CN108046338A - A kind of cobalt doped molybdenum disulfide original position electrode and preparation method thereof - Google Patents
A kind of cobalt doped molybdenum disulfide original position electrode and preparation method thereof Download PDFInfo
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- CN108046338A CN108046338A CN201711342109.3A CN201711342109A CN108046338A CN 108046338 A CN108046338 A CN 108046338A CN 201711342109 A CN201711342109 A CN 201711342109A CN 108046338 A CN108046338 A CN 108046338A
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- C—CHEMISTRY; METALLURGY
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The present invention provides a kind of cobalt doped molybdenum disulfide original position electrode, and the cobalt doped molybdenum disulfide is uniformly substituted the cobalt doped molybdenum disulfide that molybdenum is formed by cobalt, and the object of cobalt doped molybdenum disulfide is mutually 2H type molybdenum disulfide.Specific preparation method is that at room temperature, molybdenum chloride is dissolved in ethanol solution, adds Cobalt salts, adds thiocarbamide, stirring and dissolving obtains body liquid before Co Mo S；It by above-mentioned preceding body drop-coated or is spun in substrate, 70 ~ 100 DEG C of rapid draings obtain precursor film；By precursor film in step 2 through 500 ~ 800 DEG C of 0.5 ~ 2 h of sintering in argon gas or nitrogen protection, furnace cooling, which is taken out, can obtain cobalt doped molybdenum disulfide original position electrode.The present invention utilizes Co, Mo, the uniform Combination of S atom and the easy homogeneous film formation of Co Mo S ethyl alcohol precursor liquids in Co Mo S precursor liquids；The molybdenum disulfide of cobalt doped is prepared using 500 ~ 800 DEG C of high temperature solid state reactions.Co in situ adulterates MoS2Electrode growth has compared with the pyrolysis better stability of Pt electrodes.
Description
Technical field
The present invention relates to electrodes in situ and preparation method thereof, belong to energy stores and conversion field of novel.
Background technology
Molybdenum disulfide is as a kind of new two-dimentional transient metal sulfide, because of its special physicochemical characteristics, all
It is multi-field all to become research hotspot, such as hydrodesulfurization, water electrolysis hydrogen production, field-effect transistor, solar cell, sensing
Device, lithium ion electronics and ultracapacitor etc..Research shows that the active site of molybdenum disulfide is located at the edge of lamellar structure, and piece
It is substantially inert in layer plane (basal plane).Therefore, substantial amounts of research work is devoted to defect regulation and control to increase molybdenum or sulphur
Edge is directed to structure optimization and allows molybdenum disulfide vertical substrate grown and expose more edge sites.Recently, bag letter and
Academician seminar, which finds that monometallic is atom doped, can become inert basal plane sulphur atom have high catalytic activity, such as：Cobalt,
Gold, platinum etc..Wherein cobalt doped is compared to gold and platinum, more inexpensively, thus more advantage.
In addition, the electric conductivity of molybdenum disulfide is weaker, and its bad biography that will also influence electronics of electrical contact with conductive substrates
It is defeated, and then restrict the stability of electro-catalysis chemical reaction and electrode.Growth in situ can often make as a kind of feasible solution
Obtaining has good Mechanical Contact and electrical contact between active material and substrate.
The content of the invention
In view of this, the object of the present invention is to provide it is a kind of be prepared in situ cobalt atom doping molybdenum disulfide reaction method,
This method has easily controllable required low raw-material cost, reaction condition, simple production process, the product formed
The advantages that uniformity is good, and environmental pollution is small is of great importance for the batch production of doped electrode in situ.For this purpose, the present invention carries
A kind of cobalt doped molybdenum disulfide original position electrode is supplied, the cobalt doped molybdenum disulfide uniformly substitutes the cobalt that molybdenum is formed by cobalt and mixes
Miscellaneous molybdenum disulfide, the object of cobalt doped molybdenum disulfide is mutually 2H type molybdenum disulfide.The cobalt, which uniformly substitutes, 5at%- in molybdenum
The cobalt of 20at% is instead of molybdenum.The cobalt is Nanoparticulate.
