CN111533186B - Preparation method and application of spherical expanded molybdenum disulfide - Google Patents
Preparation method and application of spherical expanded molybdenum disulfide Download PDFInfo
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Abstract
A preparation method and application of spherical expanded molybdenum disulfide belong to the technical field of zinc ion battery anode materials, and aim at the problem that the hydration radius of zinc ions is large and the distance between molybdenum disulfide layers is relatively small, the method comprises the following steps: mixing a molybdenum source and a sulfur source in a certain proportion with the stirred PVP solution, and reacting in a reaction kettle at 180 ℃ for 24 hours; and centrifugally drying the obtained product, placing the product in a high-temperature tubular furnace, and reacting for 2 hours at the temperature of 400-450 ℃ to obtain a final product. Taking the product as an active substance, and mixing the active substance with a conductive agent and a binder in a ratio of 7:2:1, uniformly mixing, coating the mixture on a cut carbon paper wafer, and drying to obtain the zinc ion battery positive plate. Compared with molybdenum disulfide, the material prepared by the invention has larger interlayer spacing for Zn 2+ Insertion/removal; meanwhile, due to the existence of amorphous carbon caused by carbonization, the conductivity of the material is improved, the volume change of the material structure in the charge and discharge process is relieved, and the cycle stability is improved.
Description
Technical Field
The invention belongs to the technical field of zinc ion battery anode materials, and particularly relates to a preparation method and application of spherical expanded molybdenum disulfide.
Background
At present, the lithium ion battery is the most widely used secondary battery and has the advantages of high discharge platform, long cycle life, high energy density and the like. However, its limitations are also evident: the low lithium content results in high production cost of the lithium ion battery; the potential safety hazard associated with organic electrolytes is not inconstant. Among the many candidates for lithium ion batteries, zinc ion batteries are one of the most promising energy storage devices. The high storage capacity of zinc can provide the possibility for low-cost production of zinc-ion batteries; the aqueous electrolyte greatly improves the safety performance of the battery; at the same time, divalent ions can provide high capacity storage. In a word, the zinc ion battery has the characteristics of large-current charging and discharging, high energy density, high power density and the like, and is expected to be applied to large and medium-sized energy storage application, such as power batteries of next-generation electric vehicles, load balancing of intermittent power sources of new energy power grids and the like.
Molybdenum disulfide (MoS) 2 ) Has a layered structure similar to graphene, and the layered structure can be Zn 2+ Provides a channel for insertion/extraction of host material. However, the insertion of zinc ions into the molybdenum disulfide layers is greatly hindered due to the large hydrated radius of zinc ions (about 0.404 to 0.43 nm); meanwhile, the conductivity of the molybdenum disulfide is poor, which is another main factor of low electrochemical activity of pure molybdenum disulfide, so that the original molybdenum disulfide is modified to be beneficial to Zn 2+ The new material of insertion/removal is a significant task.
Disclosure of Invention
The invention provides a preparation method of spherical expanded molybdenum disulfide and application thereof, aiming at the problems that the hydration radius of zinc ions is larger and the interlayer spacing of molybdenum disulfide is relatively smaller 2+ The resistance to intercalation. Meanwhile, for the problem of poor conductivity of molybdenum disulfide, PVP is used as an intercalating agent and also used as a carbon source, and the spherical nano material is obtained through further sintering, so that the conductivity is increased.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of spherical expanded-layer molybdenum disulfide comprises the following steps:
the method comprises the following steps: heating PVP in a water bath, and continuously stirring to obtain a colloidal solution with the mass concentration of 5%;
step two: pouring the mixed solution of the molybdenum source and the sulfur source into the PVP solution in the step one, wherein the mixing volume ratio of the mixed solution to the PVP solution is 1:4, stirring for 2-3 h;
step three: dropwise adding 1mol/L HCl into the mixed solution obtained in the second step, and adjusting the pH value to 4-5;
step four: adding the mixed solution obtained in the fourth step into the inner liner of the reaction kettle, placing the inner liner in a blast drying oven, and drying for 24 hours at 180 ℃ to obtain PVP intercalated molybdenum disulfide;
step five: and putting the PVP intercalated molybdenum disulfide into a corundum porcelain boat, and sintering in a high-temperature tube furnace to obtain the spherical expanded layer molybdenum disulfide.
Compared with the prior art, the invention has the beneficial effects that:
(1) In the invention, the layer expanding effect on the molybdenum disulfide is obvious, and the interlayer spacing is increased from about 0.62nm of the bulk material to more than 0.95 nm.
