CN110371934A - A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material - Google Patents
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material Download PDFInfo
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Abstract
It is respectively that thiocarbamide is soluble in water the invention discloses a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, stir to get thiourea solution；Sodium molybdate is soluble in water, stir to get sodium molybdate aqueous solution；Selenium powder is dissolved in hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；Then after being uniformly mixed above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor in beaker, carbon material is added, is transferred in autoclave, solvent thermal reaction is carried out, confined reaction for a period of time, is cooled to after room temperature, washing, vacuum drying；It will anneal in the tube furnace of obtained product under nitrogen protection to get carbon-based sulphur selenizing molybdenum composite material is arrived.This method is conducive to shorten lithium ion diffusion path, enhancing electrode reaction.Low in cost, simple process of the invention increases reaction site, is conducive to promote battery performance by building vacancy.
Description
Technical field
The invention belongs to C-base composte materials to synthesize field, and in particular to a kind of preparation of carbon-based sulphur selenizing molybdenum composite material
Method.
Background technique
In recent years, people start increasingly to pay close attention to higher performance and cheap rechargeable battery on an electronic device
Application.Carbon-based material as it is a kind of be easy to get, green electric conductor, because it is with more micromorphology, high thermal stability
And its stronger mechanical performance endures always the concern of electrochemical research scholar to the fullest extent.Other electricity are added to as conductive filler
Among the material of pole, it can not only improve the electronics and ion transport capability of combination electrode material, can also significantly increase electrode material
Mechanical performance, and be easy in the synthesis process of electrode material carry out growth in situ synthesis, make its energy convert and store up
The fields such as memory device, electronic sensor all have extremely wide application prospect.
Transition metal dichalcogenide on battery high capacity, high security, conversion reaction high availability the advantages that and
Its sandwich being made of multi-layer atomic layer is alkali metal ion insertion/deintercalation ideal anode, they having the same two
The class graphene layer structure of a six sides layered crystal structure composition, they between layers mainly by weaker Van der Waals force
Connection, this unique crystal structure make it in battery, the Material Fields such as supercapacitor and electro-chemical water decomposition catalyst
Possess biggish potentiality.
Pure molybdenum sulfide and selenizing molybdenum is because its reaction site is less, and sulphur selenizing molybdenum is during the reaction because of sulphur and selenium
Atomic radius gap so that interlayer has more reaction sites exposed, after carrying out carbon-based load, sulphur selenizing molybdenum
It is not easy to reunite, it is dispersed in carbon material surface, improves the stability of material.
Therefore, by the carbon material of high conductivity in conjunction with sulphur selenizing molybdenum, dispersion problem and surface reaction site are solved
Problem can preferably play the advantage of the two.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of carbon-based sulphur selenizing molybdenum composite material, and a kind of electrification is prepared
Learn the carbon-based sulphur selenizing molybdenum composite material of low cost of good performance；Preparation process is simple, facilitates operation, is a kind of efficient quick
Synthetic method.
The technical solution adopted by the present invention to solve the technical problems is: a kind of preparation of carbon-based sulphur selenizing molybdenum composite material
Method includes the following steps
A), thiocarbamide is soluble in water, stir to get thiourea solution；
B), sodium molybdate is soluble in water, stir to get sodium molybdate aqueous solution；
C), selenium powder is dissolved in hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, add
Entering carbon material, be transferred in autoclave, carries out solvent thermal reaction, confined reaction for a period of time, is cooled to after room temperature,
Centrifugation is washed, vacuum drying；
E), it will anneal in the tube furnace under nitrogen protection of product obtained in step d) to get to carbon-based sulphur selenizing molybdenum
Composite material.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, 0.01~0.1mmol thiocarbamide in step a)
Corresponding 10 mL distilled water.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, 0.01~0.1mmol molybdic acid in step b)
Sodium corresponds to 10 mL distilled water.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, 0.01~0.1mmol selenium powder in step c)
Corresponding 10 mL hydrazine hydrates.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, element sulphur, molybdenum element and selenium in step d)
The molar ratio of element is 1:1:1, and mixing time is 0.5~2h, and whipping temp is 25~50 DEG C.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, carbon material are carbon-fiber film, carbon paper or carbon
Cloth.
A kind of preparation method of the carbon-based sulphur selenizing molybdenum composite material, carbon material be added quality be 0.01~
0.12g。
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, the solvent thermal reaction temperature in step d) are
150~230 DEG C, the reaction time is 10~20h.
A kind of preparation method of the carbon-based sulphur selenizing molybdenum composite material, the drying temperature in step d) is 65~
110 DEG C, drying time be 12~30h.
A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, the cycle of annealing rate of heat addition in step e)
For 3~7 DEG C/min, annealing temperature is 300~800 DEG C, and the retention time is 3~15h.
