CN110212165A - A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material - Google Patents
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material Download PDFInfo
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Abstract
The present invention provides a kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material: step 1: being washed after carbon cloth is impregnated removal of impurities in acetone, carry out anodized, dried after washing；Step 2: taking graphene oxide and antimony trichloride to be added in dehydrated alcohol and obtain antimony solution, sodium hydrate aqueous solution is then added in antimony solution, adjust pH to 8~12 and obtain mixed solution, the pretreated carbon cloth of step 1 is immersed in mixed solution and is impregnated；Step 3: by step 2 gained mixed solution and carbon cloth, going in reaction vessel the hydro-thermal reaction at 150~180 DEG C, be cooled to room temperature after reaction and take out carbon cloth and clean and dry to obtain carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material.Sb produced by the present invention2O5/ GO/ carbon cloth anode material of lithium-ion battery shows excellent electrochemistry cycle performance, while the preparation method is simple and novel, short preparation period, and repeatability is high, is suitble to large-scale production.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to a kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5/
The preparation method of GO/ carbon cloth electrode material.
Background technique
Sodium element and the same main group of elemental lithium, there are many similar physicochemical properties.But since sodium ion radius (0.113nm) is remote
Greater than lithium ion radius (0.076nm), so that some negative electrode materials for lithium ion battery are applied to sodium-ion battery, meeting
There is capacity is low, difference of magnification and cycle life are short problem, exploring that high-performance anode material of lithium-ion battery has very much thus must
It wants.The research of anode material of lithium-ion battery mainly has carbon material, alloy material, metal oxide, phosphorus etc. at present.Wherein, golden
Belonging to oxide has higher theoretical specific capacity, and by extensive concern.Some metal oxides such as CuO, NiO and Fe2O3, store up sodium
One step conversion reaction only occurs for process, and reaction mechanism is Wherein M is metal, usually
It cannot further be reacted with Na+.Obviously, if metal M can continue occur alloying reaction, further with Na+Reaction, specific volume
Amount can be higher.
Due to Sb and Na+Between alloying reaction can occur, then sb oxide is as anode material of lithium-ion battery
Very high concern is obtained.But metal oxide makees battery material, with being repeated for deintercalation sodium reaction, can generate larger
Bulk effect.Then, it is often modified using compound method in the preparation of traditional electrode.Currently, sb oxide is made
It is Sb that electrode material, which is studied more,2O3Such as JingZhou is prepared for Sb using wet chemistry method2O3/ RGO, as sodium ion electricity
Pond negative electrode material has preferable cyclical stability, is 50mAg in current density-1, first discharge specific capacity 1769mAhg-1,
Reversible capacity is positively retained at 562mAhg after 100 circulations-1(3D nest-shaped Sb2O3/RGO composite
based high-performance lithium-ion batteries.Nanoscale.2016；8(39):17131-
17135).Xiao zhong Zhou etc. is prepared for Sb using wet chemical method2O3/ CNTs/rGO, as sodium-ion battery cathode
Material has preferable cyclical stability, is 200mAg in current density-1, specific capacity is 1090mAhg for the first time-1, 50 circulations
Reversible capacity is positively retained at 543.8mAhg later-1(Facile and rapid synthesis of Sb2O3/CNTs/rGO
nanocomposite with excellent sodium storage performances.Materials
Letters.2016；213:201-203).
It can be seen that Sb can be improved by compound2O3Cyclical stability, but at present for high-valence state sb oxide
Sb2O5Make secondary battery electrode material not report temporarily but.