(2) PVP has a dual role: an intercalating agent and a carbon source. The conductivity of the molybdenum disulfide is effectively enhanced while the interlayer distance is enlarged.
(3) The amorphous carbon obtained by carbonization can play a role in buffering the volume expansion of the material in the charge-discharge process, and the structural stability of the material is enhanced, so that the cycle performance is improved.
(4) Particle size can be adjusted by adjusting the amount of PVP used.
(5) Material prepared by the invention and common MoS 2 In contrast, it has a larger interlayer spacing for Zn 2+ Insertion/removal; meanwhile, due to the existence of amorphous carbon caused by carbonization, the conductivity of the material is improved, the volume change of the material structure in the charge and discharge process is relieved, and the cycle stability is improved.
Drawings
FIG. 1 shows MoS in comparative example 1 2 And E-MoS in example 1 2 XRD spectrum of the/C sample;
FIG. 2 is a MoS of 2 μm in comparative example 1 2 Scanning an electron microscope picture;
FIG. 3 is a MoS of 500 nm in comparative example 1 2 Scanning electron microscope photos;
FIG. 4 is the 3 micron E-MoS of example 1 2 A scanning electron micrograph of/C;
FIG. 5 is a 1 μm E-MoS of example 1 2 A scanning electron micrograph of/C;
FIG. 6 shows MoS in comparative example 1 2 And E-MoS in example 1 2 AC impedance comparison graph of zinc ion battery when/C is used as anode material;
FIG. 7 shows MoS in comparative example 1 2 100 cycles of the zinc ion battery when used as the anode material;
FIG. 8 shows the results of E-MoS in example 1 2 200 cycles of the zinc ion battery with/C as the anode material.
Detailed Description
The technical solution of the present invention is further described below with reference to the drawings and examples, but not limited thereto, and other embodiments obtained by modifying or substituting the technical solution of the present invention without inventive achievement are within the scope of the present invention.
The first embodiment is as follows: the embodiment describes a method for preparing spherical expanded molybdenum disulfide, which comprises the following steps:
the method comprises the following steps: heating PVP in a water bath, and continuously stirring to obtain a colloidal solution with the mass concentration of 5%;
step two: pouring a mixed solution of a molybdenum source and a sulfur source into the PVP solution in the first step, wherein the mixing volume ratio of the mixed solution to the PVP solution is 1:4, stirring for 2-3 h; use of PVP as an intercalating agent that increases viscosity during hydrothermal processing, thereby inhibiting MoS 2 And to some extent prevent agglomeration.
Step three: dropwise adding 1mol/L HCl into the mixed solution obtained in the second step, and adjusting the pH value to 4-5;
step four: adding the mixed solution obtained in the fourth step into the inner liner of the reaction kettle, placing the inner liner in a blast drying oven, and drying for 24 hours at 180 ℃ to obtain PVP intercalated molybdenum disulfide (E-MoS) with expanded interlayer spacing 2 -PVP)；
Step five: putting the PVP intercalated molybdenum disulfide with enlarged interlayer spacing into a corundum porcelain boat, and sintering in a high-temperature tube furnace to obtain spherical molybdenum disulfide (E-MoS) with enlarged interlayer spacing 2 /C)。
The second embodiment is as follows: in the first step of the preparation method of spherical expanded molybdenum disulfide according to the first embodiment, in order to facilitate the dissolution of PVP, the temperature of the water bath is 80 to 90 ℃, and the time is 2 to 3 hours in order to make the PVP solution more uniform.
The third concrete implementation mode: in the second step of the preparation method of spherical expanded molybdenum disulfide according to the first embodiment, in the mixed solution of the molybdenum source and the sulfur source, the ratio of the molybdenum source to the sulfur source to the deionized water is 1mmol:30mmol:10mL.
The fourth concrete implementation mode is as follows: in the second step of the method for preparing molybdenum disulfide for spherical diffusion layer according to the first or third embodiment, the molybdenum source is ammonium molybdate tetrahydrate ((NH) 4 ) 6 Mo 7 O 24 ·4H 2 O) or sodium molybdate (Na) 2 MoO 4 ) (ii) a The sulfur source is thiourea. The two molybdenum sources react with thiourea to generate stable molybdenum disulfide, and residual NH in the molybdenum sources in the reaction process 4 + And Na + Or can be inserted between the molybdenum disulfide layers to play a certain layer expanding effect.