A kind of preceding body liquid prepares cobalt doped molybdenum disulfide original position electrode into solid-phase sintering under protective atmosphere again after uniform films
Method includes the following steps：
(1) at room temperature, molybdenum chloride is dissolved in ethanol solution, adds Cobalt salts, add thiocarbamide, stirring is molten
Solution, obtains body liquid before Co-Mo-S；
(2) by above-mentioned preceding body drop-coated or it is spun in substrate, 70~100 DEG C of rapid draings obtain precursor film；
(3) precursor film in step 2 is sintered 0.5~2h, furnace cooling in argon gas or nitrogen protection through 500~800 DEG C
It takes out and can obtain cobalt doped molybdenum disulfide original position electrode.
The Cobalt salts are the salt for dissolving in polar solvent, including cobaltous sulfate, cobalt chloride, cobalt nitrate, cobalt acetate, grass
Sour cobalt or bicarbonate cobalt.
The molar ratio of Cobalt salts and molybdenum chloride is 1:2~18, the concentration of molybdenum chloride is 100~700mM, metallic atom with
The molar ratio of thiocarbamide is 1：2~7.
By above-mentioned preceding body drop-coated or be spun in the step (2) in substrate, 70~100 DEG C in dry air from
It so dries or in dry 5-15min in thermal station, obtains precursor film.
In argon gas or nitrogen protection, the temperature of solid-phase sintering is 500~800 DEG C.
Molybdenum chloride under the conditions of being stirred at room temperature, is dissolved in ethyl alcohol, adds Cobalt salts by the first step, is cobalt chloride, sulfuric acid
One or more of cobalt, cobalt acetate after stirring and dissolving, add thiocarbamide, stirring and dissolving.Wherein, the metal salt of cobalt and chlorination
The molar ratio of molybdenum is 1：2~18, the concentration of molybdenum chloride is 100~700mM, and the molar ratio of metallic atom and thiocarbamide is 1：2~7.
The meaning of the step is：Reaction reagent uniformly disperses, and obtains on uniformly tri- kinds of Elements Atom scales of the Co-Mo-S without precipitation
The preceding body liquid of even mixing, this cobalt doped molybdenum disulfide that single molybdenum atom is substituted to prepare single cobalt atom lay good basis；
Almost without hydrone in precursor liquid, prevent molybdenum chloride from hydrolyzing.
Second step by above-mentioned preceding body drop-coated or is spun in substrate, such as electro-conductive glass, graphite paper, carbon cloth, copper or nickel
Paper tinsel is dried or in dry air in 70~100 DEG C of rapid draing in thermal station, and the meaning of the step is：Ethanol system is easy to
Precursor film is dried to, uniform coating is still obtained after ensureing follow-up solid phase reaction.
Precursor film in step 2 is sintered 0.5~2h by the 3rd step in argon gas or nitrogen protection through 500~800 DEG C, with stove
Cooling, which is taken out, can obtain cobalt atom doping molybdenum disulfide original position electrode.By taking the villaumite of cobalt as an example, 500~800 DEG C of sintering 0.5~
Solid phase doping reaction in 2h is：
3N2H4S→2NH3↑+2N2↑+3H2S↑(1)
The preparation principle of cobalt atom doping molybdenum disulfide original position electrode is exactly：1. utilize Co, Mo, S in Co-Mo-S precursor liquids
The uniform Combination of atom and the easy homogeneous film formation of Co-Mo-S ethyl alcohol precursor liquids；2. utilize 500~800 DEG C of high temperature solid state reactions
Prepare the molybdenum disulfide of cobalt doped.
Description of the drawings
Fig. 1 is the XRD diagram of embodiment 1 and embodiment 2.
Fig. 2 is the distribution map of the SEM figures and Co, Mo, S element in sample of 1 sample of embodiment, wherein Co, Mo, S.
Fig. 3 is embodiment 1 with being not added with pure MoS prepared by cobalt chloride in embodiment 12XPS comparison diagrams, (a-d) be respectively
Full spectrogram, Mo 3d, S 2p, Co 2p.
Fig. 4 is that the CV of sample and pyrolysis Pt in embodiment 1 cycles comparison diagram.
Fig. 5 is that the SEM-EDS of embodiment 3 schemes.