Summary of the invention
The purpose of the present invention is to provide a kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material
The preparation method of material, by Sb2O5It directly uses in sodium-ion battery cathode, and shows good chemical property.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: carbon cloth being placed in after impregnating removal of impurities in acetone and wash and dry, the carbon cloth after drying carries out at anodic oxidation
Reason, is dried again after washing；
Step 2: 3~10mg graphene oxide and 0.3~1.0g antimony trichloride being taken to be added in 20~60mL dehydrated alcohol
And dissolve, obtain antimony solution；Mixed solution is obtained with sodium hydrate aqueous solution adjusting antimony solution ph to 8~12, after anodic oxidation
Carbon cloth merging mixed solution in impregnate；
Step 3: step 2 gained mixed solution and carbon cloth are gone into reaction vessel the hydro-thermal reaction at 150~180 DEG C,
It is cooled to room temperature after reaction, takes out carbon cloth and cleaned and dried, obtain carbon cloth base flexibility sodium-ion battery cathode Sb2O5/
GO/ carbon cloth electrode material.
Further, it is washed respectively with deionized water and dehydrated alcohol after impregnating 24~72h in carbon cloth merging acetone in step 1
It washs.
Further, electrolyte used in step 1 Anodic Oxidation be concentration be 15~25g/L ammonium dihydrogen phosphate, carbonic acid
One of ammonium dihydrogen, ammonium carbonate, ammonium hydrogen carbonate；Anodic oxidation voltage is 5~10V, and the time is 3~10min.
Further, the mass ratio of graphene oxide and antimony trichloride is 0.5%~1.7% in step 2.
Further, graphene oxide is single-layer graphene oxide powder, and the piece diameter of graphene oxide powder is 0.5~5 μ
M, with a thickness of 0.8~1.2nm.
Further, in step 2 sodium hydrate aqueous solution adjust antimony solution ph process be sodium hydrate aqueous solution by
Step is added in antimony solution and stirs to obtain mixed solution；Impregnate in carbon cloth merging mixed solution after anodic oxidation and stir 20~
40min。
Further, stirring uses magnetic agitation in step 2.
Further, reaction vessel is polytetrafluoroethylkettle kettle in step 3, and mixed solution and carbon cloth go to polytetrafluoroethylkettle kettle
Inside it is placed in 4~48h of hydro-thermal reaction in homogeneous reaction instrument；Cleaning is to be cleaned repeatedly with deionized water and dehydrated alcohol respectively.
Further, the carbon cloth base flexibility sodium-ion battery cathode Sb prepared in step 32O5/ GO/ carbon cloth electrode material
Middle Sb2O5Partial size be 50~100nm, Sb2O5It is uniformly distributed in the carbon cloth substrate that graphene oxide is buffer layer.
Further, carbon cloth is hydrophilic carbon cloth, specification 4cm*2cm.
The beneficial effects of the present invention are embodied in:
The present invention provides a kind of preparations of carbon cloth base flexibility sodium-ion battery cathode Sb2O5/GO/ carbon cloth electrode material
Method, it is innovative by Sb on the basis of combining flexible electrode2O5It is grown into carbon cloth flexible substrates with GO In-situ reaction, and
By the Sb2O5/ GO/ carbon cloth composite material is directly used in sodium-ion battery cathode, and good chemical property is shown；The system
Preparation Method combines Sb2O5As battery electrode material height ratio capacity property and can be with oxygen-enriched functional group as polar oxygen compound
Graphene oxide form firm chemical bonding, while having both graphene oxide and have the characteristics that good dispersion, pass through regulation
The mass ratio of precursors antimony trichloride and graphene oxide, effectively regulates and controls out Sb2O5Homoepitaxial is buffer layer in GO
The composite construction of carbon cloth；The preparation method that the present invention uses is simple and novel, short preparation period, and repeatability is high, compound for preparing
Carbon cloth flexible electrode material has great importance.
Detailed description of the invention
Fig. 1 is carbon cloth base flexibility sodium-ion battery cathode Sb prepared by embodiment 32O5/ GO/ carbon cloth electrode material
X-ray diffracting spectrum；
Fig. 2 is carbon cloth base flexibility sodium-ion battery cathode Sb prepared by embodiment 32O5/ GO/ carbon cloth electrode material
Stereoscan photograph；
Fig. 3 is carbon cloth base flexibility sodium-ion battery cathode Sb prepared by embodiment 32O5/ GO/ carbon cloth electrode material
Electrochemistry cycle performance figure.