The fifth concrete implementation mode: in the fourth step, the obtained molybdenum disulfide is repeatedly centrifuged and washed, and dried at 60 ℃ to obtain black powder. The method can thoroughly wash out the residual PVP.
The sixth specific implementation mode: in the fifth step, the sintering temperature is 400-450 ℃ and the time is 2 hours.
The seventh embodiment: in the fifth step of the method for preparing spherical expanded-layer molybdenum disulfide according to the first or sixth specific embodiment, the temperature rise rate of the tube furnace is 5 ℃/min.
The specific implementation mode eight: an application of the layer-expanded molybdenum disulfide prepared by the method in any one of the first to seventh embodiments in a zinc ion battery positive electrode material.
The specific implementation method nine: the application of the expanded molybdenum disulfide in the positive electrode material of the zinc ion battery in the embodiment eight is that the expanded molybdenum disulfide is used as an active substance of the positive electrode material of the zinc ion battery, and the active substance, the conductive agent and the binder are mixed according to the weight ratio of 7:2:1, coating the mixture on a carbon paper current collector, drying to obtain a zinc ion battery positive plate, and assembling the water system zinc ion battery.
Example 1:
1. 2g PVP was weighed into a beaker containing 40mL deionized water, heated to 80 ℃ in a water bath, maintained for 3h and stirred continuously.
2. Weighing a mixture with a molar ratio of 1:30mmol ammonium molybdate tetrahydrate (0.325 g) and thiourea (0.6 g) were stirred in 10mL deionized water until fully dissolved, and the mixed solution was mixed with the above PVP solution at a ratio of 1:4, and stirring for 2 hours.
3. Adding 1mol/L HCl into the solution drop by drop, and adjusting the pH value to 4-5.
4. Transferring the mixed solution into the inner liner of a high-pressure kettle, placing the inner liner in a forced air drying oven, adjusting the reaction temperature to 180 ℃, and reacting for 24 hours; centrifugally washing the black product, drying in a drying oven at 60 ℃ overnight, and grinding to obtain PVP intercalated molybdenum disulfide (E-MoS) with enlarged interlayer spacing 2 -PVP)。
5. Mixing the above E-MoS 2 Putting a PVP sample into a corundum porcelain boat, sintering in a high-temperature tubular resistance furnace, setting the sintering temperature to be 400 ℃, maintaining for 2 hours, and raising the temperature at 5 ℃/min; taking out the sample after the temperature is reduced to room temperature, repeatedly centrifuging and washing, drying, and grinding to obtain the carbon-doped extended-layer molybdenum disulfide (E-MoS) 2 C) sample.
6. Taking the sample as an active substance, and taking the active substance: conductive agent: binder =7:2:1, coating the paste on a carbon paper current collector, drying the paste to obtain a zinc ion battery positive plate, and assembling the water-based zinc ion battery.
Comparative example 1:
1. weighing a mixture with a molar ratio of 1:30mmol ammonium molybdate tetrahydrate (0.325 g) and thiourea (0.6 g) were placed in a beaker with 50mL deionized water and magnetically stirred until completely dissolved.
2. 1mol/L HCl is added into the solution drop by drop, and the PH value is adjusted to 4-5.
3. The solution is poured into a 100mL reaction kettle lining and placed in a forced air drying oven, the reaction temperature is set to be 180 ℃, and the reaction time is 24 hours. Centrifuging and washing the black product, drying the black product in a drying box at 60 ℃ overnight, and grinding the dried product to obtain MoS 2 And (4) sampling.
4. Using the black powder obtained above as an active material, adding: conductive agent: binder =7:2:1, coating the paste on a carbon paper current collector, drying the paste to obtain a zinc ion battery positive plate, and assembling the water-based zinc ion battery.
