CN109888223A - A kind of preparation method and application of four vanadic sulfides@redox graphene composite granule - Google Patents
A kind of preparation method and application of four vanadic sulfides@redox graphene composite granule Download PDFInfo
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Abstract
A kind of preparation method of four vanadic sulfides@redox graphene composite granule weighs 20~120mg graphene oxide and is added to ultrasound in 58~62ml deionized water, obtains finely dispersed dark solution A；It weighs 0.9~1.1g sodium metavanadate and 3.5~3.7g thioacetamide and is added in solution A simultaneously, magnetic agitation obtains solution B；Liner is then placed in homogeneous reaction instrument loaded on fixation in outer kettle, then reacts under speed conditions by sealing after solution B is poured into reaction liner；Hydro-thermal reaction terminates to naturally cool to reaction kettle into room temperature, then takes out the product cooled down after reaction, collects product after water and 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, covered seal closure, collect product after vacuum drying, four vanadic sulfide@redox graphene composite granules can be obtained.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@redox graphene composite granule technical fields, in particular to one kind four vulcanizes
The preparation method and application of vanadium@redox graphene 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, the purpose of the present invention is to provide a kind of four vanadic sulfide@reduction-oxidations
The preparation method and application of graphene composite powder, the present invention are distinguished using water as solvent with sodium metavanadate and thioacetamide
For vanadium source and sulphur source, and graphene oxide carbon source is introduced, passes through their concentration of Collaborative Control and proportion, reaction temperature, reaction
The parameters such as time, packing ratio realize an one-step template-free agent hydro-thermal method and grow in redox graphene surface in situ bonding type
VS4Be bent nanometer rods structure, this method reaction process is simple, temperature is low, it is easily-controllable and do not need large scale equipment and harshness it is anti-
Condition is answered, VS can be directly realized by a reaction process4Formation and growth in situ on redox graphene surface.
When applying above-mentioned product for lithium/anode material of lithium-ion battery and optical electrical catalyst, it can show excellent electrification
Learn performance and catalytic performance.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of preparation method of four vanadic sulfides@redox graphene composite granule, includes the following steps；
Step 1: weighing 20~120mg graphene oxide and be added in 58~62ml deionized water, 1.5~2.5h of ultrasound,
Obtain finely dispersed dark solution A；
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, 12~30h 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 4~10 water and 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@redox graphene 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 composite granule is made of irregular piece, and the inside of piece is the oxygen reduction of few layer (ultra-thin, 5~15nm)
Graphite alkene, the surface of piece be by uniform, diameter be 20~50nm, length be 50~150nm bending nanometer rods form, and
VS4It is bent nanometer rods crystallinity with higher and the orientations along (110) crystal plane direction.
Chemical bonds are combined between four vanadic sulfides and redox graphene, rather than physical bond.
The application of four vanadic sulfide@redox graphene composite granules can be lithium/sodium-ion battery field and be also possible to
Optical electrical catalytic field, and excellent performance can be shown in the two fields.
Beneficial effects of the present invention:
(1) present invention is entire former due to directly synthesizing final composite construction using an one-step template-free hydro-thermal reaction
Position growth course is using the oxygen-containing functional group of surface of graphene oxide as active site.Thus there is low synthesis temperature, simply
Synthesis path, the advantage of reaction condition that is easily-controllable, efficient, inexpensive, not needing large scale equipment and harshness；
(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, it is cheap and easy to get, at low cost, and entire reaction yield is high, easily-controllable and environmental-friendly, product is not necessarily to post-processing, can
To be 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, can sufficiently be rolled into a ball by surface of graphene oxide oxygen-containing hat abundant, make VS4Surface of graphene oxide uniformly at
Core, and its growth is relied on, simultaneous oxidation graphene is reduced to redox graphene under hydrothermal conditions and becomes very thin,
To form VS4Bending nanometer rods are laid in the composite construction on redox graphene surface in situ；
(5) additive amount of graphene oxide is for VS4It is evenly laid out in redox graphene surface knot to be bent nanometer rods
The acquisition of structure has the function of key.Excessive graphene oxide introduces, and can make the VS for being grown on surface of graphene oxide4Bending
Nanometer rods become very sparse or even partial oxidation of graphite alkene surface is not distributed VS4It is bent nanometer rods.Very few graphite oxide
Alkene introduces, and can make the VS for being grown on surface of graphene oxide4Nanometer rods become very dense or even part VS4It is bent nanometer rods not
Surface of graphene oxide can be grown on；
(6) reaction time is to VS4Be bent nanometer rods it is evenly laid out in redox graphene surface texture also
Crucial effect, too short reaction time be easy to occur VS in the reaction product2Nanometer sheet miscellaneous phase；
(7)VS4Redox graphene surface in situ growth during, redox graphene surface functional group and
The synergistic effect in temperature field and pressure field caused by hydro-thermal makes to form chemistry between four vanadic sulfides and redox graphene
Bonding；
(8) product prepared by the present invention has unique composite construction, wherein VS4Reduction is carried in a manner of tiling
Surface of graphene oxide and the crystal structure for sufficiently exposing edge (110) high preferred orientation arrangement, since (110) crystal face has maximum
Interplanar distance, as metal ion disengaging interchain channel, be very beneficial for metal ion in VS4Interchain storage and transmission.
