CN109980208A - A kind of flexible four vulcanize three vanadium-carbon composite anode material and its preparation method and application - Google Patents
A kind of flexible four vulcanize three vanadium-carbon composite anode material and its preparation method and application Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of flexible four vulcanizations, three vanadium-carbon composite anode materials and its preparation method and application, by flexible carbon fiber and the spherical V of nanometer for being carried on flexible carbon fiber surface3S4It constitutes, wherein the spherical V of nanometer3S4Load capacity be 1-2mg/cm2.The composite positive pole has outstanding electric conductivity and flexibility, V3S4Crystal structure be conducive to the insertion and abjection of zinc ion, improve the storage and transport of zinc ion, improve the capacity of battery, carbon fiber is greatly improved the electron conduction of positive electrode, further enhance the chemical property of battery, entire electrode has excellent flexibility, repeatedly still has excellent chemical property after bending.
Description
Technical field
The present invention relates to a kind of flexible four vulcanizations, three vanadium-carbon composite anode materials and its preparation method and application, belong to water
Property Zinc ion battery technical field.
Background technique
Make rapid progress with scientific and technical and industrialization development, the living standard of numerous people also has benefited from various civilian
The appearance of electronic equipment and increasingly improve.These tools of emerging electronic product as people's daily work life, it is common that
Use electric energy as its energy source, and the current common developing direction of electronic equipment be all lightweight, it is portable, long
Continuation of the journey, while in miscellaneous different application equipment, battery will also have both universality and safety, this hair for battery
A harsh problem has undoubtedly been shown in exhibition.Such as in this hot fields of flexible power devices, if battery is not able to maintain
Bending synchronous with flexible device is simultaneously with good performance, then flexible power devices also will be meaningless.Flexible lithium ion
Although battery is widely used at present, but still has several the drawbacks of cannot being missed.Firstly, its electrolyte it is usually used be to have
Based on machine series solvent, the major accidents such as spontaneous combustion or explosion easily occur in improper use or day-to-day loss.Second, lithium ion
Requirement of the battery for working condition is very harsh, it is clear which increase the costs of its production.And emerging Water-Electrolyte can
Charging water system flexible battery is a kind of substitute of promising flammable organic bath, with traditional expensive, inflammable flexibility
Lithium battery is compared, and chargeable water system flexible battery is at low cost with its, safety is good, the advantages that being easily assembled to causes the wide of people
General concern.
Although water system Zinc ion battery has many advantages, such as, also there is its unfavorable one side.Such as water system zinc ion electricity
Pond positive electrode electronic conductivity is insufficient, and the diffusion of ion is poor, causes its stored energy capacitance lower.Therefore, high-performance is studied
Zinc ion battery positive electrode meets the needs of present society is to novel water system flexibility Zinc ion battery, is that current urgent need solves
The problem of.
In current research, the just extremely conducting polymer/fibre of that soldier equal (application number 201810083285.8) preparation
Plain paper/graphite nano plate composite material is tieed up, is to use cellulose paper and nano-cellulose as the skeleton material of Zinc ion battery
Material is made with the Zinc ion battery compared with high-flexibility and bending stability, so as to be applied to wearable electronic
And the fields such as artificial intelligence, but the electric conductivity of its anode is still to be improved；(application numbers 201810083285.8) such as all boats
Sheet manganese dioxide and graphene composite and flexible electrode then is prepared with vacuum filtration method, does not need addition binder, improves
Mass ratio of the active material in entire electrode, to improve the energy density of electrode.
By above-mentioned retrieval it can be found that current technical step is relatively complicated, still pay attention to traditional positive electrode, such as
The development and utilization of manganese dioxide etc., it is still insufficient for the promotion of positive electrode electric conductivity and battery capacity, for novel
Positive electrode, such as vanadium sulfide (V3S4) etc. be applied to flexible electrode, promoted water system battery performance be also rarely reported.
