CN109909511A - A kind of preparation method and application of bismuthino hollow nano-material - Google Patents
A kind of preparation method and application of bismuthino hollow nano-material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and application of bismuthino hollow nano-material, preparation method obtains the first solution the following steps are included: copper nano material is dissolved in solvent, by BiI3It is dissolved in solvent and obtains the second solution, first solution is mixed with second solution, obtain bismuthino hollow nano-material after reacting a period of time, the solvent is dimethyl sulfoxide or N, N- dimethyl propylene alkenyl urea.The bismuthino hollow nano-material being prepared using this method can be used as negative electrode material and apply in sodium-ion battery or lithium ion battery, with good high rate performance, the cyclical stability of overlength and higher specific capacity.
Description
Technical field
The present invention relates to sodium-ion battery technical fields, and in particular to a kind of preparation method of bismuthino hollow nano-material and
Using.
Background technique
Sodium-ion battery receives the extensive concern of academia and industry in extensive energy storage field in recent years.It is cell performance
Anode, cathode, electrolyte and the compatibility between them can be strongly depend on.Wherein negative electrode material is sodium-ion battery development
Key factor.Therefore it develops extremely urgent for the high-performance negative electrode material of chargeable sodium-ion battery.Bismuth metal is very
One of potential anode material of lithium-ion battery, but after storing up sodium serious volume expansion can occur for bismuth, cause material powder
Change, seriously affects the stability of battery.
Summary of the invention
In order to overcome the above technical defects, it the present invention provides a kind of preparation method of bismuthino hollow nano-material and answers
With, the bismuthino hollow nano-material being prepared using this method can be used as negative electrode material apply sodium-ion battery or lithium from
Sub- battery, with good high rate performance, the cyclical stability of overlength and higher specific capacity.
In order to reach above-mentioned technical effect, the present invention provides a kind of preparation methods of bismuthino hollow nano-material, including
Following steps: copper nano material being dissolved in solvent and obtains the first solution, by BiI3It is dissolved in solvent and obtains the second solution, by institute
It states the first solution to mix with second solution, obtains bismuthino hollow nano-material after reacting a period of time, the solvent is two
Methyl sulfoxide or N, N- dimethyl propylene alkenyl urea.
Further technical solution is that the shape of the copper nano material is copper nano particles, copper nano-wire, copper nanometer
Any one in pipe, copper nanocone or copper nano cubic block.
Further technical solution is that the diameter of the copper nano particles is 2-500nm, and the width of the copper nano-wire is 2-
500nm, a length of 1-1000 μm；The diameter of copper nanotube is 10-100nm, long are as follows: 1-1000 μm；The size bottom of copper nanocone
Diameter is 50-150nm, tip diameter are as follows: 10-45nm, length are 1-10 μm；Copper nano cubic block diameter is 10-200nm.
Further technical solution is that the concentration of first solution is 0.01-500mg/mL.
Further technical solution is that the configuration method of second solution is by BiI3It is dissolved in dimethyl sulfoxide or N, N-
In dimethyl propylene alkenyl urea, the tetrabutyl ammonium tetrafluoroborate of 0-1mol/L is then added, obtains the second solution, second solution
Concentration be 0.001-5mol/L.
Further technical solution is that the molar ratio of copper and bismuth is 1:0.5-5 in the hollow nano-material.
Further technical solution is that the reaction time of first solution and the second solution is greater than five minutes.
The present invention also provides a kind of applications of bismuthino hollow nano-material, and bismuthino hollow nano-material is used for sodium ion
The negative electrode material of battery or lithium ion battery.
Compared with prior art, the invention has the following beneficial effects: the present invention mixes the first solution and the second solution
Displacement reaction occurs afterwards, simultaneously because copper species are faster than the inside diffusion velocity of bismuth to the speed of external diffusion to form tubulose knot
Structure, that is, so-called Kirkendall effect.Prepared hollow nano-material, can effectively padded coaming volume
Expansion, to improve the performance of battery, using bismuthino hollow nano-material as negative electrode material apply sodium-ion battery or lithium from
In sub- battery, when such material is used as the negative electrode material of sodium ion or lithium ion battery, there is good high rate performance, overlength
Cyclical stability and higher specific capacity.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram of bismuth nanotube；
Fig. 2 is the transmission electron microscope picture of bismuth nanotube；
The high rate performance schematic diagram of Fig. 3 bismuth nanotube cathode sodium-ion battery；
The cyclical stability schematic diagram of Fig. 4 bismuth nanotube cathode sodium-ion battery.