Redox graphene can provide good conductive network not only for charge and discharge process, but also can be VS4In charge and discharge
The volume change of process provides cushion space.VS4Chemical bonding effect between redox graphene, not only can be into one
Rock-steady structure is walked, may also speed up the transmission of charge between them.Under the synergistic effect of above structure advantage, four vulcanizations
Vanadium@redox graphene electrode 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 thickness direction.
Fig. 4 is the super-high power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product in-plane.
Fig. 5 is the high power transmission electron microscope picture that the embodiment of the present invention 1 prepares product.
Fig. 6 is the high-resolution-ration transmission electric-lens figure that the embodiment of the present invention 1 prepares product.
Fig. 7 sweeps figure for the face TEM-EDS that the embodiment of the present invention 1 prepares product.
Fig. 8 is the scanning that the additional amount of the graphene oxide in the embodiment of the present invention 1 is reduced to products therefrom after 20mg
Electron microscope.
Fig. 9 is the scanning that the additional amount of the graphene oxide in the embodiment of the present invention 1 is increased to products therefrom after 120mg
Electron microscope.
Figure 10 is the surface sweeping electron microscope that the reaction time in the embodiment of the present invention 1 is shortened to products therefrom after 6h.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1:
Step 1: weighing 50mg graphene oxide and be added in 60ml deionized water, ultrasonic 2.0h, ultrasonic power 400
~600W obtains finely dispersed dark solution A.
Step 2: 1.0g sodium metavanadate and 3.6g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation
30min 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 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 6 water and 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@redox graphene composite granules can be obtained.
Embodiment 2:
Step 1: weighing 20mg graphene oxide and be added in 58ml deionized water, ultrasonic 1.5h, and ultrasonic power is
400W obtains finely dispersed dark solution A；
Step 2: 0.9g sodium metavanadate and 3.5g thioacetamide are weighed and is added in solution A simultaneously, magnetic agitation 30
~60min 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 12h 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 4 water and 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@redox graphene composite granules can be obtained.
Embodiment 3:
Step 1: weighing 120mg graphene oxide and be added in 62ml deionized water, ultrasonic 2.5h, and ultrasonic power is
600W obtains finely dispersed dark solution A；
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 30h 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 10 water and 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@redox graphene composite granules can be obtained.
Embodiment 4:
Step 1: weighing 70mg graphene oxide and be added in 60ml deionized water, ultrasonic 2h, ultrasonic power 500W,
Obtain finely dispersed dark solution A；
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, then packing ratio 60% exists, under the speed conditions of 7r/min, react 20h at 180 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 7 water and 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@redox graphene composite granules can be obtained.
As shown in Figure 1, all diffraction maximums can be well matched with VS substantially4Standard card PDF#72-1294.By
In the content of reduction-oxidation alkene, less and crystallinity is lower, therefore spreading out for redox graphene can not be observed in Fig. 1
Penetrate peak.
As shown in Fig. 2, what composite granule was made of irregular nanometer sheet, the inside of piece is redox graphene, table
Face is VS4It is bent nanometer rods.
As shown in figure 3, nanometer sheet inside redox graphene with a thickness of 5~15nm.
As shown in figure 4, VS4Bending nanometer rods are uniformly distributed in the surface of redox graphene in a manner of tiling, and
VS4The diameter for being bent nanometer rods is 20~50nm, and length is 50~150nm.
As shown in figure 5, VS4Bending nanometer rods are uniformly distributed in redox graphene surface in a manner of tiling, and also
Former graphene oxide has ultra-thin structure.
