can be obtained by being ground after drying
Pond negative material, embedded CoSb diameters are 30nm or so, and the length of side of each mesh is about 600nm.Due to outside NaCl
It is wrapped in the carbon source (C in the present embodiment6H8O7·H2O), carbon source and carbon turns to thin layer carbon after heat treatment, is washed with deionized water
Three-dimensional pore structure is left after NaCl masterplates just becomes the carbon network layer of ultra-thin interconnection.
Fig. 4 schemes for SEM, it can be seen that the carbon net of hole shape rule and wherein embedded nanoscale Co-Sb small metal particles,
Fig. 5 is XRD spectrum, and comparison finds that the diffracting spectrum of sample fits like a glove with standard diagram, based on the material that can prove synthesis
It is CoSb to want ingredient.
Embodiment 3
1) C of 2.5g is weighed6H8O7·H2Bi (the NO of the NaCl of O, 20.7g, 0.4328g3)2·5H2O, 0.2035g's
SbCl3, it is dissolved in 75mL water, magnetic agitation 12h.
2) solution after stirring evenly moves into surface plate, covers preservative film, is put into refrigerator and freezes, will after for 24 hours
The material that build-ups ice takes out, and is put into freeze drier, is freeze-dried at -50 DEG C to being completely dried.Sodium chloride is that the center of area is vertical
Square structure, in freezing dry process, sodium chloride is further assembled into three-dimensional structure, the template as carbon net.
3) powder after drying is taken out, puts into crucible, is heat-treated in tube furnace.It is passed through argon with 200ml/min
For gas 30min to exclude air, then using hydrogen as carrier gas, hydrogen is 250 with argon flow amount ratio：100, with the heating speed of 5 DEG C/min
Rate keeps the temperature 2h, cooled to room temperature to 690 DEG C.
4) powder after taking-up washed repeatedly with deionized water, filtered, until NaCl is completely removed.By the powder of washes clean
Body is put into baking oven dries at 80 DEG C, after drying grinding can obtain tridimensional network embed BiSb the compound potassium ion of carbon it is negative
Pole material, embedded NiSb3Diameter is 30nm or so, and the length of side of each mesh is about 600nm.
Fig. 7 schemes for SEM, it can be seen that fine metal particles are equably embedded in inside carbon net, and the size of metallic particles
It is Nano grade, within the scope of 10-20nm；Fig. 8 is XRD spectrum, and comparison finds that the diffracting spectrum of sample and standard diagram are complete
It coincide, can prove that the material of synthesis be main component is BiSb.
Material prepared by Example 1, by it with carbon black, poly- inclined fluorine vinyl chloride (PVDF) according to weight ratio 8:1:1 mixing
Uniformly, it is coated on copper foil, is to electrode by working electrode, metallic potassium piece of the mixing material, glass fibre is diaphragm, 1mol
L-1KPF6(EC:DEC=1:1) it is that electrolyte is assembled into kalium ion battery, tests its chemical property.
As shown in figure 3, being 100mAg in current density-1Under, for cycle after 100 weeks, charging and discharging capacity is respectively 248mAh/
G, 290mAh/g, with the increase of cycle-index, then capacity, which continuously decreases, to be kept stablizing.
Equally, material prepared by embodiment 2 and embodiment 3 is same as above way respectively, the performance measured such as Fig. 6 and Fig. 9 institutes
Show, as can be seen from Figure 6, CoSb alloy material of cathode is after 10 weeks, charge specific capacity held stationary, and 50 weeks charge specific capacities are
237mAh/g, 80 weeks charge specific capacities are 241.5mAh/g, have good cyclical stability；As can be seen from Figure 9, BiSb alloys
Negative material is after cycle 100 weeks, and efficiency can be maintained at 99.58%, and charging and discharging capacity is respectively 274.2mAh/g,
275.3mAh/g。
The above results show：Synthesized three-dimensional netted embedded antimony-containing alloy material be used as kalium ion battery cathode due to
Its unique structure and there is good cycle performance, nanoscale alloy is equably mounted among firm carbon net, this is solely
Special structure can not only play the role of buffer volumes expansion, and can effectively prevent the alloying pellet in charge and discharge process
Aggregation and crushing, these features make material have excellent cycle performance.
Claims (6)
1. three-dimensional netted carbon embeds antimony-containing alloy kalium ion battery negative material, which is characterized in that including tridimensional network
Thin carbon layer and antimony-containing alloy particle, the antimony-containing alloy particle are uniformly embedded among thin carbon layer.
2. three-dimensional netted carbon as described in claim 1 embeds antimony-containing alloy kalium ion battery negative material, which is characterized in that institute
It is 5nm~100nm to state antimony-containing alloy particle size, is selected from binary antimony-based compounds Fe-Sb, Ta-Sb, Bi-Sb, Sn-Sb, Ni-
One of Sb, Cu-Sb, Co-Sb, Mg-Sb, Mn-Sb, Zn-Sb, Zr-Sb, Ti-Sb, V-Sb or ternary antimony-based compounds Cu-Sn-
One of Sb, Fe-Ni-Sb.
3. three-dimensional netted carbon as described in claim 1 embeds antimony-containing alloy kalium ion battery negative material, which is characterized in that institute
The thickness for stating thin carbon layer is 1~3nm.
4. three-dimensional netted carbon as described in claim 1 embeds the preparation method of antimony-containing alloy kalium ion battery negative material,
It is characterized in that, includes the following steps：
(1) it will be dissolved in deionized water as the NaCl of template, the ionic compound of formation antimony-containing alloy and carbon source, magnetic force stirs
It mixes 3-12h and mixed solution is made, wherein the molar ratio of antimony ion and carbon source contained in ionic compound is 1:10~1:500,
Molar ratio with NaCl is 1:100~1:500；
(2) mixed solution made from step (1) is freezed, is placed into freeze drier after freezing reality completely, at -70 DEG C
Vacuum drying removes moisture removal to keep the cubic structure of NaCl under the conditions of to -10 DEG C, and it is presoma then to collect dried object；
(3) presoma made from step (2) is put into crucible, is placed in tube furnace and is heat-treated under reducibility gas atmosphere, makes
Carbon source and carbon turns to carbon simple substance, and metal ion is reduced into metal simple-substance, and metal simple-substance is assembled to form alloy, in this process, first
First into tube furnace inert gas 30-60min is passed through with the flow of 50-500ml/min, to exclude air, according still further to hydrogen with
Inert gas 250:100~100:200 flow-rate ratio is passed through hydrogen and inert gas, and with the speed of 5 DEG C/min~10 DEG C/min
Rate is warming up to 550 DEG C~750 DEG C, keeps the temperature cooled to room temperature after 2h~5h；
(4) product of step (3) is taken out from tube furnace, is washed, filtered repeatedly with deionized water, until thoroughly removes
NaCl；The mixture of washes clean is dried under conditions of 60~80 DEG C in baking oven again and is embedded to get to three-dimensional netted carbon
Antimony-containing alloy material.
5. three-dimensional netted carbon as claimed in claim 4 embeds the preparation method of antimony-containing alloy kalium ion battery negative material,
It is characterized in that, the carbon source is one or more of citric acid, sucrose, Victoria C, glucose, starch.
6. three-dimensional netted carbon as claimed in claim 4 embeds the preparation method of antimony-containing alloy kalium ion battery negative material,
It is characterized in that, the inert gas is one or more of nitrogen, argon gas or helium.
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Application publication date: 20180918 |