CN109904422A - A kind of preparation method and application of four vanadic sulfides@Super P composite granule - Google Patents
A kind of preparation method and application of four vanadic sulfides@Super P composite granule Download PDFInfo
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Abstract
A kind of preparation method of four vanadic sulfides@Super P composite granule, includes the following steps；The Super P for weighing 48~52mg is added in 58~62ml deionized water, and 1.5~2.5h of ultrasound obtains the dark solution A that is uniformly dispersed；It weighs 0.9~1.1g sodium metavanadate and 3.5~3.7g thioacetamide and is added in solution A simultaneously, 30~60min of magnetic agitation obtains solution B；Liner is then placed in homogeneous reaction instrument loaded on fixation in outer kettle, then under the speed conditions of 5~10r/min, 23~25h is reacted at 175~185 DEG C by sealing after solution B is poured into reaction liner；Hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the product cooled down after reaction, collects product after 2~5 water and 2~5 alcohol alternately clean；The product of collection is placed in the cold well of freeze drier and is freezed, then the product after freezing is placed in pallet, cover seal closure, it is evacuated down to 10~20Pa, product is collected after dry 12~18h, the present invention has the characteristics that reaction process is simple, temperature is low, reaction condition that is easily-controllable and not needing large scale equipment and harshness.
Description
Technical field
The present invention relates to four vanadic sulfide@Super P composite granule technical fields, in particular to four vanadic sulfide@Super of one kind
The preparation method and application of P composite granule.
Background technique
As a kind of typical transient metal sulfide, VS4With one-dimensional catenary structure.Wherein, two S2 2-Group (four
A S) close around around V, and expanded along the direction c and form VS4Strand, two neighboring VS4By weak between strand
Van der Waals force connection, chain spacing can reach(Rout CS,Kim B-H,et al.J Am Chem
Soc.2013,135:8720-8725.).It is similar to FeS2, VS4From natural minerals patronite, and the valence state of S is -1,
The valence state of V is+4.Above structure characteristic makes VS4Photocatalysis, hydrofining reaction, lithium ion battery, supercapacitor, aluminium from
The fields such as sub- battery, Magnesium ion battery are applied.However, since the characteristic of V easily oxyphie, reaction process require accurate S
The presence of partial pressure and various non-stoichiometric vanadic sulfides, since VS in 19704By since reporting for the first time, about their conjunction
At receiving biggish obstruction (Xu X, Jeong S, et al.J Mater Chem is A.2014,2:10847-10853.).And
And for VS4Synthesis usually require introduce template.Sun R et al. is prepared for being grown on reduced graphene using hydro-thermal method
The VS on surface4(Sun R,Wei Q,et al.ACS Appl Mater Inter.2015,7:20902-20908.).Li S etc.
People has synthesized VS by flexible hydro-thermal method4Nanometer sheet is stacked in nanocomposite (Li S, He on redox graphene
W,et al.Mater Lett.2017,205:52-55.).Pang Q et al. is assisted by CTAB cationic surfactant
Hydro-thermal method is prepared for the VS of uniform graphene film anchoring4Nano particle, then by changing the additional amount of graphene film, control
VS4The size (Pang Q, Zhao Y, et al.ChemSusChem.2018,11:735-742.) of nano particle.Wang S
Et al. use in-situ oxidation graphene hydrothermal template method, by control graphene oxide template content be made uniform rectangular
Figure VS4Nano particle (Wang S, Gong F, et al.Adv Funct Mater.2018,28:1801806.).Rout CS
Et al. pass through in hydrothermal system introduce graphene oxide, the carbon nanotube of carboxylated, the pyrene rich in lock machine, tetracarboxylic acid two
The carbon materials such as acid anhydride, graphite have successfully obtained they and VS4Compound (Rout CS, Kim B-H, et al.J Am Chem
Soc.2013,135:8720-8725.).However, it is above-mentioned it has been reported that composite material in, a part of VS4It is not grown on
Carbon material surface, only VS4With the compound of carbon material, although another part has been grown in carbon material surface, but be distributed
It is more sparse and random, and VS4Pattern also it is irregular uniformly.It is this insufficient and inefficient compound to make VS4High-performance
It can not be played well.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is multiple that the purpose of the present invention is to provide four vanadic sulfide@Super P of one kind
Close raw powder's production technology and application, the present invention using water as solvent, with sodium metavanadate and thioacetamide be respectively vanadium source with
Sulphur source, and Super P carbon source is introduced, pass through their concentration of Collaborative Control and proportion, reaction temperature, reaction time, packing ratio
Etc. parameters, realize an one-step template-free agent hydro-thermal method in Super P nanosphere surface in situ and generate flexible winding shape VS4Nanometer rods
Structure, this method reaction process is simple, temperature is low, reaction condition that is easily-controllable and not needing large scale equipment and harshness, can be one
VS is directly realized by a reaction process4Formation and P nanometers of ball surfaces of Super original position winding.When by above-mentioned product application
When for lithium/anode material of lithium-ion battery and optical electrical catalyst, it can show excellent chemical property and catalytic
Energy.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of preparation method of four vanadic sulfides@Super P composite granule, includes the following steps；