The beneficial effects of the present invention are: preparation method simple process of the present invention, being easily achieved, and low in cost, furthermore
The method of the present invention builds defect by annealing process in sulphur selenizing molybdenum layer, introduces vacancy, increases reaction site, improve carbon-based
The chemical property of sulphur selenizing molybdenum composite material.
Detailed description of the invention
Fig. 1 is the photomacrograph of carbon-based sulphur selenizing molybdenum composite material in the embodiment of the present invention 1；
Fig. 2 is the stereoscan photograph of carbon-based sulphur selenizing molybdenum composite material in the embodiment of the present invention 1；
Fig. 3 is the transmission electron microscope photo of carbon-based sulphur selenizing molybdenum composite material in the embodiment of the present invention 1；
Fig. 4 is that carbon-based sulphur selenizing molybdenum composite material exists with unannealed material and bright sulfur selenizing molybdenum in the embodiment of the present invention 1
0.2A·g-1Current density under, fill for potassium electricity button cell performance test comparison.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Referring to figs. 1 to 4, the method that this method uses solvent heat, prepares carbon-based sulphur selenizing molybdenum composite material, passes through
Load on carbon-fiber film, using the bigger serface of carbon material, so that sulphur selenizing molybdenum uniform load on carbon-fiber film, suppression
The reunion of sulphur selenizing molybdenum processed improves the stability of material, improves the cycle life of potassium battery.By obtaining potassium after annealing
The carbon-based sulphur selenizing molybdenum composite material of anode, has built the defect of material, has built sulphur selenium vacancy, increased reaction site,
Improve the specific discharge capacity of potassium electricity.
Embodiment 1
A), 0.02mmol thiocarbamide is dissolved in 10ml water, stirs to get thiourea solution；
B), 0.02mmol sodium molybdate is dissolved in 10ml water, stirs to get sodium molybdate aqueous solution；
C), 0.02mmol selenium powder is dissolved in 10ml hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, 30
1h is stirred at DEG C, the quality that carbon-fiber film is added is 0.01g, is transferred in 50ml autoclave, solvent thermal reaction is carried out,
150 DEG C of confined reaction 10h, are cooled to after room temperature, distill water washing three times, 65 DEG C of vacuum drying 12h；
E, by the tube furnace under nitrogen protection of product obtained in step d to be heated under the heating rate of 3 DEG C/min
400 DEG C of holding 10h are cooled to room temperature and obtain carbon-based sulphur selenizing molybdenum composite material later.
Embodiment 2
A), 0.05mmol thiocarbamide is dissolved in 10ml water, stirs to get thiourea solution；
B), 0.05mmol sodium molybdate is dissolved in 10ml water, stirs to get sodium molybdate aqueous solution；
C), 0.05mmol selenium powder is dissolved in 10ml hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, 25
0.5h is stirred at DEG C, 0.05g carbon paper is added, is transferred in 50ml autoclave, carries out solvent thermal reaction, and 200 DEG C closed anti-
15h is answered, is cooled to after room temperature, distills water washing three times, 75 DEG C of vacuum drying 12h；
E, by the tube furnace under nitrogen protection of product obtained in step d to be heated under the heating rate of 5 DEG C/min
300 DEG C of holding 15h are cooled to room temperature and obtain carbon-based sulphur selenizing molybdenum composite material later.
Embodiment 3
A), 0.1mmol thiocarbamide is dissolved in 10ml water, stirs to get thiourea solution；
B), 0.1mmol sodium molybdate is dissolved in 10ml water, stirs to get sodium molybdate aqueous solution；
C), 0.1mmol selenium powder is dissolved in 10ml hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, 45
2h is stirred at DEG C, 0.01g carbon fiber is added, is transferred in 50ml autoclave, carries out solvent thermal reaction, and 180 DEG C closed anti-
20h is answered, is cooled to after room temperature, distills water washing three times, 110 DEG C of vacuum drying 30h；
E, by the tube furnace under nitrogen protection of product obtained in step d to be heated under the heating rate of 7 DEG C/min
500 DEG C of holding 5h are cooled to room temperature and obtain carbon-based sulphur selenizing molybdenum composite material later.