Specific embodiment
It elaborates with reference to the accompanying drawings and examples to the present invention.
Embodiment 1:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 72h cleans uses deionized water respectively
It washs with dehydrated alcohol to clean, places after washing and dry at 60 DEG C in an oven；Carbon cloth after drying makees anode, and graphite plate is
Cathode, the ammonium dihydrogen phosphate aqueous solution of 20g/L are that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is to be electrolysed under 5V
3min；The carbon cloth after anodic oxidation is washed to clean with deionized water and dehydrated alcohol, puts and is dried for standby at 60 DEG C of baking oven；
Step 2: taking 3mg graphene oxide and 0.34g antimony trichloride to be added in 20mL dehydrated alcohol and dissolve, it is molten to obtain antimony
Liquid；The sodium hydrate aqueous solution of 0.6g/mL be added dropwise in antimony solution and magnetic agitation adjust antimony pH value of solution must be mixed to 8 it is molten
Liquid；Simultaneously magnetic agitation 30min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single layer
Graphene oxide powder, the piece diameter of graphene oxide powder is 0.5 μm, with a thickness of 0.8nm；
Step 3: step 2 gained mixed solution and carbon cloth are gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument,
The hydro-thermal reaction 6h at 180 DEG C, is cooled to room temperature taking-up carbon cloth after reaction；It is cleaned repeatedly with deionized water and dehydrated alcohol
Carbon cloth to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material；
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 50nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, is assembled into CR2032 type battery, with blue electricity
Test macro carries out cycle performance test, shows higher electrochemistry capacitance and stability.
Embodiment 2:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 72h cleans uses deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, is placed in 60 DEG C of baking ovens and dries after washing；Carbon cloth after drying makees anode, graphite plate
For cathode, the ammonium dihydrogen phosphate aqueous solution of 20g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is to be electrolysed under 5V
5min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, put dried at 60 DEG C of baking oven it is standby
With；
Step 2: taking 6mg graphene oxide and 0.57g antimony trichloride to be added in 30mL dehydrated alcohol and dissolve, it is molten to obtain antimony
Liquid；The sodium hydrate aqueous solution of 0.6g/mL be added dropwise in antimony solution and magnetic agitation adjust antimony pH value of solution must be mixed to 9 it is molten
Liquid；Simultaneously magnetic agitation 30min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single layer
Graphene oxide powder, the piece diameter of graphene oxide powder is 0.8 μm, with a thickness of 1.2nm；
Step 3: step 2 gained mixed solution and carbon cloth are gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument,
The hydro-thermal reaction 12h at 180 DEG C, is cooled to room temperature taking-up carbon cloth after reaction；It is repeatedly clear with deionized water and dehydrated alcohol
Carbon cloth is washed to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material；
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 75nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, is assembled into CR2032 type battery, with blue electricity
Test macro carries out cycle performance test, shows higher electrochemistry capacitance and stability.
