CN110137456A - A kind of Ag/SnS2@rGO, preparation method and application - Google Patents
A kind of Ag/SnS2@rGO, preparation method and application Download PDFInfo
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- CN110137456A CN110137456A CN201910378267.7A CN201910378267A CN110137456A CN 110137456 A CN110137456 A CN 110137456A CN 201910378267 A CN201910378267 A CN 201910378267A CN 110137456 A CN110137456 A CN 110137456A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 provides a kind of Ag/SnS2The preparation method of@rGO weighs a kind of 0.25g flower ball-shaped SnS of Ag modification as described in right 32Preparation method prepare the flower ball-shaped SnS of resulting Ag modification2It is uniform for magnetic agitation in the single-layer graphene oxide dispersion liquid of 1mg/ml that 3~10ml concentration is added, Ag/SnS is prepared in the ascorbic acid self assembly that 0.1~0.5g is then added2@rGO；Inhibit SnS using the lamellar structure of graphene oxide2In insertion/embedding huge volume expansion problem caused out of sodium ion, to further increase the cyclical stability of material, the lamellar structure of simultaneous oxidation graphene can also further limit Ag ion from SnS2The abjection of piece interlayer.
Description
Technical field
The present invention relates to belong to sodium-ion battery technical field, and in particular to a kind of Ag/SnS2It@rGO, preparation method and answers
With.
Background technique
With battery industry fast development, the disadvantage of lithium ion battery is gradually obvious, and lithium resource reserves are limited and can not
Meet the growing energy demand of people, and sodium-ion battery is due to at low cost, rich reserves, widely distributed spy
Point will be increasingly becoming the ideal replacer of lithium ion battery.
Battery technology is the threshold that electric car is widelyd popularize and developed, and current battery industry is in lead-acid battery
It will be battery industry and electric vehicle after graphene energy storage device is succeeded in developing at the time of meeting bottleneck with the development of traditional lithium battery
Industry brings new change.
Graphene is a kind of flat film for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom, is had
Superhigh intensity, extremely strong thermal conductivity, thermal coefficient are up to 5300W/mk, are higher than carbon nanotube and diamond, and electric conductivity is extremely strong,
Its electron mobility is more than 15000cm under room temperature2/ Vs, it is higher than carbon nanotube and silicon crystal, and resistivity only has about 8~10
Ω, it is lower than copper or silver, it is the smallest material of resistivity, from a manufacturing perspective, the graphite as graphene raw materials for production is at me
State's rich reserves, it is cheap, make China that there is unique advantage in graphene research.
SnS2Due to its theoretical capacity with higher, unique layer structure, small polarizing voltage and moderate work electricity
The characteristics of pressure, can be used as the negative electrode material of sodium-ion battery.But SnS2Volume change is larger in charge and discharge process, and electrode is steady
Qualitative difference easily causes granule atomization and reduces capacity.
Summary of the invention
The purpose of the present invention is to provide a kind of Ag/SnS2@rGO, preparation method and application solve existing SnS2
Volume change is larger in charge and discharge process, the defect of electrode stability difference.
In order to achieve the above object, the technical solution adopted by the present invention is that:
A kind of flower ball-shaped SnS provided by the invention2Preparation method, comprising the following steps:
By 0.1~1g SnCl5·5H2O and 20ml polyvinyl alcohol is mixed, and solution A is obtained；By 0.01~0.5g sulfydryl
Acetic acid and 20ml polyvinyl alcohol are mixed, and solution B is obtained；0.1~0.5g CTAB and 30ml polyvinyl alcohol is mixed,
Obtain solution C；
It carries out being stirred by ultrasonic uniformly after solution A and solution C are mixed with the volume ratio of 2:3, obtains product D；
Product D and solution B are mixed with the volume ratio of 5:2, obtain product E；
Product E is put into reaction kettle, hydro-thermal reaction is carried out；Obtained product washed, drying and processing, and bouquet is made
Shape SnS2。
A kind of flower ball-shaped SnS2, based on a kind of flower ball-shaped SnS2Preparation method prepare gained.
A kind of flower ball-shaped SnS of Ag modification2Preparation method, weigh a kind of 0.2~0.5g flower ball-shaped as described in right 1
SnS2Preparation method prepare resulting flower ball-shaped SnS2It being added in the Tollens reagent of 10~30ml, gentle agitation is uniform, it
It instills 3~5ml formaldehyde again afterwards to be stirred uniformly, carries out washing and drying later and recall the flower ball-shaped SnS modified to get Ag2。
Preferably, the preparation method of Tollens reagent: by concentration is 2% silver nitrate and concentration is 2% ammonium hydroxide with 5:1
Volume ratio carry out that obtained Tollens reagent is mixed.