Embodiment 4
A), 0.01mmol thiocarbamide is dissolved in 10ml water, stirs to get thiourea solution；
B), 0.01mmol sodium molybdate is dissolved in 10ml water, stirs to get sodium molybdate aqueous solution；
C), 0.01mmol selenium powder is dissolved in 10ml hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, 50
1.5h is stirred at DEG C, 0.12g carbon cloth is added, is transferred in 50ml autoclave, carries out solvent thermal reaction, and 230 DEG C closed anti-
18h is answered, is cooled to after room temperature, three times, 90 DEG C of vacuum drying are for 24 hours for distillation water washing；
E, by the tube furnace under nitrogen protection of product obtained in step d to be heated under the heating rate of 5 DEG C/min
800 DEG C of holding 3h are cooled to room temperature and obtain carbon-based sulphur selenizing molybdenum composite material later.
The present invention is by the carbon-based sulphur selenizing molybdenum composite material of solvent-thermal method growth in situ one-step synthesis, and moving back by the later period
Fiery program carries out building vacancy processing, the carbon-based sulphur selenizing molybdenum composite material being had excellent performance.
Carbon-based sulphur selenizing molybdenum composite material prepared by the present invention makes full use of the high-specific surface area and electric conductivity of carbon material
The advantages of, so that sulphur selenizing molybdenum is evenly coated above carbon base body, the reunion and stacking of bright sulfur selenizing molybdenum are effectively inhibited, is increased
Response area enhances stability, and by the annealing in later period, defect is built between nanoscale twins, carries out drawing for vacancy
Enter, obtains the carbon-based sulphur selenizing molybdenum composite material of more multiple reaction site.
Carbon-based sulphur selenizing molybdenum composite material prepared by the present invention as a kind of promising electrochemical field new material,
Be conducive to improve potassium battery performance during potassium battery applications, and be expected to urge applied to other batteries, supercapacitor and electricity
The electrochemical fields such as change.
The above-described embodiments merely illustrate the principles and effects of the present invention, and the embodiment that part uses, for
For those skilled in the art, without departing from the concept of the premise of the invention, can also make it is several deformation and
It improves, these are all within the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material, it is characterised in that: include the following steps
A), thiocarbamide is soluble in water, stir to get thiourea solution；
B), sodium molybdate is soluble in water, stir to get sodium molybdate aqueous solution；
C), selenium powder is dissolved in hydrazine hydrate, ultrasonic disperse, obtains selenium powder hydrazine hydrate mixed liquor；
D), after above-mentioned thiourea solution, sodium molybdate aqueous solution, selenium powder hydrazine hydrate mixed liquor being uniformly mixed in beaker, add
Entering carbon material, be transferred in autoclave, carries out solvent thermal reaction, confined reaction for a period of time, is cooled to after room temperature,
Centrifugation is washed, vacuum drying；
E), it will anneal in the tube furnace under nitrogen protection of product obtained in step d) to get to carbon-based sulphur selenizing molybdenum
Composite material.
2. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
0.01~0.1mmol thiocarbamide corresponds to 10 mL distilled water in step a).
3. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
0.01~0.1mmol sodium molybdate corresponds to 10 mL distilled water in step b).
4. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
0.01~0.1mmol selenium powder corresponds to 10 mL hydrazine hydrates in step c).
5. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that the step
It is rapid d) in element sulphur, molybdenum element and selenium element molar ratio be 1:1:1, mixing time be 0.5~2h, whipping temp 25
~50 DEG C.
6. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
Carbon material is carbon-fiber film, carbon paper or carbon cloth.
7. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
It is 0.01~0.12g that quality, which is added, in carbon material.
8. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
Solvent thermal reaction temperature in step d) is 150~230 DEG C, and the reaction time is 10~20h.
9. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
Drying temperature in step d) is 65~110 DEG C, drying time is 12~30h.
10. a kind of preparation method of carbon-based sulphur selenizing molybdenum composite material according to claim 1, which is characterized in that described
Step e) in the cycle of annealing rate of heat addition be 3~7 DEG C/min, annealing temperature be 300~800 DEG C, the retention time be 3~
15h。
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| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Spherical MoSe1.48S0.52@C cathode composite and aluminum ion battery |
| CN114335468A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | A kind of lithium-sulfur battery positive electrode/negative electrode material and preparation method thereof |
| CN114335408A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Composite electrode and preparation method and application thereof |
| CN114349053A (en) * | 2021-12-02 | 2022-04-15 | 安庆师范大学 | Preparation method and application of molybdenum sulfide nanosheets with controllable sulfur vacancy concentration |
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| CN114335408A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Composite electrode and preparation method and application thereof |
| CN114477103A (en) * | 2022-01-20 | 2022-05-13 | 西安工业大学 | MoS2-xSex graded gas sensor material with high activity at room temperature and preparation method |
| CN114477103B (en) * | 2022-01-20 | 2023-10-24 | 西安工业大学 | MoS with high activity at room temperature 2-x Se x Hierarchical gas-sensitive material and preparation method thereof |
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