Summary of the invention
Aiming at the problem that existing water system Zinc ion battery positive electrode poorly conductive and off-capacity etc., the present invention
Purpose be to be the provision of a kind of flexible four vulcanizations, three vanadium-carbon composite anode material and its preparation method and application, this is compound
Positive electrode has outstanding electric conductivity and flexibility, V3S4Structure be conducive to the insertion and abjection of zinc ion, improve zinc ion
Storage and transport, improve the capacity of battery, carbon fiber is greatly improved the electron conduction of positive electrode, further increase
The strong chemical property of battery, entire electrode have excellent flexibility, repeatedly still have excellent chemical property after bending.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of flexible four vulcanizations, three vanadium-carbon composite anode material, by flexible carbon fiber and is carried on flexible carbon fiber surface
The spherical V of nanometer3S4It constitutes, wherein the spherical V of nanometer3S4Load capacity be 1-2mg/cm2。
Preferably, the spherical V of the nanometer3S4Partial size be 200-500nm.
The present invention also provides the preparation methods of above-mentioned flexible four vulcanizations, three vanadium-carbon composite anode material, including walk as follows
It is rapid:
Step 1
Sulphur powder and vanadyl acetylacetonate powder are added in N-N dimethylformamide (DMF) with mass ratio 1:4~2:3 and stirred
Mix and be mixed to get mixed solution, control 65-80 DEG C of whipping temp, stirring rate be 300~800r/min, mixing time be 12~
For 24 hours, the solid-to-liquid ratio of mixed-powder and DMF are 1g:10~30mL；
Step 2
It is 0.8~1.5g:4~9cm by the mass area ratio of mixed-powder and carbon cloth2, step 1 is obtained mixed
2~4h of solvent thermal reaction is carried out at 140~180 DEG C up to composite material precursor after closing solution and carbon cloth mixing；
Step 3
The composite material precursor for taking step 2 to obtain under inert atmosphere protection in 400~700 DEG C of 2~4h of calcining to obtain the final product
Flexibility four vulcanizes three vanadium-carbon composite anode material.
The present invention selects specific sulphur source and vanadium source, is aided with specific solvent DMF, is first mixed under certain conditions
Presoma is obtained, solvent-thermal method is then used, controls reaction temperature and time, using DMF as inducer, presoma forming core is grown up
The substance spherical to nanometer, is finally calcined under protective atmosphere, obtains the spherical flexible V of nanometer3S4C composite.Invention
People's discovery, selects other sulphur sources, such as thioacetamide etc. selects other vanadium source, such as vanadic anhydride, ammonium metavanadate
Deng selecting other solvents, such as water, ethyl alcohol etc., cannot obtain the V of pure phase3S4, component, which matches, must also control at this
In invention scope, when the mass ratio of sulphur powder and vanadyl acetylacetonate powder is less than 1:4, sulphur powder amount cannot be vulcanized to needs
Object phase, only obtain the mixture of the vanadium sulfide of Low-valent Titanium；And when the mass ratio of sulphur powder and vanadyl acetylacetonate powder is greater than
When 2:3, sulphur powder amount be it is excessive, can obtain other proportion or high-valence state vanadium sulfide mixture.
Inventor also found, in preparation process, either react before stirring, solvent thermal reaction still react after forge
It burns, the washing after even reacting, the parameter of each step need to strictly regulate and control, not so will lead to last product and become
Change, the present invention is based on raw material components and its synergistic effect of proportion and preparation process parameter, the nanometer for finally obtaining pure phase are spherical
Flexible V3S4C composite.
Preferably, in step 1, the average grain diameter of sulphur powder is 400~800 mesh, the average grain diameter of vanadyl acetylacetonate powder
For 600~1000 mesh, sulphur powder, vanadyl acetylacetonate powder purity are that analysis is pure.
The present invention also provides the applications of above-mentioned flexible four vulcanizations, three vanadium-carbon composite anode material, are used as water system zinc
Ion battery positive electrode.
Preferably, with V3S4- C deposits zinc using on carbon cloth as cathode, assembling obtains water system zinc ion as anode
Flexible battery, 0 ° -90 ° -180 ° -0 ° under different bending states, 500mAg-1Current density under, respectively recycle 50 circle,
After 200 circles, battery still has the specific capacity of 143-151mAh/g, and capacity retention ratio reaches 91-93%.