Step 1: the Super P for weighing 48~52mg is added in 58~62ml deionized water, and 1.5~2.5h of ultrasound is obtained
To the dark solution A that is uniformly dispersed；
Step 2: weighing 0.9~1.1g sodium metavanadate and 3.5~3.7g thioacetamide and be added in solution A simultaneously,
30~60min of magnetic agitation obtains solution B；
Solution B: being poured into sealing after reacting in liner by step 3, is then placed on liner homogeneously loaded on fixed in outer kettle
It reacts in instrument, then under the speed conditions of 5~10r/min, 23~25h is reacted at 175~185 DEG C；
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction
Out, product is collected after 2~5 water and 2~5 alcohol alternately clean；
Step 5: the product of collection being placed in the cold well of freeze drier and freezed, then by the product after freezing
It is placed in pallet, covers seal closure, be evacuated down to 10~20Pa, collect product after dry 12~18h, four vulcanizations can be obtained
Vanadium@Super P composite granule.
Ultrasonic power is 400~600W in the step 1, and is carried out at normal temperature.
The revolving speed of magnetic agitation is 400~600r/min in the step 2, and is carried out at normal temperature.
It is 58~62% that solution B, which pours into the packing ratio of reaction liner, in the step 3.
Alternately cleaning is collected also mainly logical mainly by way of filtering or being centrifuged for water and alcohol in the step 4
The mode for filtering or being centrifuged is crossed to carry out.
The freezing conditions of the step 5 are as follows: -60~-40 DEG C, freeze 2~5h.
The step 5 product is sealed it before being put into pallet and being dried, with preservative film, and to preservative film
It carries out pricking hole processing, to guarantee to its abundant drying under lower pressure.
The sub-micro ball that the composite granule is about 200nm by uniform diameter forms, and core-shell structure is presented in sub-micro ball,
Its center is the Super P that diameter is about 30nm, and shell is by flexible VS4Nanometer rods are entwined, and VS4Nanometer rods have higher
Crystallinity and along (110) crystal plane direction orientations.
Chemical bonds are combined between four vanadic sulfides and Super P, rather than physical bond.
The application of vanadic sulfide@Super P composite granule can be lithium/sodium-ion battery field and be also possible to optical electrical catalysis
Field.
Beneficial effects of the present invention:
(1) present invention is due to directly synthesizing final composite construction using an one-step template-free hydro-thermal reaction, thus has
There is low synthesis temperature, simple synthesis path does not need large scale equipment and harsh reaction condition；
(2) vanadium source used in the present invention is sodium metavanadate, sulphur source is thioacetamide, and solvent is water, these three substances are
Common raw material, cheap and easy to get and at low cost, entire reaction yield is high, easily-controllable and environmental-friendly, and product is not necessarily to post-processing, can be with
It is suitble to large-scale production；
(3) it can be showed when product prepared by the present invention being used as lithium/anode material of lithium-ion battery and optical electrical catalyst
Excellent performance out；
(4) present invention passes through stringent Collaborative Control vanadium source, the concentration and proportion, reaction temperature, reaction time, filling of sulphur source
Than etc. parameters, make full use of vanadium source and sulphur source in the absorption on the surface Super P, make VS4P nanometers of ball surfaces of Super uniformly at
Core, and its growth is relied on, to form VS4Nanometer rods are wrapped in the composite construction on Super P nanosphere in situ；
(5) additive amount of Super P is for uniform VS4The formation that nanometer rods wind Super P nanometers of spherical structure has
Crucial effect.The introducing of excessive and very few Super P, all cannot be VS4Nucleating growth suitable site is provided, thus
Also it just cannot get uniform composite construction；
(6) reaction time is for uniform VS4The formation that nanometer rods wind Super P nanometers of spherical structure has crucial work
With.The too long and too short reaction time is all unfavorable for preferable VS4Nanometer rods wind the building of Super P nanometers of spherical structure；
(7) present invention does not introduce any template or surface-active during synthesizing four vanadic sulfide@Super P
Agent, entire growth in situ process are thus the entire reaction letters using the surface Super P oxygen-containing functional group abundant as active site
It is single, easily-controllable, efficient and inexpensive；
(8)VS4During the growth of Super P nanosphere surface in situ, the surface Super P oxygen-containing functional group abundant
Make VS with the synergistic effect in temperature field caused by hydro-thermal and pressure field4Chemical bonding is formd between Super P；
(9) combination product prepared by the present invention has unique composite construction, wherein being wound in the outer surface Super P
VS4Primarily serve storage Na+Effect, Super P can provide conductive path well not only for charge and discharge process, but also
It can inhibit VS4In the volume change of charge and discharge process.VS4The crystal structure along the arrangement of (110) high preferred orientation is sufficiently exposed,
Since (110) crystal face has maximum interplanar distance, as the channel of metal ion disengaging interchain, it is very beneficial for metal ion
In VS4Interchain stores and transmits.Under the synergistic effect of these structural advantages, four vanadic sulfide@Super P can show excellent
Cycle performance and high rate performance.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram that the embodiment of the present invention 1 prepares product.