Embodiment 3:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 72h cleans uses deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, places after washing and dry at 60 DEG C in an oven；Carbon cloth after drying makees anode, graphite
Plate is cathode, and the ammonium dihydrogen phosphate aqueous solution of 20g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is to be electrolysed under 5V
5min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, put dried at 60 DEG C of baking oven it is standby
With；
Step 2: taking 10mg graphene oxide and 0.57g antimony trichloride to be added in 30mL dehydrated alcohol and dissolve, obtain antimony
Solution；The sodium hydrate aqueous solution of 0.6g/mL, which is added dropwise in antimony solution, and magnetic agitation adjusts antimony pH value of solution must mix to 11
Close solution；Simultaneously magnetic agitation 30min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is
Single-layer graphene oxide powder, the piece diameter of graphene oxide powder is 1.5 μm, with a thickness of 0.9nm；
Step 3: step 2 gained mixed solution and carbon cloth are gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument,
Hydro-thermal reaction for 24 hours, is cooled to room temperature taking-up carbon cloth after reaction at 180 DEG C；It is repeatedly clear with deionized water and dehydrated alcohol
Carbon cloth is washed to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material；
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, as shown in Figure 1, discovery
The Sb that sample and PDF number are 11-06902O5Structure is consistent.As shown in Fig. 2, by sample FEI Co., U.S. S-4800 type
Field emission scanning electron microscope observed, it can be seen that prepared Sb2O5Evengranular be grown in is covered with oxidation stone
On the carbon cloth of black alkene, Sb2O5Partial size be 90nm.As shown in figure 3, with prepared Sb2O5/ GO/ carbon cloth is negative for sodium-ion battery
Pole material is assembled into CR2032 type battery, carries out cycle performance test with blue electrical measurement test system, shows higher electrochemistry and holds
Amount and stability.
Embodiment 4:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 72h cleans uses deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, places after washing and dry at 60 DEG C in an oven；Carbon cloth after drying makees anode, graphite
Plate is cathode, and the ammonium dihydrogen phosphate aqueous solution of 20g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is to be electrolysed under 5V
10min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, put dried at 60 DEG C of baking oven it is standby
With；
Step 2: taking 3mg graphene oxide and 1g antimony trichloride to be added in 40mL dehydrated alcohol and dissolve, obtain antimony solution；
The sodium hydrate aqueous solution of 0.6g/mL be added dropwise in antimony solution and magnetic agitation adjust antimony pH value of solution must be mixed to 10 it is molten
Liquid；Simultaneously magnetic agitation 30min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single layer
Graphene oxide powder, the piece diameter of graphene oxide powder is 2.5 μm, with a thickness of 1nm；
Step 3: mixed solution obtained by step 2) and carbon cloth are gone in polytetrafluoroethylkettle kettle and be placed in homogeneous reaction instrument,
Hydro-thermal reaction for 24 hours, is cooled to room temperature taking-up carbon cloth after reaction at 180 DEG C；It is repeatedly clear with deionized water and dehydrated alcohol
Carbon cloth is washed to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material；
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 70nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, is assembled into CR2032 type battery, with blue electricity
Test macro carries out cycle performance test, shows higher electrochemistry capacitance and stability.
Embodiment 5:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 72h cleans uses deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, places after washing and dry at 60 DEG C in an oven；Carbon cloth after drying makees anode, graphite
Plate is cathode, and the ammonium dihydrogen phosphate aqueous solution of 20g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is electricity under 10V
Solve 5min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, puts and is dried at 60 DEG C of baking oven
It is spare；
Step 2: taking 6mg graphene oxide and 0.8g antimony trichloride to be added in 20mL dehydrated alcohol and dissolve, it is molten to obtain antimony
Liquid；The sodium hydrate aqueous solution of 0.6g/mL, which is added dropwise in antimony solution, and magnetic agitation adjusts antimony pH value of solution must mix to 12
Solution；Simultaneously magnetic agitation 30min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single
Layer graphene oxide powder, the piece diameter of graphene oxide powder is 3.5 μm, with a thickness of 1.1nm；
Step 3: mixed solution obtained by step 2) and carbon cloth are gone in polytetrafluoroethylkettle kettle and be placed in homogeneous reaction instrument,
The hydro-thermal reaction 4h at 180 DEG C, is cooled to room temperature taking-up carbon cloth after reaction；It is cleaned repeatedly with deionized water and dehydrated alcohol
Carbon cloth to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material.
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 80nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, is assembled into CR2032 type battery, with blue electricity
Test macro carries out cycle performance test, shows higher electrochemistry capacitance and stability.