Principle and advantage
The present invention raw material, finally obtained flexibility based on sulphur powder, vanadyl acetylacetonate powder and flexible carbon fiber
V3S4- C Zinc ion battery composite positive pole has outstanding electric conductivity and flexibility, V3S4Crystal structure be conducive to zinc ion
Insertion and abjection, improve the storage and transport of zinc ion, improve the capacity of battery；Flexible carbon in composite positive pole
Fibre composition is greatly improved the electron conduction of positive electrode, further enhances the electrochemistry correlated performance of battery, and
And the presence of carbon cloth allows entire electrode to have outstanding flexibility, repeatedly still has outstanding battery performance after bending.
The present invention overcomes existing technical disadvantages, compensate for the deficiency of existing cell positive material electric conductivity, realize
V3S4Controllable preparation and load, make composite positive pole have fabulous flexibility and electric conductivity, improve battery capacity, enhance
The chemical property of battery, and preparation flow is simple and easy, have very vast potential for future development and economic benefit.
Detailed description of the invention
Fig. 1 is the XRD diagram of composite positive pole made from embodiment 1；
Fig. 2 is SEM and the TEM figure of composite positive pole made from embodiment 1；
Fig. 3 is the XPS figure of composite positive pole made from embodiment 1；
Fig. 4 is composite positive pole made from embodiment 1 at different bending states (0 ° -90 ° -180 ° -0 °)
Under test chart；
Fig. 5 is the specific capacitance and coulombic efficiency figure of composite positive pole made from embodiment 1；
Fig. 6 is the XRD diagram of composite positive pole made from comparative example 1；
Fig. 7 is the XRD diagram of composite positive pole made from comparative example 2；
Fig. 8 is the XRD diagram of composite positive pole made from comparative example 3；
Fig. 9 is the XRD diagram of composite positive pole made from comparative example 4；
Figure 10 is the XRD diagram of composite positive pole made from comparative example 5；
Figure 11 is the XRD diagram of composite positive pole made from comparative example 6；
Figure 12 is the XRD diagram of composite positive pole made from comparative example 7；
Figure 13 is the XRD diagram of composite positive pole made from comparative example 8；
Figure 14 is the XRD diagram of composite positive pole made from comparative example 9；
Figure 15 is the XRD diagram of composite positive pole made from comparative example 10；
Figure 16 is the XRD diagram of composite positive pole made from comparative example 11；
Figure 17 is the XRD diagram of composite positive pole made from comparative example 12.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments.
Embodiment 1
(1) composite material is prepared: sulphur powder 20%, vanadyl acetylacetonate powder 80% by mass percentage, according to solid
Powder: DMF solution is added in the ratio of N-N dimethylformamide (DMF) solution=1g:10mL, is stirred at 65 DEG C
Even, control stirring rate is 600r/min, mixing time 12h, guarantees solid powder being uniformly mixed in DMF solution；?
To mixed solution pour into high-temperature high-pressure reaction kettle, by mass percentage, thereto be added 2cm × 2cm carbon cloth
It is a piece of, then reaction kettle is placed in baking oven, after reacting 2h at 140 DEG C, is rinsed 3 times with ethyl alcohol.
(2) it prepares flexible battery composite positive pole: taking composite material obtained in (1) in tube furnace, in 400 DEG C of nitrogen
Under gas atmospheric condition, 2h is calcined to get flexible battery composite positive pole.Its XRD diagram is shown in that Fig. 1, SEM and TEM figure are shown in Fig. 2, from
It can be seen that in Fig. 1 and Fig. 2 and V be successfully prepared3S4；The spherical V of flexible carbon fiber surface uniform load nanometer3S4；Nanometer
Spherical V3S4It is medicine ball.As shown in figure 3, XPS analysis V3S4Chemical valence composition, it can be seen that wherein there are two types of chemical valence
V element, trivalent and 4 valences.
(3) assembling of flexible battery: being anode with flexible battery composite material obtained in (2), to sink on carbon cloth
Product zinc carries out V as cathode3S4The assembling of-C anode composite flexible battery.
(4) electrochemical property test under bending: by gained anode composite flexible battery in (3) in different bending states
Lower 0 ° -90 ° -180 ° -0 ° (as shown in Figure 4), 500mAg-1Current density under, respectively recycle 50 circle, 200 circle after, battery still has
There is the specific capacity of 148mAh/g, capacity retention ratio reaches 92%, as shown in Figure 5.