A kind of flower ball-shaped SnS of Ag modification2, the flower ball-shaped SnS based on a kind of Ag modification2Preparation method preparation
Gained.
A kind of Ag/SnS2The preparation method of@rGO weighs a kind of 0.25g flower ball-shaped SnS of Ag modification as described in right 32
Preparation method prepare the flower ball-shaped SnS of resulting Ag modification2The single-layer graphene oxide that 3~10ml concentration is 1mg/ml is added
Magnetic agitation is uniform in dispersion liquid, and Ag/SnS is prepared in the ascorbic acid self assembly that 0.1~0.5g is then added2@rGO。
A kind of Ag/SnS2@rGO, based on a kind of Ag/SnS2The preparation method of@rGO prepares gained.
A kind of Ag/SnS2The application of@rGO, by the SnS2/ CNTs@rGO composite construction is as the negative of sodium-ion battery
Pole material, is assembled into button cell.
Preferably, the specific method for assembling button cell is: cathode uses DMF for solvent, and the formula of pole piece is according to Ag/
SnS2@rGO:PVDF: acetylene black=7:2:1 mass ratio is modulated into slurry, and then slurry is evenly applied on copper foil, is put into
It is dried in vacuum oven, obtains experimental cell negative electrode tab by punching later；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
Compared with prior art, the present invention at least has the advantages that
A kind of flower ball-shaped SnS provided by the invention2And preparation method, flower ball-shaped SnS is prepared using traditional hydro-thermal method2,
It is easy to operate, short preparation period, prepared flower ball-shaped SnS2Thickness is thin, purity is high, crystallinity is strong, and pattern is uniform, possess compared with
Big specific surface area can be gone out with the insertion of sodium ion/embedding more contact sites.
A kind of Ag/SnS provided by the invention2@rGO and preparation method are inhibited using the lamellar structure of graphene oxide
SnS2In insertion/embedding huge volume expansion problem caused out of sodium ion, to further increase the stable circulation of material
Property, meanwhile, the modification of Ag ion can make up SnS2Because the problem of poorly conductive, improving the conduction of material caused by reuniting
Property.
In conclusion the present invention uses a solvent structure SnS2Nano flower, the simple process of synthesis is easy to operate,
And it is nontoxic.The flower ball-shaped SnS of synthesis2Thickness is thin, and purity is high, crystallinity is strong, and pattern is uniform, and it is more to possess biggish specific surface area
Sodium ion contact site, the modification of Ag ion can make up SnS2Because the problem of poorly conductive, improving material caused by reuniting
The electric conductivity of material.Inhibit SnS using the lamellar structure of graphene oxide2Sodium ion insertion/it is embedding go out caused by it is huge
Volume expansion problem, to further increase the cyclical stability of material, the lamellar structure of simultaneous oxidation graphene can also be into
The limitation Ag ion of one step is from SnS2The abjection of piece interlayer.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the flower ball-shaped SnS of superthin section2SEM figure；
Fig. 2 is the flower ball-shaped SnS of amplification2SEM figure；
Fig. 3 is the SnS of 0.35g2The flower ball-shaped SnS for the Ag ion modification being mixed to prepare with the Tollens reagent of 20ml2's
SEM figure.
Specific embodiment
With reference to the accompanying drawing, the present invention is described in more detail.
Ag ion modification flower ball-shaped SnS is wrapped up in a kind of graphene self assembly provided by the invention2It is negative as sodium-ion battery
The preparation method of pole material, comprising the following steps:
Step 1, flower ball-shaped SnS2Preparation:
By 0.1~1g SnCl5·5H2O and 20ml polyvinyl alcohol is mixed, and solution A is obtained；By 0.01~0.5g sulfydryl
Acetic acid and 20ml polyvinyl alcohol are mixed, and solution B is obtained；0.1~0.5g CTAB and 30ml polyvinyl alcohol is mixed,
Obtain solution C, wherein the concentration of solution A is 0.05~0.1ml/L；The concentration of solution B is 0.1~0.5ml/L；
Ultrasound 30min is handled after solution A and solution C are mixed with the volume ratio of 2:3, obtains product D；
Product D and solution B are mixed with the volume ratio of 5:2 again, obtain product E；Product E is put into reaction kettle,
It is carried out hydro-thermal reaction 8~10 hours at 150~220 DEG C；Product water and alcohol after reaction dry at 80 DEG C after respectively washing three times
It is dry, flower ball-shaped SnS is made2；
Step 2, Ag modify flower ball-shaped SnS2Preparation:
Tollens reagent: being that 2% silver nitrate with the ammonium hydroxide that concentration is 2% mix stirring with the volume ratio of 5:1 by concentration
Mixing obtains Tollens reagent.
