CN109081377A - A kind of three-dimensional molybdenum disulfide bouquet array and its preparation method and application - Google Patents
A kind of three-dimensional molybdenum disulfide bouquet array and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of three-dimensional molybdenum disulfide bouquet arrays and its preparation method and application.The preparation method includes the following steps: S1: molybdenum source and sulphur source are dissolved to obtain mixed solution；The molar ratio of the molybdenum element in element sulphur and molybdenum source in the sulphur source is 3:1 ~ 6:1；S2: titanium wire network is added in mixed solution described in S1, under closed environment at 200 DEG C ~ 220 DEG C hydro-thermal reaction 8 ~ for 24 hours, silk screen is taken out after cooling and is rinsed, three-dimensional molybdenum disulfide bouquet array is dried to obtain.Preparation method simple process provided by the invention can with rapid, high volume synthesize large specific surface area, the three-dimensional molybdenum disulfide bouquet array of stable structure；The three-dimensional molybdenum disulfide bouquet array that the present invention synthesizes is expected to be widely applied in the fields such as lithium ion battery electrode material and elctro-catalyst.
Description
Technical field
The present invention relates to inorganic micro Nano material preparation field, more particularly to a kind of three-dimensional molybdenum disulfide bouquet array and
Preparation method and application.
Background technique
Along with a large amount of uses of economic globalization process and fossil fuel, the problem of environmental pollution and energy shortage increasingly
It is prominent.In order to reduce the pollution of fossil fuel use process, develop wind, light, the sustainable renewable sources of energy of electricity and novel power battery
With high-efficiency energy-storage system, the reasonable disposition and electric adjustment of renewable energy are realized, for improving the level of resources utilization, solving energy
Source crisis and protection environment all have own strategic significance.Lithium ion battery has the high and low self discharge of specific energy, cycle performance
Good, memory-less effect and it is environmentally protective the advantages that, be current high efficient secondary battery most with prospects and change with fastest developing speed
Learn accumulation power supply.Graphite type material good conductivity, crystallinity are high, there is stable charge and discharge platform, be current commercialization degree most
High lithium ion battery negative material.
However, due to cycle efficieny is relatively low, voltage with capacity variation it is big, lack stable discharge platform, hard carbon conduct
Negative electrode material, using being restricted always.The synthesis and photoelectric properties research of nearest stratiform transient metal sulfide micro nano structure
The extensive concern of people is obtained.
Molybdenum disulfide (MoS2) there is the layer structure for being similar to graphite, due to anisotropic design feature, MoS2Easy shape
At the nanometer sheet of two-dimensional structure.Since accumulation or overlapping easily occur when in use for nanometer sheet at random, lead to its available ratio
Surface area substantially reduces.Studies have shown that nanometer sheet is formed three-dimensional hierarchical organization by certain way, not only there is bigger ratio table
Area, the channel of more ion transports, and there is better structural stability.Furthermore uniform nanostructure can be improved
Ion diffusion rates, and then improve its chemical property.The advantage of this structure is each nano structured unit is directly connected to
To collector, the needs usually prepared in electrode to adhesive and conductive additive are eliminated in this way.In addition, this self assembly
Nanostructure provides numerous conductive channels for electron-transport to collector, so as to improve chemical property.
MoS at present2The preparation of nano material mainly prepares the two-dimentional MoS being grown on carbon paper, carbon cloth and titanium metal plate2
Nanometer sheet causes its available specific surface area substantially to subtract since accumulation or overlapping easily occur when in use for nanometer sheet at random
It is small.It is, thus, sought for a kind of simple process, low-cost preparation method prepare large specific surface area, stability is high
MoS23-D nano, structure.
Summary of the invention
It is an object of the invention to overcome specific surface possessed by the two-dimentional molybdenum disulfide nano structure of prior art preparation
The defect that product is small, structural stability is poor provides a kind of preparation method of three-dimensional molybdenum disulfide bouquet array.System provided by the invention
Preparation Method simple process can with rapid, high volume synthesize large specific surface area, the three-dimensional molybdenum disulfide bouquet array of stable structure；This
The three-dimensional molybdenum disulfide bouquet array of invention synthesis is expected to obtain in the fields such as lithium ion battery electrode material and elctro-catalyst wide
General application.
Another object of the present invention is to provide the three-dimensional molybdenum disulfide bouquet arrays that a kind of above method is prepared.