Specific embodiment
Embodiment 1：
At room temperature, 0.9mmol molybdenum chlorides are dissolved in the ethanol solution of 3mL, add 0.1mmol cobalt chlorides, treat chlorine
After changing cobalt stirring and dissolving, 3mmol thiocarbamides are added in, after thiocarbamide stirring and dissolving.The preceding body drop of 100 μ L is coated onto smooth
2.5cm × 2.5cm graphite papers surface, with 90 DEG C in thermal station dry 10min.The substrate that surface is scribbled to Co-Mo-S is put into tubular type
Stove, 600 DEG C of solid phase reaction 1h under Ar protections.After furnace temperature natural cooling, taking-up.It can obtain and uniformly be born on graphite paper
The electrode of cobalt doped molybdenum disulfide is carried, load capacity is about 270 μ g/cm2.Fig. 1 shows cobalt doped curing prepared by embodiment 1
The powder X-ray RD of molybdenum, the object of cobalt doped molybdenum disulfide is mutually 2H type molybdenum disulfide as seen from the figure, there is no other dephasigns, preliminary table
Bright cobalt does not form the dephasign of other sulfide, but enters the lattice of molybdenum disulfide.Fig. 2 is that the SEM of 1 sample of embodiment schemes
With the distribution map of Co, Mo, S element in sample, wherein Co (being represented with blue dot), Mo (being represented with red point), S are (with green point
Represent), cobalt is evenly distributed in molybdenum disulfide as seen from the figure, this further illustrates that cobalt uniformly substitutes molybdenum to enter molybdenum disulfide
In lattice.Fig. 3 is embodiment 1 with being not added with pure MoS prepared by cobalt chloride in embodiment 12XPS comparison diagrams, comparison understand when to
When cobalt salt is added in precursor liquid, cobalt is mixed with molybdenum disulfide really, forms CoMoS keys, as shown in the 2p open scores of Fig. 3 (d) Co.
XPS analysis also understand that the atom of Co and Co+Mo are about 10%.Fig. 1, Fig. 2 and Fig. 3, which are integrated, to be illustrated prepared by embodiment
Sample for Nanoparticulate Co uniformly substitute Mo Co adulterate MoS2, growth in situ is uniform thin in conductive substrates
Film.Fig. 4 is that the CV of sample and pyrolysis Pt in embodiment 1 cycles comparison diagram.Electrolyte used is:0.1MLiClO4,10mM LiI,
1mM I2Acetonitrile solution, used test method be three-electrode method, reference electrode is saturated calomel electrode, to electrode be Pt pieces, work
Make electrode and adulterate MoS for original position Co2Or pyrolysis Pt electrodes, sweep speed are 50mV s-1, scanning range：- 0.2V~1.0V.From
It can be seen from the figure that, Co in situ adulterate MoS2The I of electrode3 -+2e-→3I-The peak current density at (that peak of the lower left corner in figure)
Absolute value is more than pyrolysis Pt electrodes, this shows sulfur family chemical combination original position Co doping MoS prepared by this patented method2Electrode has fine
Electro catalytic activity, be even better than pyrolyzed Pt.In addition, from the point of view of the result of 100 Xun Huans, Co in situ adulterates MoS2Electrode 100
Peak point current after secondary CV cycle and peak-to-peak away from variation all very littles, and the variation for being pyrolyzed Pt electrodes increases relatively large, this illustrates original
Position Co doping MoS2Electrode growth securely has compared with the pyrolysis better stability of Pt electrodes very much.
Embodiment 2：
At room temperature, 1.8mmol molybdenum chlorides are dissolved in the ethanol solution of 3mL, add 0.2mmol cobalt chlorides, treat chlorine
After changing cobalt stirring and dissolving, 4mmol thiocarbamides are added in, after thiocarbamide stirring and dissolving.The preceding body drop of 100 μ L is coated onto smooth
2.5cm × 2.5cm graphite papers surface, with 70 DEG C in thermal station dry 20min.The substrate that surface is scribbled to Co-Mo-S is put into tubular type
Stove, 600 DEG C of solid phase reaction 1h under Ar protections.After furnace temperature natural cooling, taking-up.It can obtain and uniformly be born on graphite paper
The electrode of cobalt doped molybdenum disulfide is carried, load capacity is about 540 μ g/cm2.Fig. 1 shows cobalt doped curing prepared by embodiment 2
The powder X-ray RD of molybdenum, mutually the overwhelming majority is 2H type molybdenum disulfide to the object of cobalt doped molybdenum disulfide as seen from the figure, but is had a small amount of
Co9S8。
Embodiment 3：
At room temperature, 0.9mmol molybdenum chlorides are dissolved in the ethanol solution of 3mL, add 0.1mmol cobalt chlorides, treat chlorine
After changing cobalt stirring and dissolving, 3mmol thiocarbamides are added in, after thiocarbamide stirring and dissolving.The preceding body drop of 100 μ L is coated onto smooth
2.5cm × 2.5cm graphite papers surface, with 80 DEG C in thermal station dry 15min.The substrate that surface is scribbled to Co-Mo-S is put into tubular type
Stove, 800 DEG C of solid phase reaction 30min under Ar protections.After furnace temperature natural cooling, taking-up.It can obtain on graphite paper
The electrode of even load cobalt doped molybdenum disulfide, load capacity is about 270 μ g/cm2.Fig. 5 illustrates cobalt doped two prepared by embodiment 3
The powder SEM-EDS of molybdenum sulfide, cobalt element is easy to be enriched in sample surfaces under 800 DEG C of high temperature as seen from the figure.