Specific embodiment
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
The copper nano particles that partial size is 2nm are configured to dimethyl sulfoxide (DMSO) solution (the first solution) of 10mg/mL.
Then the 0.01mol/L BiI of the ammonium tetrafluoroborate of the tetrabutyl containing 0.01mol/L (TBABF4) is prepared3DMSO solution, copper/bismuth mole
Than for 1:1.5 (the second solution).It is stirred after first solution and the second solution are mixed on magnetic stirring apparatus, mixing speed is
It 100 revs/min, reacts 0.5 hour.By product ethanol washing, centrifugation, hollow bismuth nanometer is obtained by vacuum drying
Grain.By hollow Nano particle, carbon black and sodium carboxymethylcellulose (CMC) according to mass ratio: 7:2:1 is configured to slurry and is coated in copper foil
On, it is assembled into half-cell with sodium sheet metal, diaphragm is glass fibre, and electrolyte is 1M NaPF6Diethylene glycol dimethyl ether
(diglyme) solution has investigated the chemical property of battery, in 100mA g-1Under current density, capacity is 375mA h g-1。
Embodiment 2
The copper nano particles that partial size is 100nm are configured to the N of 20mg/mL, N- dimethyl propylene alkenyl urea (DMPU) solution
(the first solution).Then 0.01mol/L BiI is prepared3DMPU solution (the second solution).First solution and the second solution are mixed,
Copper/bismuth molar ratio is 1:2, is reacted 72 hours.By product ethanol washing, centrifugation, hollow bismuth is obtained by vacuum drying and is received
Rice grain.Hollow bismuth nano particle, carbon black and CMC are configured to slurry according to mass ratio 8:1:1 to be coated on copper foil, and golden with sodium
Belong to thin slice and be assembled into half-cell, diaphragm is glass fibre, and electrolyte is 1M NaPF6Diglyme solution, test battery
Chemical property, in 200mA g-1Under current density, capacity is 321mA h g-1。
Embodiment 3
The copper nano particles that partial size is 300nm are configured to the DMSO (the first solution) of 10mg/mL.Then it prepares
BiI3DMSO solution (the second solution) mixes the first solution, the second solution, and copper/bismuth molar ratio is 1:3, reacts 0.5 hour.
By product ethanol washing, centrifugation, hollow bismuth nano particle is obtained by vacuum drying.By hollow bismuth nano particle, carbon black
With CMC according to mass ratio: 8:1:1 is configured to slurry and is coated on copper foil, is assembled into half-cell with sodium sheet metal, diaphragm is glass
Fiber, electrolyte are 1M NaPF6Diglyme solution, the chemical property of battery is tested, in 1000mA g-1Current density
Under, capacity is 287mA h g-1。
Embodiment 4
The copper nano particles that diameter is 500nm are configured to the DMSO (the first solution) of 20mg/mL.Then it prepares and contains
The 0.01mol/L BiI of 0.1mol/L tetrabutyl ammonium tetrafluoroborate (TBABF4)3DMSO (the second solution).By the first solution,
Two solution stir after mixing on magnetic stirring apparatus, and mixing speed is 300 revs/min, and bell metal/bismuth molar ratio is 1:2, and reaction 1 is small
When.By product ethanol washing, centrifugation, hollow bismuth nano particle is obtained by vacuum drying.By hollow bismuth nano particle, charcoal
Black and CMC is according to mass ratio: 8:1:1 is configured to slurry and is coated on copper foil, is assembled into Symmetrical cells with sodium sheet metal, diaphragm is
Glass fibre, electrolyte are 1M NaPF6Dimethyl ether (DME) solution, the chemical property of battery is tested, in 1000mA g-1
Under current density, capacity is 295mA h g-1。
Embodiment 5
The copper nano-wire that diameter is 45nm is configured to dimethyl sulfoxide (DMSO) solution (the first solution) of 5mg/mL.So
The 0.1mol/L BiI of the ammonium tetrafluoroborate of the tetrabutyl containing 0.1mol/L (TBABF4) is prepared afterwards3DMSO solution (the second solution).It will
First solution, the second solution stir after mixing on magnetic stirring apparatus, and copper/bismuth molar ratio is 1:2, and mixing speed is 300 revs/min
Clock reacts 2 hours.By product ethanol washing, centrifugation, bismuth nanotube, crystal structure such as Fig. 1 institute are obtained by vacuum drying
Show, is pure bismuth, has no the diffraction maximum of other substances, pattern is illustrated in figure 2 tubulose, and diameter is about 50nm.By bismuth nanotube, charcoal
Black and CMC is configured to slurry according to mass ratio 7:2:1 and is coated on copper foil, is assembled into half-cell with sodium sheet metal, diaphragm is glass
Glass fiber, electrolyte are 1M NaPF6DME solution, test the chemical property of battery.Fig. 3 is electricity under different current densities
The high rate performance in pond: in 100mA g-1、200mA g-1、600mA g-1、1000mA g-1、2000mA g-1、6000mA g-1And
10000mA g-1Specific capacity under current density is respectively 350mA h g-1、328mA h g-1、309mA h g-1、285mA h
g-1、244mA h g-1、160mA h g-1With 95mA h g-1, as can be seen from the figure when current density returns to 100mA g-1, can
Inverse capacity restores again to the capacity 350mAh g under initial current density-1, it was demonstrated that battery has good high rate performance.Fig. 4 is
The cyclical stability test chart of battery, in 1A g-1High current density it is lower 1500 times circulation after, the capacity of battery still maintains
198mAh g-1, it was demonstrated that battery has the cyclical stability of overlength.