Another object of the present invention is to provide above-mentioned three-dimensional molybdenum disulfide bouquet array electrochemical field application.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of three-dimensional molybdenum disulfide bouquet array, includes the following steps:
S1: molybdenum source and sulphur source are dissolved into obtain mixed solution；The molar ratio of the molybdenum element in element sulphur and molybdenum source in the sulphur source
For 3:1 ~ 6:1；
S2: titanium wire network is added in mixed solution described in S1, under closed environment at 200 DEG C ~ 220 DEG C hydro-thermal reaction 8 ~
For 24 hours, titanium wire network is taken out after cooling and is rinsed, be dried to obtain three-dimensional molybdenum disulfide bouquet array.
The molar ratio of above-mentioned specific element sulphur and the molybdenum element in molybdenum source can ensure that three-dimensional molybdenum disulfide bouquet array
It generates.
Inventors have found that the molybdenum disulfide for reacting generation is flower ball-shaped structure by selecting titanium wire network as substrate.It is other
Metal such as Ni, Cu, Co or Fe etc. can only obtain laminated structure with carbon fibre web etc. because itself can participate in reaction without can be selected
Molybdenum disulfide.And titanium wire network is easy to obtain and will not react with solution as substrate advantage of lower cost, obtained flower
The size of ball, pattern are more uniform, and structure is more stable.
Above-mentioned specific reaction time and reaction temperature can ensure that product is large specific surface area, two sulphur of three-dimensional of stable structure
Change molybdenum bouquet array.
Molybdenum source conventional in the art and sulphur source are used equally in the present invention.
Molybdenum source described in S1 is the one or more of ammonium molybdate, sodium molybdate or potassium molybdate；The sulphur source is thioacetamide
Or one or both of thiocarbamide.
Preferably, molybdenum element concentration is 0.02 ~ 0.05mol/L in mixed solution described in S1.
Above-mentioned specific concentration range can allow the pattern of three-dimensional molybdenum disulfide bouquet array obtained more uniform, and structure is more
Add stabilization.
Preferably, the molar ratio of the molybdenum element in the element sulphur and molybdenum source in sulphur source described in S1 is 4:1 ~ 6:1.
The molar ratio of above-mentioned specific element sulphur and the molybdenum element in molybdenum source can guarantee the abundant reduction and vulcanization of molybdenum, avoid
The impurity such as molybdenum oxide are generated, and the pressure of reaction kettle is unlikely to too high generation danger.
Preferably, hydrothermal temperature described in S2 is 200 DEG C, time 16h.
Above-mentioned specific reaction temperature and time can allow the size of three-dimensional molybdenum disulfide bouquet array obtained more uniform.
Rinse reagent, dry environment are this field conventional selection.
Preferably, the reagent that selection is rinsed described in S2 is deionized water and dehydrated alcohol；The process of the drying are as follows:
It is dried under 60 ~ 80 DEG C of vacuum environment.
A kind of three-dimensional molybdenum disulfide bouquet array, is obtained by above-mentioned preparation method.
The size of the three-dimensional molybdenum disulfide bouquet array obtained by above-mentioned preparation method, pattern are uniform, large specific surface area,
Stable structure.
Above-mentioned three-dimensional molybdenum disulfide bouquet array is also within the scope of the present invention in the application of electrochemical material field.
Preferably, the three-dimensional molybdenum disulfide bouquet array is in elctro-catalyst, lithium ion battery electrode material field
Using.
Compared with prior art, the invention has the following beneficial effects:
Preparation process of the invention is simple, can with rapid, high volume synthesize large specific surface area, the three-dimensional molybdenum disulfide of stable structure
Bouquet array；The three-dimensional molybdenum disulfide bouquet array that the present invention synthesizes is expected in lithium ion battery electrode material and elctro-catalyst etc.
Field is widely applied.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram for the three-dimensional molybdenum disulfide bouquet array that embodiment 1 provides；
Fig. 2 is the scanning electron microscope and transmission electron microscope picture for the three-dimensional molybdenum disulfide bouquet array that embodiment 1 provides；
Fig. 3 is the scanning electron microscope (SEM) photograph for the three-dimensional molybdenum disulfide bouquet array that embodiment 2 provides；
Fig. 4 is the scanning electron microscope (SEM) photograph of the molybdenum disulfide nano sheet for the titanium sheet load that comparative example 1 provides；
Fig. 5 is the scanning electron microscope for the molybdenum disulfide nano sheet that comparative example 2 provides.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of three-dimensional molybdenum disulfide bouquet arrays.It is prepared via a method which to obtain:
The thiocarbamide of the sodium molybdate of 1.5mmol and 9mmol is dissolved in 60mL deionized water under stiring and forms solution, finally by this
Solution is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against into reaction
Kettle liner wall surface, is placed in drying box, hydro-thermal reaction 12 hours at 200 DEG C.Then cooled to room temperature uses titanium wire network
Deionized water and dehydrated alcohol rinse three times respectively, and are dried in vacuo 12 hours in 60 DEG C and obtain three-dimensional molybdenum disulfide bouquet battle array
Column.
