CN108054359A - A kind of preparation method of molybdenum disulfide hybrid material - Google Patents
A kind of preparation method of molybdenum disulfide hybrid material Download PDFInfo
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- CN108054359A CN108054359A CN201711286874.8A CN201711286874A CN108054359A CN 108054359 A CN108054359 A CN 108054359A CN 201711286874 A CN201711286874 A CN 201711286874A CN 108054359 A CN108054359 A CN 108054359A
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- H—ELECTRICITY
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of preparation method of molybdenum disulfide hybrid material, sodium molybdate, thioacetamide are mixed and added into solvent and dissolved by (1)；(2) solvent thermal reaction is carried out to the mixed solution heating of step (1)；(3) centrifuge washing after the product cooling obtained step (2)；(4) after linear polymeric is taken to carry out ultrasonic mixing intercalation to the product obtained in step (3), it is then transferred to freeze dryer freeze-drying；(5) sample in step (4) is placed in tube furnace and calcined, molybdenum disulfide hybrid material is prepared.Molybdenum disulfide prepared by the present invention/carbon heterojunction material, support of the carbochain between interlayer and piece, provide not only interlayer active site, and ion transmission provides quick passage between piece, the electric conductivity of molybdenum disulfide is also substantially increased simultaneously, so that each lamella can effective energy storage, be a kind of excellent energy storage material for having the characteristics that specific capacity height, good cycle, stable structure in ultracapacitor.
Description
Technical field
The present invention relates to energy storage device field, more particularly, to a kind of preparation method of molybdenum disulfide hybrid material.
Background technology
Electrochmical power source is to realize the device that electric energy and chemical energy are converted mutually, be it is a kind of can more reasonable energy utilization weight
Want medium.Electrochmical power source using lithium ion battery and ultracapacitor as representative has extremely wide application.Lithium ion battery
With operating voltage is high, energy density is high, self-discharge rate is low and has extended cycle life and the excellent performances such as memory-less effect, also deposit
It is low in power density, the defects of cyclical stability is poor；Ultracapacitor is fast with charging rate, and service life cycle is long, energy
Many excellent performances such as high conversion efficiency, safety coefficient height, but still it is difficult to solve the problems, such as that power density is low etc..With a new generation
The further development of energy storage device, the more excellent electrode material of development performance become urgent problem.Molybdenum disulfide is made
For a kind of typical transition metal binary compound, there is class graphene-structured.Covalent bond is formed between Mo and S atom in layer,
Structure is highly stable.The physicochemical properties of molybdenum disulfide uniqueness, have been widely used in electrochemical energy storage, and have presented pole
Good performance.The research core of current molybdenum disulfide material, is effective intercalation that 002 crystal face is carried out to it.Specifically, super
Grade capacitor area improves the conduction velocity of electronics and ion by introducing the carbon material of high conductivity in 002 crystal face of interlayer,
And then active site in layer is made full use of, realize high power, high energy storage.
Chinese patent CN106848228A discloses the method for preparing molybdenum disulfide/carbon combined multi-stage Porous materials, by molybdic acid
Heating water bath after sodium, thioacetamide and Agarose water dissolving, pours out cooling, by sample after cooling while hot after reaction
Be transferred to refrigerator freezing, after be transferred in freeze dryer dry, be finally placed in tube furnace and calcine, molybdenum disulfide/carbon is prepared
Combined multi-stage Porous materials.Although being all macroscopically aerogel material, which can only be known as carbon material and molybdenum disulfide
Simple composite structure cannot be known as heterojunction structure in nanoscale, and his aerogel material is the carbon formed with agarose
Based on skeleton.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of molybdenum disulfide hybrids
The preparation method of material.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of molybdenum disulfide hybrid material, using following steps：
(1) sodium molybdate, thioacetamide are mixed and added into solvent dissolving；
(2) solvent thermal reaction is carried out to the mixed solution heating of step (1)；
(3) centrifuge washing after the product cooling obtained step (2)；
(4) after linear polymeric is taken to carry out ultrasonic mixing intercalation to the product obtained in step (3), it is then transferred to lyophilized
Machine is freeze-dried；
(5) sample in step (4) is placed in tube furnace and calcined, molybdenum disulfide hybrid material is prepared.