Embodiment 6
The copper nano-wire that diameter is 100nm is configured to the DMSO (the first solution) of 15mg/mL.Then it prepares and contains
The 0.2mol/L BiI of 0.5mol/L tetrabutyl ammonium tetrafluoroborate (TBABF4)3DMSO (the second solution).By the first solution,
Two solution stir after mixing on magnetic stirring apparatus, and copper/bismuth molar ratio is 1:2, and mixing speed is 600 revs/min, and reaction 72 is small
When.By product ethanol washing, centrifugation, bismuth nanotube is obtained by vacuum drying.By bismuth nanotube, carbon black and CMC according to
Mass ratio: 7:1.5:1.5 is configured to slurry and is coated on copper foil, is assembled into half-cell with sodium sheet metal, and diaphragm is glass fibre,
Electrolyte is 1M NaPF6Diglyme solution, the chemical property of battery is tested, in 200mA g-1Under current density, hold
Amount is 330mA h g-1。
Embodiment 7
The copper nano cubic block that diameter is 100nm is configured to 10mg/mL DMSO solution (the first solution).Then it prepares
The 0.01mol/L BiI of the ammonium tetrafluoroborate of the tetrabutyl containing 0.1mol/L (TBABF4)3DMSO solution (the second solution).It is molten by first
Liquid, the second solution stir after mixing on magnetic stirring apparatus, and mixing speed is 450 revs/min, and copper/bismuth molar ratio is 1:2.5,
Reaction 2 hours.By product ethanol washing, centrifugation, hollow bismuth nano cubic block is obtained by vacuum drying.Hollow bismuth is received
Cubic block, carbon black and CMC are according to mass ratio: 7:2:1 is configured to slurry and is coated on copper foil, is assembled into symmetrical electricity with sodium sheet metal
Pond, diaphragm are glass fibre, and electrolyte is 1M NaPF6Diglyme solution, test the chemical property of battery,
1000mA g-1Under current density, capacity is 275mA h g-1。
Embodiment 8
The copper nano particles that diameter is 50nm are configured to the DMSO solution (the first solution) of 5mg/mL.Then it prepares and contains
The 0.01mol/L BiI of 0.1mol/L tetrabutyl ammonium tetrafluoroborate (TBABF4)3DMSO solution (the second solution).It is molten by first
Liquid, the second solution stir after mixing on magnetic stirring apparatus, and mixing speed is 300 revs/min, and copper/bismuth molar ratio is 1:2, instead
It answers 24 hours.By product ethanol washing, centrifugation, hollow bismuth nano particle is obtained by vacuum drying.By hollow bismuth nanometer
Grain, carbon black and CMC are according to mass ratio: 7:2:1 is configured to slurry and is coated on copper foil, is assembled into Symmetrical cells with lithium metal thin slice,
Diaphragm is glass fibre, and electrolyte is 1M LiPF6EC/DMC/EMC (volume ratio 1:1:1) solution, test the electrification of battery
Performance is learned, in 1000mA g-1Under current density, capacity is 282mA h g-1。
Embodiment 9
The copper nano-wire that diameter is 50nm is configured to the DMPU (the first solution) of 10mg/mL.Then it prepares and contains 0.1mol/
The 0.01mol/L BiI of L tetrabutyl ammonium tetrafluoroborate (TBABF4)3DMPU (the second solution).First solution, the second solution are existed
It is stirred after being mixed on magnetic stirring apparatus, mixing speed is 500 revs/min, and copper/bismuth molar ratio is 1:2, is reacted 50 hours.It will produce
Object ethanol washing, centrifugation obtain bismuth nanotube by vacuum drying.By bismuth nanotube, carbon black and CMC according to mass ratio: 8:
1:1 is configured to slurry and is coated on copper foil, is assembled into Symmetrical cells with lithium metal thin slice, diaphragm is glass fibre, electrolyte 1M
LiPF6EC/DMC/EMC (volume ratio 1:1:1) solution, the chemical property of battery is tested, in 100mA g-1Current density
Under, capacity is 383mA h g-1。
Embodiment 10
