CN106252616A - A kind of nickelous selenide/hollow carbon fiber composite and preparation method thereof - Google Patents
A kind of nickelous selenide/hollow carbon fiber composite and preparation method thereof Download PDFInfo
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- CN106252616A CN106252616A CN201610612729.3A CN201610612729A CN106252616A CN 106252616 A CN106252616 A CN 106252616A CN 201610612729 A CN201610612729 A CN 201610612729A CN 106252616 A CN106252616 A CN 106252616A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
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- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
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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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to Transition-metal dichalcogenide material with carbon element technical field, be specially a kind of nickelous selenide/hollow carbon fiber composite and preparation method thereof.Preparation process of the present invention includes: utilize high temperature cabonization Cotton Gossypii to prepare hollow carbon fiber, the nickel hydroxide nano sheet being vertically oriented by chemical bath deposition method growth in situ on hollow carbon fiber again, finally the nickel hydroxide of gained/hollow carbon fiber composite is carried out selenizing, prepare nickelous selenide/hollow carbon fiber composite.In the present invention, the carbon fiber of preparation is hollow structure, and specific surface area is big, good conductivity, and preparation process is simple, with low cost;Nickelous selenide/hollow carbon fiber composite the morphology controllable of final preparation, nickelous selenide is grown on the inside and outside tube wall of hollow carbon nanofiber equably, make full use of the unique hollow tubular structure of hollow carbon fiber and high specific surface area, can be as preferable high-performance electric catalysis material, and the electrode material of the new energy devices such as sodium-ion battery and ultracapacitor.
Description
Technical field
The invention belongs to Transition-metal dichalcogenide-material with carbon element technical field, be specifically related to a kind of nickelous selenide/hollow carbon
Fibrous composite and preparation method thereof.
Background technology
Nickelous selenide is the Transition-metal dichalcogenide of a quasi-representative, and itself has high electrical conductivity (resistivity simultaneously
< 10-2Ω cm), therefore, nickelous selenide is widely used in fields such as electrochemical catalysis liberation of hydrogen, DSSCs,
But pure nickelous selenide is prone to reunite so that its electro-chemical activity site cannot fully be exposed, have a strong impact on its catalysis
Characteristic and the performance of energy storage.Nickelous selenide and the base material of excellent in stability are carried out the most compound significant.
Carbon fiber, due to itself high conductivity, the advantage of chemical stability, can be as the base material supported active of function admirable
Material.Carbon fiber is generally prepared by by cellulose high-temperature calcination in an inert atmosphere, and what research was more at present is to use carefully
Fungin and artificial synthetic fiber are presoma, but the preparation technology of its complexity limits its production application.Cotton Gossypii, as
A kind of pure natural substance, with low cost, wide material sources, and content of cellulose own is up to 90%-95%, can as one great before
The persursor material preparing carbon fiber of scape.
The present invention, by simple technological design, prepares a kind of novel nickelous selenide/hollow carbon fiber composite.
This composite has the advantage that carbon fiber prepared by Cotton Gossypii high-temperature calcination in an inert atmosphere has hollow structure, in it
Outer tube wall can provide bigger surface area load nickelous selenide nanoparticle so that nickelous selenide nanoparticle activity edge can be abundant
Ground exposes, and effectively containment himself is reunited, and nickelous selenide itself possesses higher hydrogen evolution activity and low-resistivity, can give composite wood
The electrochemical catalysis performance that material is excellent;The excellent electric conductivity of carbon fiber is conducive to the transmission of electronics, can improve composite whole
The electric conductivity of body;Its hollow structure is conducive to the infiltration of electrolyte in electrochemical process simultaneously, thus improves its chemical property;
Therefore, carry out effectively being combined by nickelous selenide nanoparticle and hollow carbon fiber to realize good synergism, with the property prepared
The composite that energy is excellent.
Summary of the invention
It is an object of the invention to provide that a kind of preparation cost is cheap, preparation process simple, the selenium of electrochemical performance
Change nickel/hollow carbon fiber composite and its preparation method and application.
Nickelous selenide/hollow carbon fiber provided by the present invention, it prepares raw material and includes: Cotton Gossypii, ethanol, six nitric hydrates
Nickel, carbamide, selenium powder, deionized water etc..