Embodiment 6:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm be placed in 50mL acetone impregnate for 24 hours removal of impurities after use deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, places after washing and dry at 90 DEG C in an oven；Carbon cloth after drying makees anode, graphite
Plate is cathode, and the ammonium dihydrogen phosphate aqueous solution of 15g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is to be electrolysed under 5V
5min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, put dried at 90 DEG C of baking oven it is standby
With；
Step 2: taking 8mg graphene oxide and 0.5g antimony trichloride to be added in 50mL dehydrated alcohol and dissolve, it is molten to obtain antimony
Liquid；The sodium hydrate aqueous solution of 0.6g/mL be added dropwise in antimony solution and magnetic agitation adjust antimony pH value of solution must be mixed to 8 it is molten
Liquid；Simultaneously magnetic agitation 20min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single layer
Graphene oxide powder, the piece diameter of graphene oxide powder is 5 μm, with a thickness of 1.2nm；
Step 3: mixed solution obtained by step 2) and carbon cloth are gone in polytetrafluoroethylkettle kettle and be placed in homogeneous reaction instrument,
Hydro-thermal reaction for 24 hours, is cooled to room temperature taking-up carbon cloth after reaction at 150 DEG C；It is repeatedly clear with deionized water and dehydrated alcohol
Carbon cloth is washed to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material.
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 60nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, is assembled into CR2032 type battery, with blue electricity
Test macro carries out cycle performance test, shows higher electrochemistry capacitance and stability.
Embodiment 7:
A kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, including it is following
Step:
Step 1: by long 4cm, the carbon cloth of wide 2cm is placed in 50mL acetone to impregnate after 48h cleans uses deionized water respectively
It is washed repeatedly with dehydrated alcohol to clean, places after washing and dry at 120 DEG C in an oven.Carbon cloth after drying makees anode, stone
Black plate is cathode, and the ammonium dihydrogen phosphate aqueous solution of 20g/L is that electrolyte carries out anodic oxidation to carbon cloth, and decomposition voltage is electricity under 5V
Solve 8min；The carbon cloth after anodic oxidation is washed repeatedly to clean with deionized water and dehydrated alcohol, puts and is dried at 120 DEG C of baking oven
It is spare；
Step 2: taking 5mg graphene oxide and 0.7g antimony trichloride to be added in 60mL dehydrated alcohol and dissolve, it is molten to obtain antimony
Liquid；The sodium hydrate aqueous solution of 0.6g/mL be added dropwise in antimony solution and magnetic agitation adjust antimony pH value of solution must be mixed to 9 it is molten
Liquid；Simultaneously magnetic agitation 40min will be impregnated in carbon cloth after anodic oxidation merging mixed solution；Wherein, graphene oxide is single layer
Graphene oxide powder, the piece diameter of graphene oxide powder is 0.9 μm, with a thickness of 1.2nm；
Step 3: mixed solution obtained by step 2) and carbon cloth are gone in polytetrafluoroethylkettle kettle and be placed in homogeneous reaction instrument,
The hydro-thermal reaction 36h at 150 DEG C, is cooled to room temperature taking-up carbon cloth after reaction；It is repeatedly clear with deionized water and dehydrated alcohol
Carbon cloth is washed to clean, after drying carbon cloth base flexibility sodium-ion battery cathode Sb2O5/ GO/ carbon cloth electrode material.
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ GO/ carbon cloth sample, discovery sample and PDF are compiled
Number be 11-0690 Sb2O5Structure is consistent.By the sample field emission scanning electron microscope of FEI Co., U.S. S-4800 type
It is observed, it can be seen that prepared Sb2O5It is evengranular to be grown on the carbon cloth for being covered with graphene oxide, Sb2O5Grain
Diameter is 100nm.With prepared Sb2O5/ GO/ carbon cloth is anode material of lithium-ion battery, CR2032 type battery is assembled into, with indigo plant
Electrical measurement test system carries out cycle performance test, shows higher electrochemistry capacitance and stability.