The mass ratio of sodium molybdate, thioacetamide described in step (1) is 0.3~0.6:0.6~1.2, described is molten
Agent is water and ethylene glycol is 2 by volume:1 mixed solvent being mixed to get.The concentration control of the sodium molybdate in a solvent
For 0.01-0.02g/ml.
The temperature of solvent thermal reaction described in step (2) is 200-240 DEG C, reaction time 20-24h.
Centrifuge washing is alternately to be washed three times using water and ethyl alcohol in step (3).
Linear polymeric described in step (4) includes polyethyleneimine or polyethylene glycol, and quality is molybdenum disulfide point
The 20%-100% of son.The ultrasonic mixing intercalation, supersonic frequency 360-440HZ, time 1-3h.The freezing
Drying control temperature is subzero 56-40 degrees Celsius, when the time is 12-24 small.
Calcining described in step (5) controlled at degree for 600-800 degrees Celsius of lasting 2-6 it is small when, heating rate is
2-5 centigrade per minutes.
The application realizes molybdenum disulfide effective intercalation using macromolecule, so that original molybdenum disulfide on nanoscale
The interlamellar spacing of intrinsic 0.62nm is expanded to 0.95nm, and support of the carbochain between interlayer and piece provides not only interlayer active sites
Point, and ion transmission provides quick passage between piece, while also substantially increase the electric conductivity of molybdenum disulfide so that it is each
Lamella can effective energy storage, be one for having the characteristics that specific capacity height, good cycle, stable structure in ultracapacitor
The excellent energy storage material of kind, the structure based on molybdenum disulfide.
The application has benefited from selection first.Molybdenum disulfide is a kind of two-dimensional material of stratiform class graphene-structured, interlayer
It is mutually supported by weaker Van der Waals force；The molybdenum disulfide material surface of hydro-thermal method synthesis is with negative electrical charge, and high molecular polythene
Imines carries positive charge, so from intercalation driving force, this electrostatic force to attract each other of positive and negative charge plays
Very big effect；In addition, in molecular dynamics, frequency is that the ultrasonic power-assisted of 400HZ is conducive to accelerate two kinds of molecules
Movement and uniformly mixing.
Compared with prior art, molybdenum disulfide/carbon heterojunction material is prepared by the above method in the present invention, and carbochain is inserted
Enter molybdenum disulfide interlayer, improve the active site of interlayer, while good supporting role is also functioned between piece, effectively prevent
The reunion of curing molybdenum sheet provides quick passage for ion transmission.The electric conductivity of molybdenum disulfide is also substantially increased simultaneously, is made
Each lamella can effective energy storage, for having specific capacity height, good cycle, stable structure etc. excellent in ultracapacitor
Gesture is a kind of excellent energy storage material.
Description of the drawings
Fig. 1 is the electron scanning micrograph of molybdenum disulfide hybrid material prepared by embodiment 1,2,3,4.
Fig. 2 is the transmission electron microscope photo of molybdenum disulfide hybrid material prepared by embodiment 1.
Fig. 3 is molybdenum disulfide hybrid material XRD and Raman figure prepared by embodiment 1.
Fig. 4 is the charge-discharge performance curve of the ultracapacitor of molybdenum disulfide hybrid material assembling prepared by embodiment 1.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
0.3 gram of sodium molybdate and 0.6 gram of thioacetamide are added in into reaction kettle, and add in 20 milliliters of water and 10 milliliters of second
Glycol dissolves.Reaction kettle is put into heating in baking oven and carries out solvent thermal reaction, sets the temperature of baking oven as 220 degrees Celsius.Reaction
24 it is small when after, shutoff device, after cooling centrifuge washing obtain molybdenum disulfide.Then the poly- second of linear polymeric of molecular weight 600 is taken
Alkene imines carries out molybdenum disulfide sample ultrasonic mixing intercalation, after be transferred in subzero 56 degrees Celsius of freeze dryers dry 24 it is small when.