Weigh the flower ball-shaped SnS of 0.2~0.5g made from step 12The Tollens reagent that 10~30ml is added mildly stirs
It mixes 30 minutes, is stirred 10 hours after instilling 3~5ml formaldehyde, finally, being dried in vacuo at 60 DEG C after for several times with water and ethanol washing
24 hours flower ball-shaped SnS to get Ag modification2。
Step 3, Ag/SnS2The preparation of@rGO:
Weigh the flower ball-shaped SnS of Ag ion modification made from 0.25g step 22It is 1mg/ml's that 3~10ml concentration, which is added,
Then self assembly system at 90 DEG C of ascorbic acid of 0.1~0.5g is added in magnetic agitation 1 hour in single-layer graphene oxide dispersion liquid
It is standby to obtain Ag/SnS2@rGO。
A kind of Ag/SnS2The application of@rGO, by SnS2Negative electrode material of/CNTs@rGO the composite construction as sodium-ion battery,
It is assembled into button cell, specifically:
Cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 quality
Than being modulated into slurry, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, passes through punching later
Obtain experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.The button electricity
Charge and discharge blanking voltage in pond is 0.01~2.6V, and charging or discharging current is 500mA/g.
Embodiment 1
(1) SnCl of 0.1g5·5H2The thioacetic acid of O, 0.01g and the CTAB of 0.1g incorporate 20ml respectively, 20ml and
It is respectively stirred 30 minutes in the polyvinyl alcohol (PEG200) of 30ml, then by SnCl5·5H2Ultrasound is after 30 minutes after O and CTAB mixing
It is mixed 2 hours with thioacetic acid again.
(2) solution being stirred is fitted into 100mL stainless steel cauldron at 200 DEG C and is reacted 10 hours.It is molten after reaction
Liquid water, alcohol are dried at 80 DEG C after respectively washing three times, and flower ball-shaped SnS is made2。
(3) Tollens reagent: 50ml2% silver nitrate is placed in 250ml beaker, be added 1ml 2% ammonium hydroxide stir to
Brown just disappears, and Tollens reagent is made.
(4) 0.2g flower ball-shaped SnS made from step 1 is weighed2It is added Tollens reagent gentle agitation 30 minutes of 10ml,
Stirred 10 hours after instilling 3ml formaldehyde, finally, be dried in vacuo at 60 DEG C after for several times with water and ethanol washing 24 hours to get
The flower ball-shaped SnS of Ag modification2。
(5) the flower ball-shaped SnS of 0.25gAg ion modification is weighed2The single-layer graphene oxide that 3ml concentration is 1mg/ml is added
Then magnetic agitation 1 hour in dispersion liquid is added self assembly at 90 DEG C of ascorbic acid of 0.1g and Ag/SnS is made2@rGO。
Ag ion modification flower ball-shaped SnS is wrapped up in gained graphene self assembly2As anode material of lithium-ion battery electrochemistry
Test method is as follows:
Cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 quality
Than being modulated into slurry, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, passes through punching later
Obtain experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
Carry out charge and discharge cycles test to the button cell: charge and discharge blanking voltage is 0.01-2.6V, and charging or discharging current is
500mA/g。
Embodiment 2
(1) by the SnCl of 0.4655g5·5H2The thioacetic acid of O, 0.2579g and the CTAB of 0.35g incorporate 20ml respectively,
It is respectively stirred 30 minutes in the polyvinyl alcohol (PEG200) of 20ml and 30ml, then by SnCl5·5H2Ultrasound 30 after O and CTAB mixing
It is mixed 2 hours with thioacetic acid again after minute.
(2) solution being stirred is fitted into 100mL stainless steel cauldron at 200 DEG C and is reacted 10 hours.It is molten after reaction
Liquid water, alcohol are dried at 80 DEG C after respectively washing three times, and flower ball-shaped SnS is made2。
(3) Tollens reagent: 50ml2% silver nitrate is placed in 250ml beaker, be added 1ml 2% ammonium hydroxide stir to
Brown just disappears, and Tollens reagent is made.