Embodiment 2
(1) composite material is prepared: sulphur powder 30%, vanadyl acetylacetonate powder 70% by mass percentage, according to solid
Powder: the ratio of N-N dimethylformamide (DMF) solution=1g:20mL is added DMF solution, is uniformly mixed at 70 DEG C,
Control stirring rate is 600r/min, and mixing time is for 24 hours, to guarantee solid powder being uniformly mixed in DMF solution；It obtains
Mixed solution pours into high-temperature high-pressure reaction kettle, by mass percentage, the business carbon cloth of 2cm × 2cm is added thereto
It is a piece of, then reaction kettle is placed in baking oven, after reacting 3h at 160 DEG C, is rinsed 3 times with ethyl alcohol.
(2) it prepares flexible battery composite positive pole: taking composite material obtained in (1) in tube furnace, in 500 DEG C of nitrogen
Under gas atmospheric condition, 2h is calcined to get flexible battery composite positive pole.
(3) assembling of flexible battery: being anode with flexible battery composite material obtained in (2), to sink on carbon cloth
Product zinc carries out the assembling of anode composite flexible battery as cathode.
(4) electrochemical property test under bending: by gained anode composite flexible battery in (3) in different bending states
Lower 0 ° -90 ° -180 ° -0 °, 500mA g-1Current density under, respectively recycle 50 circle, 200 circle after, battery still has 143mAh/g
Specific capacity, capacity retention ratio reaches 93%.
Embodiment 3
(1) composite material is prepared: sulphur powder 40%, vanadyl acetylacetonate powder 60% by mass percentage, according to solid
Powder: the ratio of N-N dimethylformamide (DMF) solution=1g:30mL is added DMF solution, is uniformly mixed at 80 DEG C,
Control stirring rate is 600r/min, and mixing time is for 24 hours, to guarantee solid powder being uniformly mixed in DMF solution；It obtains
Mixed solution pours into high-temperature high-pressure reaction kettle, by mass percentage, the business carbon cloth of 2cm × 2cm is added thereto
It is a piece of, then reaction kettle is placed in baking oven, after reacting 4h at 180 DEG C, is rinsed 3 times with ethyl alcohol.
(2) it prepares flexible battery composite positive pole: taking composite material obtained in (1) in tube furnace, in 700 DEG C of nitrogen
Under gas atmospheric condition, 4h is calcined to get flexible battery composite positive pole.
(3) assembling of flexible battery: being anode with flexible battery composite material obtained in (2), to sink on carbon cloth
Product zinc carries out the assembling of anode composite flexible battery as cathode.
(4) electrochemical property test under bending: by gained anode composite flexible battery in (3) in different bending states
Lower 0 ° -90 ° -180 ° -0 °, 500mAg-1Current density under, respectively recycle 50 circle, 200 circle after, battery still has 151mAh/g
Specific capacity, capacity retention ratio reaches 91%.
Comparative example 1
With embodiment 3, difference is only that sulphur powder 10%, the proportion of vanadyl acetylacetonate powder 90% add by mass percentage
Enter, in such cases, obtains a series of mixture of other vanadium sulfide, the mutually correct V of object cannot be obtained3S4, such as Fig. 6.
Comparative example 2
With embodiment 3, difference is only that sulphur powder 50%, the proportion of vanadyl acetylacetonate powder 50% add by mass percentage
Enter, in such cases, is similarly obtained a series of mixture of other vanadium sulfide, the mutually correct V of object cannot be obtained3S4, such as Fig. 7.
Comparative example 3
With embodiment 3, only setting whipping temp is that room temperature cannot obtain the mutually correct V of object in such cases for difference3S4,
Such as Fig. 8.
Comparative example 4
With embodiment 3, only setting solvent thermal reaction temperature is 100 DEG C for difference, in such cases, it is mutually correct cannot to obtain object
V3S4, such as Fig. 9.
Comparative example 5
With embodiment 3, only setting solvent thermal reaction temperature is 200 DEG C for difference, in such cases, it is mutually correct cannot to obtain object
V3S4, such as Figure 10.
Comparative example 6
With embodiment 3, only the setting solvent thermal reaction time is that it is mutually correct cannot to obtain object in such cases by 1h for difference
V3S4, such as Figure 11.
Comparative example 7
With embodiment 3, only the setting solvent thermal reaction time is that it is mutually correct cannot to obtain object in such cases by 5h for difference
V3S4, such as Figure 12.