Above-mentioned sample is placed in tube furnace and is calcined, experiment condition for 800 degrees Celsius continue 6 it is small when, heating rate be 2 degrees Celsius every point
Clock.As shown in Figure 1A, the figure is it can be seen that the molybdenum disulfide of hydrothermal method synthesis uniformly divides prepared sample in flower piece shape
Cloth without significantly accumulating and reunite, and shows certain transparency, shows that the molybdenum disulfide lamella is very thin, interlayer and
Contain a small amount of graphited carbon in equally distributed part between piece.
Fig. 2 is the transmission electron microscope photo of molybdenum disulfide hybrid material prepared by embodiment 1.A and B is schemed to be somebody's turn to do
MoS2The low power transmission picture of/C hetero-junctions aerogel materials, with high molecular intercalation, layer of molybdenum-disulfide is in certain bending
Rugosity, and can significantly be seen that there is between the interlayer and piece of molybdenum disulfide the presence of partially-crystallized graphitic carbon；Scheme C more
Be measurement intercalation after heterojunction material 0.95nm is expanded to by original 0.62nm.And the intercalation of carbon, two sulphur in opposite
Change molybdenum atom and be placed with certain perturbation action so that lattice is placed with certain distortion in face, sees figure D.Fig. 3 is implementation
Molybdenum disulfide hybrid material XRD and Raman figure prepared by example 1.Using X-ray diffraction and Raman spectrum to the crystalline structure of sample
It is analyzed, finds raw material h-MoS before intercalation2Diffraction maximum position mainly 13.8 °, 33.1 °, 40.3 ° and 60.0 ° of position
It puts, such as Fig. 3 A, corresponds respectively to (002), (100), (103) and (100) crystal face (JCPDS card 37-1492).Regardless of
Macromolecule PEI or PEG, there is apparent Forward in 002 peak position after intercalation, it is each at 8.9 ° and 17.6 ° there are one
Apparent spike, it is 0.98nm to be respectively labeled as peak 1 and 2. corresponding interlamellar spacing of peak, than 002 interplanar distance of pure molybdenum disulfide
0.65nm expands nearly 0.33nm, just corresponds to the distance of one layer of carbon.This will be attributed to macromolecule and effectively insert curing
The interlayer of molybdenum molecule, after high-temperature heat treatment under inert protective atmosphere, macromolecule becomes the graphited carbon in part and stays in interlayer,
The experimental result and tem observation to data coincide.Fig. 3 B Raman spectrum test results show, the A of h-MoS21gAnd E2gVibration
The peak of pattern is located at 375.6 and 405.9cm respectively-1, the out-of-plane vibration and in plane vibration of Mo-S keys are represented respectively.And for inserting
For material after layer, the heterojunction material either after PEG or PEI intercalations, in 1350.1 and 1590.9cm-1There are two
Stronger peak corresponds respectively to D the and G peaks of carbon material after intercalation.And high molecular intercalation, to the vibration frequency of molybdenum disulfide in itself
Rate has certain interference so that A1gAnd E2gThere are certain red shift and blue-shifted phenomenon respectively, the peak position after offset is located at respectively
378.1 and 403.2cm-1.Fig. 4 is that the charge and discharge of the ultracapacitor of molybdenum disulfide hybrid material assembling prepared by embodiment 1 is electrical
It can curve.In 1Ag-1When, capacity is up to 4143.8F g-1.This has benefited from effective intercalation of high molecular material, and layer is obtained through calcining
The widened heterojunction electrode material of spacing.Support of the carbochain between the intercalation and piece of molybdenum disulfide interlayer, not only increases interlayer
Active site, and ion transmission provides quick passage between piece, while also substantially increases the electric conductivity of molybdenum disulfide,
So that each lamella can effective energy storage, therefore obtain the energy storage effect of superelevation, and in high magnification 10Ag-1When, capacity also can
Reach 2483.02F g-1。
Embodiment 2
0.3 gram of sodium molybdate and 0.6 gram of thioacetamide are added in into reaction kettle, and add in 20 milliliters of water and 10 milliliters of second