(4) 0.3g flower ball-shaped SnS made from step 1 is weighed2It is added Tollens reagent gentle agitation 30 minutes of 20ml,
Stirred 10 hours after instilling a little formaldehyde, finally, be dried in vacuo at 60 DEG C after for several times with water and ethanol washing 24 hours to get
The flower ball-shaped SnS of Ag modification2, as shown in exemplary diagram 3.
(5) the flower ball-shaped SnS of 0.25gAg ion modification is weighed2The single-layer graphene oxide that 5ml concentration is 1mg/ml is added
Then magnetic agitation 1 hour in dispersion liquid is added self assembly at 90 DEG C of ascorbic acid of 0.35g and Ag/SnS is made2@rGO。
Ag ion modification flower ball-shaped SnS is wrapped up in gained graphene self assembly2As anode material of lithium-ion battery electrochemistry
Test method is as follows:
Cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 quality
Than being modulated into slurry, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, passes through punching later
Obtain experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
Carry out charge and discharge cycles test to the button cell: charge and discharge blanking voltage is 0.01-2.6V, and charging or discharging current is
500mA/g。
Embodiment 3
(1) by the SnCl of 1g5The thioacetic acid of 5H2O, 0.5g and the CTAB of 0.5g incorporate 20ml respectively, 20ml and
It is respectively stirred 30 minutes in the polyvinyl alcohol (PEG200) of 30ml, then by SnCl5·5H2Ultrasound is after 30 minutes after O and CTAB mixing
It is mixed 2 hours with thioacetic acid again.
(2) solution being stirred is fitted into 100mL stainless steel cauldron at 200 DEG C and is reacted 10 hours.It is molten after reaction
Liquid water, alcohol are dried at 80 DEG C after respectively washing three times, and flower ball-shaped SnS is made2。
(3) Tollens reagent: 50ml2% silver nitrate is placed in 250ml beaker, be added 1ml 2% ammonium hydroxide stir to
Brown just disappears, and Tollens reagent is made.
(4) 0.5g flower ball-shaped SnS made from step 1 is weighed2It is added Tollens reagent gentle agitation 30 minutes of 30ml,
Stirred 10 hours after instilling 5ml formaldehyde, finally, be dried in vacuo at 60 DEG C after for several times with water and ethanol washing 24 hours to get
The flower ball-shaped SnS of Ag modification2。
(5) the flower ball-shaped SnS of 0.25gAg ion modification is weighed2The mono-layer graphite oxide that 10ml concentration is 1mg/ml is added
Then magnetic agitation 1 hour in alkene dispersion liquid is added self assembly at 90 DEG C of ascorbic acid of 0.5g and Ag/SnS is made2@rGO。
Ag ion modification flower ball-shaped SnS is wrapped up in gained graphene self assembly2As anode material of lithium-ion battery electrochemistry
Test method is as follows:
Cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 quality
Than being modulated into slurry, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, passes through punching later
Obtain experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
Carry out charge and discharge cycles test to the button cell: charge and discharge blanking voltage is 0.01-2.6V, and charging or discharging current is
500mA/g。
Embodiment 4
(1) by the SnCl of 0.4655g5The thioacetic acid of 5H2O, 0.2579g and the CTAB of 0.35g incorporate 20ml respectively,
It is respectively stirred 30 minutes in the polyvinyl alcohol (PEG200) of 20ml and 30ml, then by SnCl5·5H2Ultrasound 30 after O and CTAB mixing
It is mixed 2 hours with thioacetic acid again after minute.
(2) solution being stirred is fitted into 100mL stainless steel cauldron at 200 DEG C and is reacted 10 hours.It is molten after reaction
Liquid water, alcohol are dried at 80 DEG C after respectively washing three times, and flower ball-shaped SnS is made2。
(3) Tollens reagent: 50ml2% silver nitrate is placed in 250ml beaker, be added 2% ammonium hydroxide stir it is rigid to brown
It just disappears, Tollens reagent is made.