The X-ray diffractogram of three-dimensional molybdenum disulfide bouquet array is shown in Fig. 1, each diffraction maximum position of molybdenum disulfide and intensity in figure
It is consistent with standard diffraction card (JCPDS37-1492).
The scanning electron microscope of three-dimensional molybdenum disulfide bouquet array is shown in that Fig. 2, Fig. 2 (a) show that the close-up view of titanium wire network, Fig. 2 (b) are
Single titanium silk figure, it can be seen that one layer of sample is deposited on titanium silk；Fig. 2 (c) is it can be seen that the sample deposited on titanium silk is size
With the relatively uniform nano flower ball array of pattern, average diameter is about 800nm.Fig. 2 (d) shows that bouquet is by many nanometer sheet groups
It fills, surface texture is dispersed with many nanometer sheets being staggered.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 107mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher
Catalytic performance.
Embodiment 2
The present embodiment provides a kind of three-dimensional molybdenum disulfide bouquet arrays.It is prepared via a method which to obtain:
The thiocarbamide of the sodium molybdate of 2mmol and 9mmol is dissolved in 60mL deionized water under stiring and forms solution, it is finally that this is molten
Liquid is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against into reaction kettle
Liner wall surface, is placed in drying box, hydro-thermal reaction 16 hours at 200 DEG C.Then cooled to room temperature spends titanium wire network
Ionized water and dehydrated alcohol rinse three times respectively, and are dried in vacuo 12 hours in 60 DEG C and obtain three-dimensional molybdenum disulfide bouquet array.
The scanning electron microscope of three-dimensional molybdenum disulfide bouquet array is shown in that Fig. 3, Fig. 3 (a) show that the close-up view of titanium wire network, Fig. 3 (b) are
Single titanium silk figure, it can be seen that more layers sample is deposited on titanium silk；Fig. 3 (c) is it can be seen that the sample deposited on titanium silk is ruler
The very little and relatively uniform nano flower ball array of pattern, average diameter is about 1.4 μm.Fig. 2 (d) shows that bouquet is by many nanometer sheets
Assemble, surface texture is dispersed with many nanometer sheets being staggered.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 159mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher
Catalytic performance.
Embodiment 3
The present embodiment provides a kind of three-dimensional molybdenum disulfide bouquet arrays.It is prepared via a method which to obtain:
The thiocarbamide of the sodium molybdate of 1.5mmol and 9mmol is dissolved in 60mL deionized water under stiring and forms solution, finally by this
Solution is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against into reaction
Kettle liner wall surface, is placed in drying box, hydro-thermal reaction 20 hours at 220 DEG C.Then cooled to room temperature uses titanium wire network
Deionized water and dehydrated alcohol rinse three times respectively, and are dried in vacuo 12 hours in 60 DEG C and obtain three-dimensional molybdenum disulfide bouquet battle array
Column.
The size and shape of gained three-dimensional molybdenum disulfide bouquet array is quite uniform, and average diameter is about 2.3 μm.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 109mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher
Catalytic performance.
Embodiment 4
The present embodiment provides a kind of three-dimensional molybdenum disulfide bouquet arrays.In preparation method, except the molybdenum that molybdenum source is changed into 1.5mmol
Sour ammonium, sulphur source change the thioacetamide of 4.5mmol into, and deionized water additional amount is 75ml；Hydrothermal temperature is 220 DEG C, and the time is
8h, drying temperature are 70 DEG C outer, remaining operation and condition are consistent with embodiment 1.
The size and shape for the three-dimensional molybdenum disulfide bouquet array that the present embodiment is prepared is close with embodiment 1.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 82mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher are urged
Change performance.
Embodiment 5
The present embodiment provides a kind of molybdenum disulfide bouquets.In preparation method, except the ammonium molybdate that molybdenum source is changed into 0.214mmol,
Sulphur source changes the thioacetamide of 6mmol into, and deionized water additional amount is 30ml；Drying temperature is 80 DEG C outer, remaining operation and item
Part is consistent with embodiment 1.
The size and shape for the three-dimensional molybdenum disulfide bouquet array that the present embodiment is prepared is close with embodiment 1.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 116mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher
Catalytic performance.