The materials of comparative example 1 and example 1 described above were subjected to XRD spectrum analysis and SEM test, and the assembled batteries were subjected to electrochemical performance test. As can be seen from FIG. 1, the MoS obtained 2 The peak position of the (002) crystal face of the sample is slightly shifted to the left, which shows that the interlayer spacing is not basically expanded; and E-MoS prepared by adding PVP 2 The (002) crystal face peak of the/C is obviously shifted to the left, which shows that the layer expanding effect is obvious. Calculated by the Bragg equation, the E-MoS 2 The interlayer spacing for/C is enlarged to 0.96nm, a significant improvement over bulk material (about 0.62 nm). In comparison, FIGS. 2 to 5 show that: moS 2 And E-MoS 2 the/C is a spherical structure formed by stacking nano sheets, and the large specific surface area of the small spheres can provide abundant active sites and ion diffusion paths. Compared with E-MoS 2 /C，MoS 2 More nanosheets stacked, resulting in a larger size; and E-MoS stacked from fewer nanosheets 2 The size of the/C pellets is much smaller; smaller dimensions can provide shorter diffusion paths, thereby greatly increasing mass transfer rates. From the ac impedance spectrum of fig. 6, it is known that: E-MoS 2 C as positive electrode materialMoS for the impedance ratio of aqueous zinc ion battery 2 Much smaller when used as a positive electrode, probably due to Zn resulting from the enlarged interlayer spacing 2+ The resistance of intercalation becomes smaller and carbonization improves the effect brought by conductivity. As can be seen from FIG. 7, the MoS was not subjected to the layer expansion and carbonization treatment 2 The capacity was low and decayed rapidly from about 50mAh/g in the first turn to about 20mAh/g and finally stabilized at about 15 mAh/g. As shown in FIG. 8, the E-MoS after the layer expansion treatment and the carbonization modification 2 Discharge capacity per C is higher than that of MoS 2 The method has the advantages that: the first discharge specific capacity is about 130mAh/g, a relatively stable state is maintained in the first 40 circles after the first discharge specific capacity is slightly reduced, the specific capacity begins to be slowly reduced after 40 circles, and finally the capacity of about 70mAh/g is maintained in 200 circles. Compared with MoS 2 ，E-MoS 2 The specific capacity of/C is improved due to the expansion of interlayer spacing and the enhancement of conductivity; meanwhile, the carbonized layer can play a certain protection role in the structure of the whole material, and the amorphous carbon can effectively buffer the volume expansion in the charging and discharging process.
Claims (6)
1. A preparation method of spherical expanded molybdenum disulfide is characterized by comprising the following steps:
the method comprises the following steps: heating PVP in a water bath, and continuously stirring to obtain a colloidal solution with the mass concentration of 5%;
step two: pouring a mixed solution of a molybdenum source and a sulfur source into the PVP solution in the first step, wherein the mixing volume ratio of the mixed solution to the PVP solution is 1:4, stirring for 2 to 3 hours; the preparation method of the mixed solution of the molybdenum source and the sulfur source comprises the following steps of weighing 0.325g of ammonium molybdate tetrahydrate and 0.6g of thiourea, adding the weighed materials into 10mL of deionized water, and stirring until the materials are fully dissolved;
step three: dropwise adding 1mol/L HCl into the mixed solution obtained in the second step, and adjusting the pH value to 4-5;
step four: adding the mixed solution obtained in the third step into a reaction kettle, placing the reaction kettle in a blast drying oven, and heating the reaction kettle at 180 ℃ for 24 hours to obtain PVP intercalated molybdenum disulfide with enlarged interlayer spacing;
step five: placing the PVP intercalated molybdenum disulfide with enlarged interlayer spacing into a corundum porcelain boatSintering in a high-temperature tube furnace to obtain E-MoS 2 C; the sintering temperature is 400 ℃ and the time is 2h.
2. The method for preparing spherical expanded molybdenum disulfide according to claim 1, wherein: in the first step, the water bath temperature is 80 to 90 ℃, and the water bath time is set to be 2 to 3 hours.
3. The method for preparing spherical expanded molybdenum disulfide according to claim 1, wherein: and in the fourth step, repeatedly centrifuging and washing the obtained molybdenum disulfide with the enlarged interlayer spacing of the PVP intercalation, and drying at 60 ℃ to obtain black powder.
4. The method for preparing spherical expanded molybdenum disulfide according to claim 1, wherein: in the fifth step, the temperature rise rate of the tube furnace is 5 ℃/min.
5. The application of the spherical molybdenum disulfide with the expanded layer prepared by the method in any one of claims 1 to 4 in a zinc ion battery positive electrode material.
6. The application of the spherical expanded molybdenum disulfide in the positive electrode material of the zinc ion battery according to claim 5, wherein: the layer-expanded molybdenum disulfide is used as an active substance of a zinc ion battery positive electrode material, and the active substance, a conductive agent and a binder are mixed according to the weight ratio of 7:2:1, coating the mixture on a carbon paper current collector, and drying to obtain the zinc ion battery positive plate.
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