(4) 0.3g flower ball-shaped SnS made from step 1 is weighed2It is added Tollens reagent gentle agitation 30 minutes of 30ml,
Stirred 10 hours after instilling a little formaldehyde, finally, be dried in vacuo at 60 DEG C after for several times with water and ethanol washing 24 hours to get
The flower ball-shaped SnS of Ag modification2。
(5) the flower ball-shaped SnS of 0.25gAg ion modification is weighed2The single-layer graphene oxide that 5ml concentration is 1mg/ml is added
Then magnetic agitation 1 hour in dispersion liquid is added self assembly at 90 DEG C of ascorbic acid of 0.35g and Ag/SnS is made2@rGO。
Gained graphene self assembly wraps up Ag ion modification flower ball-shaped SnS2 as anode material of lithium-ion battery electrochemistry
Test method is as follows:
Cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 quality
Than being modulated into slurry, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, passes through punching later
Obtain experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to
The volume ratio of 1:1 is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm,
Negative electrode tab, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
Carry out charge and discharge cycles test to the button cell: charge and discharge blanking voltage is 0.01-2.6V, and charging or discharging current is
500mA/g。
Claims (9)
1. a kind of flower ball-shaped SnS2Preparation method, which comprises the following steps:
By 0.1~1g SnCl5·5H2O and 20ml polyvinyl alcohol is mixed, and solution A is obtained；By 0.01~0.5g thioacetic acid
It is mixed with 20ml polyvinyl alcohol, obtains solution B；0.1~0.5g CTAB and 30ml polyvinyl alcohol is mixed, is obtained
Solution C；
It carries out being stirred by ultrasonic uniformly after solution A and solution C are mixed with the volume ratio of 2:3, obtains product D；
Product D and solution B are mixed with the volume ratio of 5:2, obtain product E；
Product E is put into reaction kettle, hydro-thermal reaction is carried out；Obtained product washed, drying and processing, and flower ball-shaped is made
SnS2。
2. a kind of flower ball-shaped SnS2, which is characterized in that it is based on a kind of flower ball-shaped SnS described in claim 12Preparation method system
Standby gained.
3. a kind of flower ball-shaped SnS of Ag modification2Preparation method, which is characterized in that weigh 0.2~0.5g one as described in right 1
Kind flower ball-shaped SnS2Preparation method prepare resulting flower ball-shaped SnS2It is added in the Tollens reagent of 10~30ml, gentle agitation
Uniformly, it instills 3~5ml formaldehyde again later to be stirred uniformly, carries out washing and drying later and recall the bouquet modified to get Ag
Shape SnS2。
4. a kind of flower ball-shaped SnS of Ag modification according to claim 32Preparation method, which is characterized in that Tollens examination
The preparation method of agent: the ammonium hydroxide that concentration is 2% silver nitrate and concentration is 2% is subjected to mixing with the volume ratio of 5:1 and is made
Tollens reagent.
5. a kind of flower ball-shaped SnS of Ag modification2, which is characterized in that based on a kind of flower ball-shaped of Ag modification as claimed in claim 3
SnS2Preparation method prepare gained.
6. a kind of Ag/SnS2The preparation method of@rGO, which is characterized in that weigh a kind of 0.25g modification of the Ag as described in right 3
Flower ball-shaped SnS2Preparation method prepare the flower ball-shaped SnS of resulting Ag modification2The single layer that 3~10ml concentration is 1mg/ml is added
Magnetic agitation is uniform in graphene oxide dispersion, and Ag/ is prepared in the ascorbic acid self assembly that 0.1~0.5g is then added
SnS2@rGO。
7. a kind of Ag/SnS2@rGO, which is characterized in that be based on a kind of Ag/SnS as claimed in claim 62The preparation method of@rGO
Preparation gained.
8. a kind of Ag/SnS2The application of@rGO, it is characterised in that: by SnS as claimed in claim 72/ CNTs@rGO composite construction
As the negative electrode material of sodium-ion battery, it is assembled into button cell.
9. a kind of Ag/SnS according to claim 82The application of@rGO, which is characterized in that assemble the specific side of button cell
Method is: cathode uses DMF for solvent, and the formula of pole piece is according to Ag/SnS2@rGO:PVDF: acetylene black=7:2:1 mass ratio tune
Slurry is made, then slurry is evenly applied on copper foil, is put into vacuum oven and is dried, is obtained later by punching
Experimental cell negative electrode tab；
Using metallic sodium as to electrode；Electrolyte is NaPF6Ethyl carbonate ester and dimethyl carbonate solution according to 1:1's
Volume ratio is mixed；Diaphragm is celgard2400 film；The sequence of assembled battery is followed successively by negative electrode casing, potassium piece, diaphragm, cathode
Piece, gasket, spring leaf, anode cover are assembled into button cell in the glove box full of inert atmosphere.
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Cited By (2)
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