Comparative example 8
With embodiment 3, difference is that reaction dissolvent cannot obtain the mutually correct V of object in such cases only with ethyl alcohol3S4,
Such as Figure 13.
Comparative example 9
With embodiment 3, difference is that it is mutually correct cannot to obtain object in such cases for reaction dissolvent only with deionized water
V3S4, such as Figure 14.
Comparative example 10
With embodiment 3, it is that it is mutually correct cannot to obtain object in such cases for sulphur source that thioacetamide is only selected in difference
V3S4, such as Figure 15.
Comparative example 11
With embodiment 3, it is that it is mutually correct cannot to obtain object in such cases for vanadium source that vanadic anhydride is only selected in difference
V3S4, such as Figure 16.
Comparative example 12
With embodiment 3, only solvent thermal reaction backlash is washed into and is washed with deionized for difference, in such cases, cannot be obtained
To the mutually correct V of object3S4, such as Figure 17.
Claims (6)
1. a kind of flexible four vulcanizations, three vanadium-carbon composite anode material, it is characterised in that: by flexible carbon fiber and be carried on flexible carbon
The spherical V of the nanometer of fiber surface3S4It constitutes, wherein the spherical V of nanometer3S4Load capacity be 1-2mg/cm2。
2. flexible four vulcanizations, three vanadium-carbon composite anode material according to claim 1, it is characterised in that: the nanosphere
Shape V3S4Partial size be 200-500nm.
3. the preparation method of flexible four vulcanizations, three vanadium-carbon composite anode material of any of claims 1 or 2, which is characterized in that packet
Include following steps:
Step 1
Stirring in N-N dimethylformamide (DMF) is added with mass ratio 1:4~2:3 in sulphur powder and vanadyl acetylacetonate powder to mix
Conjunction obtains mixed solution, controls 65-80 DEG C of whipping temp, and stirring rate is 300~800r/min, and mixing time is 12~for 24 hours,
The solid-to-liquid ratio of mixed-powder and DMF are 1g:10~30mL；
Step 2
It is 0.8~1.5g:4~9cm by the mass area ratio of mixed-powder and carbon cloth2, mixed solution that step 1 is obtained
2~4h of solvent thermal reaction is carried out after mixing with carbon cloth at 140~180 DEG C up to composite material precursor；
Step 3
The composite material precursor for taking step 2 to obtain is under inert atmosphere protection in 400~700 DEG C of 2~4h of calcining up to flexible
Four vulcanization three vanadium-carbon composite anode materials.
4. preparation method according to claim 3, it is characterised in that: in step 1, the average grain diameter of sulphur powder is 400~
The average grain diameter of 800 mesh, vanadyl acetylacetonate powder is 600~1000 mesh, and sulphur powder, vanadyl acetylacetonate powder purity are point
It analyses pure.
5. claim 1-2 described in any item flexible four vulcanizations any one of three vanadium-carbon composite anode materials or claim 3-4
The application of the vulcanization three vanadium-carbon composite anode material of flexibility four made from the preparation method, it is characterised in that: be used as water
It is Zinc ion battery positive electrode.
6. the application of flexible four vulcanizations, three vanadium-carbon composite anode material according to claim 5, it is characterised in that: with
V3S4- C deposits zinc using on carbon cloth as cathode, assembling obtains water system zinc ion flexible battery, different as anode
Lower 0 ° -90 ° -180 ° -0 ° of bending state, 500mA g-1Current density under, respectively recycle 50 circle, 200 circle after, battery still has
The specific capacity of 143-151mAh/g, capacity retention ratio reach 91-93%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111554931A (en) * | 2020-05-11 | 2020-08-18 | 中科廊坊过程工程研究院 | Composite positive electrode material, preparation method thereof and application thereof in zinc ion battery |
| CN111554931B (en) * | 2020-05-11 | 2021-09-14 | 中科廊坊过程工程研究院 | Composite positive electrode material, preparation method thereof and application thereof in zinc ion battery |
| WO2021227594A1 (en) * | 2020-05-11 | 2021-11-18 | 中国科学院过程工程研究所 | Composite positive electrode material, preparation method therefor, and application in zinc ion battery |
| CN114142043A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
| CN114142048A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium cell |
| CN114142048B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium battery |
| CN114142043B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
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