Glycol dissolves.Reaction kettle is put into heating in baking oven and carries out solvent thermal reaction, sets the temperature of baking oven as 220 degrees Celsius.Reaction
24 it is small when after, shutoff device, after cooling centrifuge washing obtain molybdenum disulfide.Then the linear polymeric of molecular weight 70000 is taken to gather
Aziridine carries out molybdenum disulfide sample ultrasonic mixing intercalation, after to be transferred in subzero 56 degrees Celsius of freeze dryers dry 24 small
When.Above-mentioned sample is placed in tube furnace and is calcined, experiment condition for 800 degrees Celsius continue 6 it is small when, heating rate be 2 degrees Celsius
It is per minute.As shown in Figure 1B, the figure is it can be seen that the molybdenum disulfide of hydrothermal method synthesis is equal in flower piece shape for prepared sample
Even distribution without significantly accumulating and reuniting, and shows certain transparency, shows that the molybdenum disulfide lamella is very thin, layer
Between contain a small amount of graphited carbon in equally distributed part between piece.The figure illustrates for same type of high score simultaneously
For son, different molecular weight intercalations influences less its sample topography, and the intercalation ability of macromolecule PEI is stronger.
Embodiment 3
0.3 gram of sodium molybdate and 0.6 gram of thioacetamide are added in into reaction kettle, and add in 20 milliliters of water and 10 milliliters of second
Glycol dissolves.Reaction kettle is put into heating in baking oven and carries out solvent thermal reaction, sets the temperature of baking oven as 220 degrees Celsius.Reaction
24 it is small when after, shutoff device, after cooling centrifuge washing obtain molybdenum disulfide.Then the poly- second of linear polymeric of molecular weight 400 is taken
Glycol carries out molybdenum disulfide sample ultrasonic mixing intercalation, after be transferred in subzero 56 degrees Celsius of freeze dryers dry 24 it is small when.It will
Above-mentioned sample, which is placed in tube furnace, to be calcined, experiment condition for 800 degrees Celsius continue 6 it is small when, heating rate be 2 degrees Celsius every point
Clock.As shown in Figure 1 C, the figure is it can be seen that the molybdenum disulfide of hydrothermal method synthesis uniformly divides prepared sample in flower piece shape
Cloth without significantly accumulating and reunite, and shows certain transparency, shows that the molybdenum disulfide lamella is very thin, interlayer and
Contain a small amount of graphited carbon in equally distributed part between piece.The figure illustrates simultaneously for different high scores similar in molecular weight
For son, there is same intercalation effect, pattern is similar.
Embodiment 4
0.3 gram of sodium molybdate and 0.6 gram of thioacetamide are added in into reaction kettle, and add in 20 milliliters of water and 10 milliliters of second
Glycol dissolves.Reaction kettle is put into heating in baking oven and carries out solvent thermal reaction, sets the temperature of baking oven as 220 degrees Celsius.Reaction
24 it is small when after, shutoff device, after cooling centrifuge washing obtain molybdenum disulfide.Then the linear polymeric of molecular weight 20000 is taken to gather
Ethylene glycol carries out molybdenum disulfide sample ultrasonic mixing intercalation, after be transferred in subzero 56 degrees Celsius of freeze dryers dry 24 it is small when.
Above-mentioned sample is placed in tube furnace and is calcined, experiment condition for 800 degrees Celsius continue 6 it is small when, heating rate be 2 degrees Celsius every point
Clock.As shown in figure iD, the figure is it can be seen that the molybdenum disulfide of hydrothermal method synthesis uniformly divides prepared sample in flower piece shape
Cloth without significantly accumulating and reunite, and shows certain transparency, shows that the molybdenum disulfide lamella is very thin, interlayer and
Between piece containing a small amount of graphited carbon in equally distributed part, the figure illustrate simultaneously for same type of macromolecule and
Speech, different molecular weight intercalations influence its sample topography little.