Fig. 2 is the low power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product.
Fig. 3 is the high power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product.
Fig. 4 is the transmission electron microscope picture that the embodiment of the present invention 1 prepares product.
Fig. 5 sweeps figure for the transmission electron microscope drawing that the embodiment of the present invention 1 prepares product.
Fig. 6 is the low power high-resolution-ration transmission electric-lens figure that the embodiment of the present invention 1 prepares product.
Fig. 7 is the high power high-resolution-ration transmission electric-lens figure that the embodiment of the present invention 1 prepares product.
Fig. 8 is the scanning electron microscope that the additional amount of the Super P in the embodiment of the present invention 1 is reduced to products therefrom after 20mg
Figure.
Fig. 9 is the scanning electron microscope that the additional amount of the Super P in the embodiment of the present invention 1 is increased to products therefrom after 80mg
Figure.
Figure 10 is the scanning electron microscope (SEM) photograph that the reaction time in the embodiment of the present invention 1 is shortened to products therefrom after 12h.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1:
Step 1: the Super P for weighing 50mg is added in 60ml deionized water, ultrasonic 2h, ultrasonic power be 400~
600W obtains the dark solution A that is uniformly dispersed.
Step 2: 1.0g sodium metavanadate and 3.6g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation
50min revolving speed is 400~600r/min, obtains solution B.
Solution B: being poured into sealing after reacting in liner by step 3, is then placed on liner homogeneously loaded on fixed in outer kettle
It reacts in instrument, packing ratio 59% is reacted for 24 hours at 180 DEG C then under the speed conditions of 10r/min.
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction
Out, product is collected after 3 water and 3 alcohol alternately clean.
Step 5: the product of collection being placed in the cold well of freeze drier and freezed, freezing conditions are as follows: -50 DEG C, cold
Freeze 4h, then the product after freezing be placed in pallet, covers seal closure, is evacuated down to 20Pa, collects product after dry 18h,
Four vanadic sulfide@Super P composite granules can be obtained.
Embodiment 2:
Step 1: the Super P for weighing 48mg is added in 58ml deionized water, ultrasonic 1.5h, ultrasonic power 400W,
Obtain the dark solution A that is uniformly dispersed；
Step 2: 0.9g sodium metavanadate and 3.5g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation
30min revolving speed is 400r/min, obtains solution B；
Solution B: being poured into sealing after reacting in liner by step 3, is then placed on liner homogeneously loaded on fixed in outer kettle
It reacts in instrument, packing ratio 58% reacts 23h at 175 DEG C then under the speed conditions of 5r/min；
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction
Out, product is collected after 2 water and 2 alcohol alternately clean；
Step 5: the product of collection being placed in the cold well of freeze drier and freezed, freezing conditions are as follows: -60 DEG C, cold
Freeze 2h, then the product after freezing be placed in pallet, covers seal closure, is evacuated down to 10Pa, collects product after dry 12h,
Four vanadic sulfide@Super P composite granules can be obtained.