The copper nano cubic block that diameter is 150nm is configured to 10mg/mL DMSO solution (the first solution).Then it prepares
The 0.01mol/L BiI of the ammonium tetrafluoroborate of the tetrabutyl containing 0.1mol/L (TBABF4)3DMSO solution (the second solution).It is molten by first
Liquid, the second solution stir after mixing on magnetic stirring apparatus, and mixing speed is 400 revs/min, and copper/bismuth molar ratio is 1:3, instead
It answers 20 hours.By product ethanol washing, centrifugation, hollow bismuth nano cubic block is obtained by vacuum drying.Hollow bismuth is received
Cubic block, carbon black and CMC are according to mass ratio: 7:2:1 is configured to slurry and is coated on copper foil, is assembled into symmetrical electricity with lithium metal thin slice
Pond, diaphragm are glass fibre, and electrolyte is 1M LiPF6EC/DMC/EMC (volume ratio 1:1:1) solution, test battery
Chemical property, in 200mA g-1Under current density, capacity is 330mA h g-1。
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. a kind of preparation method of bismuthino hollow nano-material, which comprises the following steps: copper nano material to be dissolved in
The first solution is obtained in solvent, by BiI3It is dissolved in solvent and obtains the second solution, by first solution and second solution
Mixing obtains bismuthino hollow nano-material after reacting a period of time, and the solvent is dimethyl sulfoxide or N, N- dimethyl allene
Base urea.
2. the preparation method of bismuthino hollow nano-material according to claim 1, which is characterized in that the copper nano material
Shape be copper nano particles, copper nano-wire, copper nanotube, copper nanocone or copper nano cubic block in any one.
3. the preparation method of bismuthino hollow nano-material according to claim 2, which is characterized in that the copper nano particles
Diameter be 2-500nm；The width of the copper nano-wire be 2-500nm, a length of 1-1000 μm；The diameter of the copper nanotube is
10-100nm, it is long are as follows: 1-1000 μm；The size base diameter of the copper nanocone is 50-150nm, tip diameter are as follows: 10-
45nm, length are 1-10 μm；Copper nano cubic block diameter is 10-200nm.
4. the preparation method of bismuthino hollow nano-material according to claim 1, which is characterized in that first solution
Concentration is 0.01-500mg/mL.
5. the preparation method of bismuthino hollow nano-material according to claim 1, which is characterized in that second solution
Configuration method is by BiI3It is dissolved in dimethyl sulfoxide or N, in N- dimethyl propylene alkenyl urea, the tetrabutyl of 0-1mol/L is then added
Ammonium tetrafluoroborate, obtains the second solution, and the concentration of second solution is 0.001-5mol/L.
6. the preparation method of bismuthino hollow nano-material according to claim 1, which is characterized in that the hollow Nano material
The molar ratio of copper and bismuth is 1:0.5-5 in material.
7. the preparation method of bismuthino hollow nano-material according to claim 1, which is characterized in that first solution with
The reaction time of second solution is greater than five minutes.
8. a kind of application of bismuthino hollow nano-material, which is characterized in that bismuthino hollow nano-material is used for sodium-ion battery
Or the negative electrode material of lithium ion battery.
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| CN115178745A (en) * | 2022-06-08 | 2022-10-14 | 西南交通大学 | Multidimensional germanium nano material and preparation method and application thereof |
| CN115178745B (en) * | 2022-06-08 | 2024-04-23 | 西南交通大学 | Multidimensional germanium nanomaterial and preparation method and application thereof |
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