Embodiment 6
The present embodiment provides a kind of molybdenum disulfide bouquets.In preparation method, except molybdenum source is changed into potassium molybdate, sulphur source is changed into
The thioacetamide of 9mmol, the hydro-thermal time, remaining operation and condition were consistent with embodiment 1 to be outer for 24 hours.
The size and shape for the three-dimensional molybdenum disulfide bouquet array that the present embodiment is prepared is close with embodiment 1.
The test of electrocatalytic hydrogen evolution reactivity worth: the molybdenum disulfide bouquet array titanium wire network after hydro-thermal reaction, which is washed into diameter, is
The disk of 7.5mm is as test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode,
Platinized platinum is used as to electrode, is urged on CHI760E electrochemical workstation with electricity of the linear sweep voltametry test material to evolving hydrogen reaction
Change performance, scanning speed 5mV/s.
Test result is shown, under -0.30Vvs.RHE (standard hydrogen electrode) current potential, on molybdenum disulfide bouquet array electrode
Electrochemical catalysis evolving hydrogen reaction current density is 131mA/cm2(in terms of actual loading area), evolving hydrogen reaction electricity with higher
Catalytic performance.
Comparative example 1
The present embodiment provides a kind of molybdenum disulfide nano sheets of titanium sheet load.In preparation method, except changing titanium wire network into titanium sheet,
Remaining operation and condition are consistent with embodiment 1.
The present embodiment molybdenum disulfide nano sheet obtained for titanium sheet load is not as shown in figure 4, generate stable three-dimensional
Molybdenum disulfide bouquet array.
Comparative example 2
The present embodiment provides a kind of molybdenum disulfide nano sheets.In preparation method, except titanium wire network is added without, remaining is operated and condition
It is consistent with embodiment 1.
The present embodiment obtained is molybdenum disulfide nano sheet at random as shown in figure 5, not generating stable two sulphur of three-dimensional
Change molybdenum bouquet array.
Those of ordinary skill in the art will understand that embodiment here be to help reader understand it is of the invention
Principle, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.This field it is common
Technical staff disclosed the technical disclosures can make the various various other tools for not departing from essence of the invention according to the present invention
Body variations and combinations, these variations and combinations are still within the scope of the present invention.
Claims (9)
1. a kind of preparation method of three-dimensional molybdenum disulfide bouquet array, which comprises the steps of:
S1: molybdenum source and sulphur source are dissolved into obtain mixed solution；The molar ratio of the molybdenum element in element sulphur and molybdenum source in the sulphur source
For 3:1 ~ 6:1；
S2: titanium wire network is added in mixed solution described in S1, under closed environment at 200 DEG C ~ 220 DEG C hydro-thermal reaction 8 ~
For 24 hours, titanium wire network is taken out after cooling and is rinsed, be dried to obtain three-dimensional molybdenum disulfide bouquet array.
2. the preparation method of three-dimensional molybdenum disulfide bouquet array according to claim 1, which is characterized in that molybdenum source described in S1
For the one or more of ammonium molybdate, sodium molybdate or potassium molybdate；The sulphur source is one or both of thioacetamide or thiocarbamide.
3. the preparation method of three-dimensional molybdenum disulfide bouquet array according to claim 1, which is characterized in that mixed described in S1
Molybdenum in Solution concentration of element is 0.02 ~ 0.05mol/L.
4. the preparation method of three-dimensional molybdenum disulfide bouquet array according to claim 1, which is characterized in that sulphur source described in S1
In element sulphur and molybdenum source in molybdenum element molar ratio be 4:1 ~ 6:1.
5. the preparation method of three-dimensional molybdenum disulfide bouquet array according to claim 1, which is characterized in that hydro-thermal described in S2
Reaction temperature is 200 DEG C, time 16h.
6. the preparation method of three-dimensional molybdenum disulfide bouquet array according to claim 1, which is characterized in that rinsed described in S2
The reagent of selection is deionized water and dehydrated alcohol；The process of the drying are as follows: done under 60 ~ 80 DEG C of vacuum environment
It is dry.
7. a kind of three-dimensional molybdenum disulfide bouquet array, which is characterized in that obtained by any preparation method of claim 1 ~ 6
It arrives.
8. application of the three-dimensional molybdenum disulfide bouquet array in electrochemical material field described in claim 7.
9. applying according to claim 8, which is characterized in that the three-dimensional molybdenum disulfide bouquet array is in elctro-catalyst, lithium
Application in ion battery electrode materials field.
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