Compared with prior art, the special intercalation configuration material of molybdenum disulfide for the method synthesis that the present invention uses, it is real for the first time
Effective intercalation is now carried out to molybdenum disulfide molecule with macromolecule, and different type can be selected, the macromolecule of different molecular weight
Widened " M-C-M " the sandwich heterojunction electrode material of interlamellar spacing is made in material, and good conductivity, preparation method is simple, innovative
By force.Support of the carbochain between interlayer and piece provides not only interlayer active site, and ion transmission provides fast between piece
Passage, while also substantially increase the electric conductivity of molybdenum disulfide so that each lamella can effective energy storage, for ultracapacitor
In there are the advantages such as specific capacity height, good cycle, stable structure.
Embodiment 5
A kind of preparation method of molybdenum disulfide hybrid material, using following steps：
(1) it is 2 by volume sodium molybdate, thioacetamide to be mixed and added into water and ethylene glycol:1 mixing being mixed to get
Solvent dissolves, and sodium molybdate, the mass ratio of thioacetamide are 0.3:1.2, and control the concentration control of sodium molybdate in a solvent
For 0.01g/ml；
(2) 200 DEG C are heated to the mixed solution of step (1) and carries out solvent thermal reaction for 24 hours；
(3) after the product cooling obtained step (2) using water and the washing of ethyl alcohol alternating centrifugal three times；
(4) after polyethyleneimine is taken to carry out ultrasonic mixing intercalation to the product obtained in step (3), polyethyleneimine adds
Enter 20% that quality is molybdenum disulfide, it is 360HZ that when supersound process, which control supersonic frequency, and time 3h is then transferred to lyophilized
Machine, controlled at subzero 56 degrees Celsius, when freeze-drying 12 is small；
(5) sample in step (4) is placed in tube furnace, heating rate is controlled to be warming up to for 2 centigrade per minutes
600 degrees Celsius continue 6 it is small when, molybdenum disulfide hybrid material is prepared.
Embodiment 6
A kind of preparation method of molybdenum disulfide hybrid material, using following steps：
(1) it is 2 by volume sodium molybdate, thioacetamide to be mixed and added into water and ethylene glycol:1 mixing being mixed to get
Solvent dissolves, and sodium molybdate, the mass ratio of thioacetamide are 0.4:0.9, and control the concentration control of sodium molybdate in a solvent
For 0.01g/ml；
(2) 220 DEG C are heated to the mixed solution of step (1) and carries out solvent thermal reaction for 24 hours；
(3) after the product cooling obtained step (2) using water and the washing of ethyl alcohol alternating centrifugal three times；
(4) after polyethyleneimine is taken to carry out ultrasonic mixing intercalation to the product obtained in step (3), polyethyleneimine adds
Enter 50% that quality is molybdenum disulfide, it is 400HZ that when supersound process, which control supersonic frequency, and time 2h is then transferred to lyophilized
Machine, controlled at subzero 50 degrees Celsius, when freeze-drying 18 is small；
(5) sample in step (4) is placed in tube furnace, heating rate is controlled to be warming up to for 3 centigrade per minutes
700 degrees Celsius continue 5 it is small when, molybdenum disulfide hybrid material is prepared.