As shown in Figure 6.It will be clear that regular VS from figure4(110) crystal face lattice fringe, which is distributed in, entirely receives
On rice stick, VS is shown4Nanometer rods crystallinity with higher and edge (110) high preferred orientation arrangement.
As shown in Figure 7.From figure, we can see that tri- kinds of elements of C, V and S are uniformly distributed in sample area, further
Confirm VS4Bending nanometer rods are uniformly distributed in the composite construction on redox graphene surface in a manner of tiling.
As shown in Figure 8.More dense VS as can be observed from Figure4Flexible nano stick has loaded to redox graphene
Surface.
As shown in Figure 9.It is carried on the VS on redox graphene surface as can be observed from Figure4Bending nanometer rods become
Less.
As shown in Figure 10.It can be seen from the figure that occurring VS in the product2The miscellaneous phase of nanometer sheet.
Claims (10)
1. a kind of preparation method of four vanadic sulfide@redox graphene composite granules, which is characterized in that include the following steps；
Step 1: weighing 20~120mg graphene oxide and be added in 58~62ml deionized water, and 1.5~2.5h of ultrasound is obtained
Finely dispersed dark 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, 12~30h 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 4~10 water and alcohol alternating cleaning；
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 also
Former graphene oxide composite granule.
2. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, ultrasonic power is 400~600W in the step 1, and is carried out at normal temperature.
3. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, the revolving speed of magnetic agitation is 400~600r/min in the step 2, and is carried out at normal temperature.
4. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, it is 58~62% that solution B, which pours into the packing ratio of reaction liner, in the step 3.
5. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, alternately cleaning is collected and also mainly passed through mainly by way of filtering or being centrifuged for water and alcohol in the step 4
It filters or the mode of centrifugation carries out.
6. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, the freezing conditions of the step 5 are as follows: -60~-40 DEG C, freeze 2~5h.
7. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, the step 5 product is sealed it before being put into pallet and being dried, with preservative film, and carries out to preservative film
Hole processing is pricked, to guarantee to its abundant drying under lower pressure.
8. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, the composite granule is made of irregular piece, and the inside of piece is the reduction-oxidation of few layer (ultra-thin, 5~15nm)
Graphene, the surface of piece be by uniform, diameter be 20~50nm, length be 50~150nm bending nanometer rods form, and
VS4It is bent nanometer rods crystallinity with higher and the orientations along (110) crystal plane direction.
9. a kind of preparation method of four vanadic sulfides@redox graphene composite granule according to claim 1, feature
It is, is combined into chemical bonds between four vanadic sulfides and redox graphene, rather than physical bond.
10. four vanadic sulfide@redox graphene composite granules are applied to the either optical electrical catalysis of lithium/sodium-ion battery field
Field.
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| CN111874950A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
| CN113247949A (en) * | 2021-04-30 | 2021-08-13 | 哈尔滨理工大学 | Preparation and application of three-dimensional rosette vanadium sulfide nanosheet sphere-reduced graphene oxide composite material |
| CN114162874A (en) * | 2021-12-09 | 2022-03-11 | 中国科学技术大学 | Preparation method of composite metal sulfide loaded mixed carbon material serving as sulfur main body material of lithium-sulfur battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110247050A (en) * | 2019-06-21 | 2019-09-17 | 东北大学 | A method of four vanadic sulfides/graphene composite material is prepared using containing vanadium leachate |
| CN111354931A (en) * | 2020-03-09 | 2020-06-30 | 天津师范大学 | Lithium-sulfur battery positive electrode composite material with high active substance content and preparation method and application thereof |
| CN111874950A (en) * | 2020-07-31 | 2020-11-03 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN111874950B (en) * | 2020-07-31 | 2022-07-29 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
| CN113247949A (en) * | 2021-04-30 | 2021-08-13 | 哈尔滨理工大学 | Preparation and application of three-dimensional rosette vanadium sulfide nanosheet sphere-reduced graphene oxide composite material |
| CN114162874A (en) * | 2021-12-09 | 2022-03-11 | 中国科学技术大学 | Preparation method of composite metal sulfide loaded mixed carbon material serving as sulfur main body material of lithium-sulfur battery |
| CN114162874B (en) * | 2021-12-09 | 2023-03-10 | 中国科学技术大学 | Preparation method of composite metal sulfide loaded mixed carbon material serving as sulfur main body material of lithium-sulfur battery |
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