Embodiment 3:
Step 1: the Super P for weighing 52mg is added in 62ml deionized water, ultrasonic 2.5h, ultrasonic power 600W,
Obtain the dark solution A that is uniformly dispersed；
Step 2: 1.1g sodium metavanadate and 3.7g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation
60min revolving speed is 600r/min, obtains solution B；
Solution B: being poured into sealing after reacting in liner by step 3, is then placed on liner homogeneously loaded on fixed in outer kettle
It reacts in instrument, packing ratio 62% reacts 25h at 185 DEG C then under the speed conditions of 10r/min；
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction
Out, product is collected after 5 water and 5 alcohol alternately clean；
Step 5: the product of collection being placed in the cold well of freeze drier and freezed, freezing conditions are as follows: -40 DEG C, cold
Freeze 5h, then the product after freezing be placed in pallet, covers seal closure, is evacuated down to 20Pa, collects product after dry 18h,
Four vanadic sulfide@Super P composite granules can be obtained.
Embodiment 4:
Step 1: the Super P for weighing 50mg is added in 60ml deionized water, ultrasonic power 500W, and ultrasonic 2h is obtained
To the dark solution A that is uniformly dispersed；
Step 2: 1g sodium metavanadate and 3.6g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation
45min revolving speed is 500r/min, obtains solution B；
Solution B: being poured into sealing after reacting in liner by step 3, is then placed on liner homogeneously loaded on fixed in outer kettle
It reacts in instrument, packing ratio 60% is reacted for 24 hours at 180 DEG C then under the speed conditions of 8r/min；
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction
Out, product is collected after 3 water and 3 alcohol alternately clean；
Step 5: the product of collection being placed in the cold well of freeze drier and freezed, freezing conditions are as follows: -50 DEG C, cold
Freeze 3h, then the product after freezing be placed in pallet, covers seal closure, is evacuated down to 15Pa, collects product after dry 15h,
Four vanadic sulfide@Super P composite granules can be obtained.
As shown in Figure 1, all diffraction maximums can be well matched with VS4Standard card PDF#72-1294.Due to
The content of Super P is less and crystallinity is lower, therefore the diffraction maximum of Super P can not be observed in Fig. 1.
As shown in Fig. 2, four vanadic sulfide@Super P are made of uniform sub-micro ball.
As shown in figure 3, the diameter of gained sub-micro ball is about 200nm, and outside is by flexible VS4Nanometer rods are entwined.
As shown in figure 4, core-shell structure is presented in gained sub-micro ball, shell is by flexible VS4Nanometer rods are entwined.
As shown in figure 5, core-shell structure is presented in gained sub-micro ball, center is the Super P that diameter is about 30nm, shell be by
Flexible VS4Nanometer rods are entwined.
As shown in Figure 6.It will be clear that VS from figure4The regular lattice fringe of nanometer rods shows its high crystallization
Degree.
As shown in Figure 7.It will be clear that VS from figure4(110) crystal face lattice fringe of nanometer rods, shows its edge
(110) crystal structure of crystal plane direction orientations.
The additional amount of Super P in the embodiment of the present invention 1 is reduced to the scanning of products therefrom after 20mg as shown in Figure 8
Electron microscope.Many VS that are small, not being combined into nanometer rods as can be observed from Figure4Particle shows VS4Not with Super P
Have and is combined with each other well.
The additional amount of Super P in the embodiment of the present invention 1 is increased to the scanning of products therefrom after 80mg as shown in Figure 9
Electron microscope.Many VS that are small, not being combined into nanometer rods have been similarly observed that from figure4Particle shows VS4With Super P
It is not combined with each other well.
Scanning electron microscope for the reaction time in the embodiment of the present invention 1 to be shortened to products therefrom after 12h as shown in Figure 10
Figure.Many VS that are small, not being combined into nanometer rods as we can see from the figure4Particle shows in a relatively short period of time, VS4With
Super P cannot be combined with each other well.
Claims (10)
1. a kind of preparation method of four vanadic sulfide@Super P composite granules, which is characterized in that include the following steps；
Step 1: the Super P for weighing 48~52mg is added in 58~62ml deionized water, and 1.5~2.5h of ultrasound is divided
Dissipate homogeneous black solution A；
Step 2: 0.9~1.1g sodium metavanadate and 3.5~3.7g thioacetamide are weighed and is added in solution A simultaneously, magnetic force
30~60min of stirring obtains solution B；
Step 3: liner is then placed on homogeneous reaction loaded on fixation in outer kettle by sealing after solution B is poured into reaction liner
In instrument, then under the speed conditions of 5~10r/min, 23~25h is reacted at 175~185 DEG C；
Step 4: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the product cooled down after reaction, warp
Product is collected after crossing 2~5 water and 2~5 alcohol alternating cleanings；
Step 5: the product of collection is placed in the cold well of freeze drier and is freezed, be then placed in the product after freezing
In pallet, seal closure is covered, 10~20Pa is evacuated down to, collects product after dry 12~18h, four vanadic sulfide@can be obtained
Super P composite granule.
2. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
Stating ultrasonic power in step 1 is 400~600W, and is carried out at normal temperature.
3. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
The revolving speed for stating magnetic agitation in step 2 is 400~600r/min, and is carried out at normal temperature.
4. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
Stating solution B in step 3 and pouring into the packing ratio of reaction liner is 58~62%.
5. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
State in step 4 water and alcohol alternately cleaning mainly collected by way of filtering and being perhaps centrifuged also mainly by filtering or
The mode of centrifugation carries out.
6. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
State the freezing conditions of step 5 are as follows: -60~-40 DEG C, freeze 2~5h.
7. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
Step 5 product is stated before being put into pallet and being dried, it is sealed with preservative film, and Zha Kongchu is carried out to preservative film
Reason, to guarantee to its abundant drying under lower pressure.
8. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
The sub-micro ball that the composite granule stated is about 200nm by uniform diameter forms, and core-shell structure is presented in sub-micro ball, and center is straight
The Super P that diameter is about 30nm, shell are by flexible VS4Nanometer rods are entwined, and VS4Nanometer rods crystallinity with higher and
Along the orientations of (110) crystal plane direction.
9. a kind of preparation method of four vanadic sulfides@Super P composite granule according to claim 1, which is characterized in that institute
Chemical bonds are combined between four vanadic sulfides stated and Super P, rather than physical bond.
10. vanadic sulfide@Super P composite granule is applied to lithium/sodium-ion battery field either optical electrical catalytic field.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112786845A (en) * | 2019-11-07 | 2021-05-11 | 广州汽车集团股份有限公司 | VS4Hierarchical pore graphitized carbon composite material, preparation method thereof, positive electrode material, positive plate, lithium-sulfur battery cell and lithium-sulfur battery pack |
| CN115744983A (en) * | 2022-11-15 | 2023-03-07 | 浙江工业大学 | Vanadium-zinc sulfide ion battery positive electrode material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108110246A (en) * | 2017-12-22 | 2018-06-01 | 陕西科技大学 | A kind of extra small VS4/ Super P composite nano-powders and preparation method and application |
| CN108598432A (en) * | 2018-05-02 | 2018-09-28 | 电子科技大学 | A kind of preparation method of four vanadic sulfides/graphene composite material for sodium-ion battery electrode |
| CN109148857A (en) * | 2018-08-28 | 2019-01-04 | 中南大学 | A kind of preparation method of four vanadic sulfides of anode material of lithium-ion battery/carbon nanotube |
| CN109264783A (en) * | 2018-10-10 | 2019-01-25 | 陕西科技大学 | A kind of hollow VS of polycrystal nanobelt self assembled three-dimensional4Microballoon and the preparation method and application thereof |
-
2019
- 2019-02-26 CN CN201910143383.0A patent/CN109904422B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108110246A (en) * | 2017-12-22 | 2018-06-01 | 陕西科技大学 | A kind of extra small VS4/ Super P composite nano-powders and preparation method and application |
| CN108598432A (en) * | 2018-05-02 | 2018-09-28 | 电子科技大学 | A kind of preparation method of four vanadic sulfides/graphene composite material for sodium-ion battery electrode |
| CN109148857A (en) * | 2018-08-28 | 2019-01-04 | 中南大学 | A kind of preparation method of four vanadic sulfides of anode material of lithium-ion battery/carbon nanotube |
| CN109264783A (en) * | 2018-10-10 | 2019-01-25 | 陕西科技大学 | A kind of hollow VS of polycrystal nanobelt self assembled three-dimensional4Microballoon and the preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112786845A (en) * | 2019-11-07 | 2021-05-11 | 广州汽车集团股份有限公司 | VS4Hierarchical pore graphitized carbon composite material, preparation method thereof, positive electrode material, positive plate, lithium-sulfur battery cell and lithium-sulfur battery pack |
| CN115744983A (en) * | 2022-11-15 | 2023-03-07 | 浙江工业大学 | Vanadium-zinc sulfide ion battery positive electrode material and preparation method and application thereof |
| CN115744983B (en) * | 2022-11-15 | 2024-05-03 | 浙江工业大学 | Vanadium zinc sulfide ion battery anode material and preparation method and application thereof |
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