In short, the present invention is on the basis of combining flexible electrode, it is innovative by Sb2O5Carbon is grown into GO In-situ reaction
In cloth flexible substrates, and by the Sb2O5/ GO/ carbon cloth composite material is directly used in sodium-ion battery cathode, is shown good
Chemical property.This method combines Sb2O5As battery electrode material height ratio capacity property and can be with as polar oxygen compound
The graphene oxide of oxygen-enriched functional group forms firm chemical bonding, while having both the spy that graphene oxide has good dispersion
Point effectively regulates and controls out Sb by regulating and controlling the mass ratio of precursors antimony trichloride and graphene oxide2O5Homoepitaxial in
GO is the composite construction of the carbon cloth of buffer layer.The preparation method that the present invention uses is simple and novel, short preparation period, and repeatability is high,
Have great importance for preparing compound carbon cloth flexible electrode material.
Claims (10)
1. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb2O5The preparation method of/GO/ carbon cloth electrode material, feature exist
In, comprising the following steps:
Step 1: carbon cloth is placed in after impregnating removal of impurities in acetone and washs and dry, the carbon cloth after drying carries out anodized,
It is dried again after washing；
Step 2: taking 3~10mg graphene oxide and 0.3~1.0g antimony trichloride to be added in 20~60mL dehydrated alcohol and molten
Solution, obtains antimony solution；Mixed solution is obtained with sodium hydrate aqueous solution adjusting antimony solution ph to 8~12, by the carbon after anodic oxidation
It is arranged into mixed solution and impregnates；
Step 3: step 2 gained mixed solution and carbon cloth are gone into hydro-thermal reaction, reaction at 150~180 DEG C in reaction vessel
After be cooled to room temperature, take out carbon cloth cleaned and dried, obtain carbon cloth base flexibility sodium-ion battery cathode Sb2O5/GO/
Carbon cloth electrode material.
2. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that use deionized water and nothing respectively after impregnating 24~72h in carbon cloth merging acetone in the step 1
Water-ethanol water washing.
3. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 1 or claim 22O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that electrolyte used in step 1 Anodic Oxidation is the di(2-ethylhexyl)phosphate that concentration is 15~25g/L
One of hydrogen ammonium, carbonic acid ammonium dihydrogen, ammonium carbonate, ammonium hydrogen carbonate；Anodic oxidation voltage is 5~10V, and the time is 3~10min.
4. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that the mass ratio of graphene oxide and antimony trichloride is 0.5%~1.7% in the step 2.
5. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 42O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that the graphene oxide is single-layer graphene oxide powder, and the piece diameter of graphene oxide powder is
0.5~5 μm, with a thickness of 0.8~1.2nm.
6. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that it is sodium hydroxide water that sodium hydrate aqueous solution, which adjusts the process of antimony solution ph, in the step 2
Solution is added step-wise in antimony solution and stirs to obtain mixed solution；It impregnates and stirs in carbon cloth merging mixed solution after anodic oxidation
Mix 20~40min.
7. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 62O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that stirring uses magnetic agitation in the step 2.
8. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that reaction vessel is polytetrafluoroethylkettle kettle in the step 3, and mixed solution and carbon cloth go to poly- four
4~48h of hydro-thermal reaction in homogeneous reaction instrument is placed in vinyl fluoride kettle；Cleaning is to use deionized water and dehydrated alcohol repeatedly respectively
Cleaning.
9. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that the carbon cloth base flexibility sodium-ion battery cathode Sb prepared in the step 32O5/ GO/ carbon cloth electricity
Sb in the material of pole2O5Partial size be 50~100nm, Sb2O5Uniformly it is distributed in the carbon cloth substrate that graphene oxide is buffer layer
On.
10. a kind of carbon cloth base flexibility sodium-ion battery cathode Sb according to claim 12O5/ GO/ carbon cloth electrode material
Preparation method, which is characterized in that the carbon cloth be hydrophilic carbon cloth, specification 4cm*2cm.
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