Claims (8)
1. a kind of cobalt doped molybdenum disulfide original position electrode, which is characterized in that the cobalt doped molybdenum disulfide uniformly substitutes for cobalt
The cobalt doped molybdenum disulfide that molybdenum is formed, the object of cobalt doped molybdenum disulfide is mutually 2H type molybdenum disulfide.
2. cobalt doped molybdenum disulfide original position electrode described in claim 1, which is characterized in that the cobalt, which is uniformly substituted in molybdenum, to be had
The cobalt of 5 at%-20 at% is instead of molybdenum.
3. cobalt doped molybdenum disulfide original position electrode described in claim 1, which is characterized in that the cobalt is Nanoparticulate.
4. the preparation method of claim 1-3 any one of them cobalt doped molybdenum disulfide original position electrode, which is characterized in that
Specific preparation method is as follows：
（1）At room temperature, molybdenum chloride is dissolved in ethanol solution, adds Cobalt salts, add thiocarbamide, stirring and dissolving obtains
Body liquid before to Co-Mo-S；
（2）It by above-mentioned preceding body drop-coated or is spun in substrate, 70 ~ 100 DEG C of rapid draings obtain precursor film；
（3）Precursor film in step 2 is taken out in argon gas or nitrogen protection through 500 ~ 800 DEG C of 0.5 ~ 2 h of sintering, furnace cooling
It can obtain cobalt doped molybdenum disulfide original position electrode.
5. the preparation method of cobalt doped molybdenum disulfide original position electrode according to claim 4, which is characterized in that the gold
It is the salt for dissolving in polar solvent to belong to cobalt salt, including cobaltous sulfate, cobalt chloride, cobalt nitrate, cobalt acetate, cobalt oxalate or bicarbonate cobalt.
6. the preparation method of cobalt doped molybdenum disulfide original position electrode according to claim 4, which is characterized in that Cobalt salts
Molar ratio with molybdenum chloride is 1:2 ~ 18, the concentration of molybdenum chloride is 100 ~ 700 mM, and the molar ratio of metallic atom and thiocarbamide is 1：
2~7。
7. the preparation method of cobalt doped molybdenum disulfide original position electrode according to claim 4, which is characterized in that
The step（2）Middle by above-mentioned preceding body drop-coated or to be spun in substrate, 70 ~ 100 DEG C are done naturally in dry air
It is dry or in dry 5-15min in thermal station, obtain precursor film.