Embodiment 7
A kind of preparation method of molybdenum disulfide hybrid material, using following steps：
(1) it is 2 by volume sodium molybdate, thioacetamide to be mixed and added into water and ethylene glycol:1 mixing being mixed to get
Solvent dissolves, and sodium molybdate, the mass ratio of thioacetamide are 0.6:0.6, and control the concentration control of sodium molybdate in a solvent
For 0.02g/ml；
(2) 240 DEG C are heated to the mixed solution of step (1) and carries out solvent thermal reaction 20h；
(3) after the product cooling obtained step (2) using water and the washing of ethyl alcohol alternating centrifugal three times；
(4) after taking polyethylene glycol carries out ultrasonic mixing intercalation to the product obtained in step (3), the addition matter of polyethylene glycol
It measures as the 100% of molybdenum disulfide, when supersound process controls supersonic frequency, and for 440HZ, time 1h is then transferred to freeze dryer,
Controlled at subzero 40 degrees Celsius, when freeze-drying 12 is small；
(5) sample in step (4) is placed in tube furnace, heating rate is controlled to be warming up to for 5 centigrade per minutes
800 degrees Celsius continue 2 it is small when, molybdenum disulfide hybrid material is prepared.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (9)
1. a kind of preparation method of molybdenum disulfide hybrid material, which is characterized in that this method uses following steps：
(1) sodium molybdate, thioacetamide are mixed and added into solvent dissolving；
(2) solvent thermal reaction is carried out to the mixed solution heating of step (1)；
(3) centrifuge washing after the product cooling obtained step (2)；
(4) after linear polymeric is taken to carry out ultrasonic mixing intercalation to the product obtained in step (3), it is cold to be then transferred to freeze dryer
It is lyophilized dry；
(5) sample in step (4) is placed in tube furnace and calcined, molybdenum disulfide hybrid material is prepared.
2. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (1)
The sodium molybdate, the mass ratio of thioacetamide are 0.3~0.6:0.6~1.2, the solvent presses body for water with ethylene glycol
Product is than being 2:1 mixed solvent being mixed to get.
3. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (1)
The concentration control of the sodium molybdate in a solvent is 0.01-0.02g/ml.
4. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (2)
The temperature of the solvent thermal reaction is 200-240 DEG C, reaction time 20-24h.
5. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (3)
Centrifuge washing is alternately to be washed three times using water and ethyl alcohol.
6. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (4)
The linear polymeric includes polyethyleneimine or polyethylene glycol, and quality is the 20%-100% of molybdenum disulfide.
7. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (4)
The ultrasonic mixing intercalation, supersonic frequency 360-440HZ, time 1-3h.
8. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (4)
The freeze-drying is controlled at subzero 56-40 degrees Celsius, when the time is 12-24 small.
9. the preparation method of a kind of molybdenum disulfide hybrid material according to claim 1, which is characterized in that in step (5)
The calcining controlled at 600-800 degrees Celsius of lasting 2-6 it is small when, heating rate is 2-5 centigrade per minutes.
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| CN109470761A (en) * | 2018-10-19 | 2019-03-15 | 重庆医科大学 | The preparation method and detection method of nanocomposite, ZEN electrochemistry aptamer sensor |
| CN111393641A (en) * | 2020-03-24 | 2020-07-10 | 四川大学 | Surfactant capable of simultaneously stripping and vinylating two-dimensional lamellar material, preparation and application |
| CN112599752A (en) * | 2021-01-06 | 2021-04-02 | 天津工业大学 | Preparation method of carbon-coated hollow kapok fiber-loaded flower-shaped molybdenum disulfide composite material as sodium ion battery negative electrode material |
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| MIN LI ET AL.: "Surfactant‐assisted hydrothermally synthesized MoS2 samples with controllable morphologies and structures for anthracene hydrogenation", 《CHINESE JOURNAL OF CATALYSIS》 * |
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| CN109470761A (en) * | 2018-10-19 | 2019-03-15 | 重庆医科大学 | The preparation method and detection method of nanocomposite, ZEN electrochemistry aptamer sensor |
| CN109470761B (en) * | 2018-10-19 | 2020-12-04 | 重庆医科大学 | Electrochemical DNA aptamer sensor for zearalenone ZEN detection and ZEN detection method |
| CN111393641A (en) * | 2020-03-24 | 2020-07-10 | 四川大学 | Surfactant capable of simultaneously stripping and vinylating two-dimensional lamellar material, preparation and application |
| CN112599752A (en) * | 2021-01-06 | 2021-04-02 | 天津工业大学 | Preparation method of carbon-coated hollow kapok fiber-loaded flower-shaped molybdenum disulfide composite material as sodium ion battery negative electrode material |
| CN112599752B (en) * | 2021-01-06 | 2023-07-18 | 天津工业大学 | Preparation method of carbon-coated hollow kapok fiber-bearing flower-shaped molybdenum disulfide composite material serving as sodium ion battery anode material |
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