8. the preparation method of cobalt doped molybdenum disulfide original position electrode according to claim 4, which is characterized in that argon gas or nitrogen
In gas shielded, the temperature of solid-phase sintering is 500 ~ 800 DEG C.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328667A (en) * | 2018-03-09 | 2018-07-27 | 三峡大学 | A kind of method that solid phase reaction in-situ prepares flower-shaped cobalt sulfide nickel nanosphere |
| CN109208027A (en) * | 2018-10-10 | 2019-01-15 | 三峡大学 | A kind of preparation method of molybdenum disulfide-cobalt sulfide-carbon tri compound original position electrode |
| CN109273729A (en) * | 2018-09-27 | 2019-01-25 | 三峡大学 | It is a kind of that molybdenum disulfide/graphite paper electrode solution methods are prepared in situ |
| CN109306501A (en) * | 2018-09-11 | 2019-02-05 | 三峡大学 | A kind of preparation method of cobalt sulfide-carbon original position electrode |
| CN109574096A (en) * | 2018-10-31 | 2019-04-05 | 南京邮电大学 | A kind of preparation method and application of metal sulfide |
| CN109817950A (en) * | 2019-03-15 | 2019-05-28 | 贵州梅岭电源有限公司 | A kind of C cladding MoxCo1-xS2The preparation method of composite positive pole |
| CN111111729A (en) * | 2019-12-18 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111377481A (en) * | 2020-03-20 | 2020-07-07 | 苏州科技大学 | Application of cobalt-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production |
| CN112939081A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Preparation method of cobalt-doped molybdenum disulfide with yolk-eggshell structure |
| CN113322484A (en) * | 2021-05-08 | 2021-08-31 | 南京师范大学 | Co-MoS anchored by hollow carbon sphere2Preparation method and application of heterogeneous composite material |
| CN113621939A (en) * | 2020-05-07 | 2021-11-09 | 北京大学 | Universal doping method for single-layer transition metal chalcogenide |
| CN113788497A (en) * | 2021-08-12 | 2021-12-14 | 华南理工大学 | Multiphase molybdenum sulfide composite material and preparation method and application thereof |
| CN116282197A (en) * | 2023-03-15 | 2023-06-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | 1T/2H heterogeneous phase molybdenum disulfide@carbon nanotube self-supporting electrode doped with cobalt and intercalated with crystal water in situ, and preparation method and application thereof |
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| CN108328667A (en) * | 2018-03-09 | 2018-07-27 | 三峡大学 | A kind of method that solid phase reaction in-situ prepares flower-shaped cobalt sulfide nickel nanosphere |
| CN109306501A (en) * | 2018-09-11 | 2019-02-05 | 三峡大学 | A kind of preparation method of cobalt sulfide-carbon original position electrode |
| CN109273729B (en) * | 2018-09-27 | 2021-05-18 | 三峡大学 | Solution method for in-situ preparation of molybdenum disulfide/graphite paper electrode |
| CN109273729A (en) * | 2018-09-27 | 2019-01-25 | 三峡大学 | It is a kind of that molybdenum disulfide/graphite paper electrode solution methods are prepared in situ |
| CN109208027A (en) * | 2018-10-10 | 2019-01-15 | 三峡大学 | A kind of preparation method of molybdenum disulfide-cobalt sulfide-carbon tri compound original position electrode |
| CN109574096A (en) * | 2018-10-31 | 2019-04-05 | 南京邮电大学 | A kind of preparation method and application of metal sulfide |
| CN109574096B (en) * | 2018-10-31 | 2021-07-30 | 南京邮电大学 | Preparation method and application of metal sulfide |
| CN109817950A (en) * | 2019-03-15 | 2019-05-28 | 贵州梅岭电源有限公司 | A kind of C cladding MoxCo1-xS2The preparation method of composite positive pole |
| CN112939081A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Preparation method of cobalt-doped molybdenum disulfide with yolk-eggshell structure |
| CN112939081B (en) * | 2019-12-11 | 2023-03-31 | 中国科学院大连化学物理研究所 | Preparation method of cobalt-doped molybdenum disulfide with yolk-eggshell structure |
| CN111111729A (en) * | 2019-12-18 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111111729B (en) * | 2019-12-18 | 2021-08-13 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111377481A (en) * | 2020-03-20 | 2020-07-07 | 苏州科技大学 | Application of cobalt-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production |
| CN113621939A (en) * | 2020-05-07 | 2021-11-09 | 北京大学 | Universal doping method for single-layer transition metal chalcogenide |
| CN113322484A (en) * | 2021-05-08 | 2021-08-31 | 南京师范大学 | Co-MoS anchored by hollow carbon sphere2Preparation method and application of heterogeneous composite material |
| CN113788497A (en) * | 2021-08-12 | 2021-12-14 | 华南理工大学 | Multiphase molybdenum sulfide composite material and preparation method and application thereof |
| CN116282197A (en) * | 2023-03-15 | 2023-06-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | 1T/2H heterogeneous phase molybdenum disulfide@carbon nanotube self-supporting electrode doped with cobalt and intercalated with crystal water in situ, and preparation method and application thereof |
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