Nickelous selenide provided by the present invention/hollow carbon fiber composite, its preparation process includes: utilize high temperature cabonization cotton
Flower obtains hollow carbon fiber, then by chemical bath deposition method growth in situ nickel hydroxide nano sheet on hollow carbon fiber, is entering
Row selenylation reaction obtains nickelous selenide/hollow carbon fiber composite.Specifically comprise the following steps that
(1) by Cotton Gossypii high temperature cabonization under an inert atmosphere, hollow carbon fiber is obtained;
(2) Nickelous nitrate hexahydrate and carbamide being dissolved in the mixed liquor of water and ethanol, stirring makes it be uniformly dispersed;
(3) hollow carbon fiber is immersed mixed liquor prepared by step (2), then reacted by chemical bath deposition method, obtain hydrogen-oxygen
Change nickel/hollow carbon fiber composite;
(4) by nickel hydroxide/hollow carbon fiber composite of preparing as air port under tube furnace, selenium powder is as windward
Mouthful, logical high pure nitrogen also heats, and to carry out selenylation reaction, obtains nickelous selenide/hollow carbon fiber composite.
In the present invention, during the high temperature cabonization described in step (1), described noble gas is high-purity argon gas or High Purity Nitrogen
Gas, high temperature cabonization temperature is 900-1200 DEG C, and the high temperature cabonization time is 1-3 h.
In the present invention, the Nickelous nitrate hexahydrate consumption of step (2) is 1-4 mmol, and amount of urea is 3-12 mmol,
Mixeding liquid volume is 20-40 mL, and in mixed liquor, water and ethanol volume ratio are 1:2-1:4, and mixed liquor can be complete by hollow carbon fiber
Full submergence.
In the present invention, the reaction of chemical bath deposition method described in step (3), heating-up temperature is 70-90 DEG C, and the response time is
6-8 h。
In the present invention, the selenylation reaction described in step (4), selenium powder consumption is 50-150 mg, programming rate is 1-10 DEG C/
Min, reaction temperature is 350-450 DEG C, is incubated 1-2 h.
Using scanning electron microscope (SEM), X x ray diffractometer x (XRD), electrochemical workstation characterizes institute of the present invention
The appearance structure of the nickelous selenide prepared/hollow carbon fiber composite and performance, its result is as follows:
(1) SEM test result shows, in the present invention, carbon fiber prepared by all carbonization Cotton Gossypiis has the structure of hollow, and it is high
Specific surface area be that nickelous selenide provides abundant load site.Prepared nickelous selenide/hollow carbon fiber composite has
Unique multilevel hierarchy, nickelous selenide is evenly distributed in the inside and outside tube wall of hollow carbon fiber, makes electrochemistry site alive obtain fully
Expose, see accompanying drawing 1;
(2) XRD test result shows, prepared nickel hydroxide/hollow carbon fiber is in addition to the Bao Feng of hollow carbon fiber, at 2 θ
The characteristic peaks of=12.6,25.3,33.9 and 60.4 display nickel hydroxides, corresponding to (003), (006), (101) and
(110) crystal face.And after selenylation reaction, obtained nickelous selenide/hollow carbon fiber in 2 θ=30.5,34.2,37.5,
The diffraction maximum of 43.4,51.2,56.1,58.4,62.9,73.5 and 75.0 corresponds respectively to (200) of nickelous selenide,
(210), (211), (220), (311), (023), (321), (400), (421) and (332) crystal face.Prepared nickelous selenide/stone
Ink alkene/carbon nano tube compound material shows the characteristic peak of nickelous selenide, illustrates that nickelous selenide nanometer sheet is the most successfully carried on graphite
On alkene/carbon nanotube aerogel, see accompanying drawing 2;
(3) Electrochemical results shows, nickelous selenide/hollow carbon fiber composite embodies the electrochemical catalysis liberation of hydrogen of excellence
Performance, its initial overpotential is at-0.96 V, with the nickel hydroxide/hollow carbon fiber composite phase almost without hydrogen evolution activity
Ratio, its Hydrogen Evolution Performance has had and has greatly promoted, and sees accompanying drawing 3.
It is an advantage of the current invention that:
1, preparation process is simple, it is easy to operation, is a kind of preparation method the most efficiently;
2, experimental design is ingenious.
First, the substrate of selection is the hollow carbon fiber that Cotton Gossypii carbonization obtains.Just in being can get by high temperature cabonization Cotton Gossypii
Empty carbon fiber, its original wide material sources, preparation process is simple.The hollow structure of carbon fiber can provide inside and outside tube wall with negative
Carry nickelous selenide, thus expose more avtive spot.Carbon fiber has the electric conductivity of excellence so that in electrochemical process, electronics can
Transmit with effective and rapid so that the excellent properties of nickelous selenide is fully used.The hollow tubular structure of carbon fiber is conducive to
The infiltration of electrolyte ion and migration, further enhance the chemical property of composite.
Second, on base material, first grown nickel hydroxide nano sheet by simple chemical bath deposition method, by its selenium
The method turning to nickelous selenide achieves nickelous selenide being uniformly distributed at hollow carbon fiber so that active material and base material excellent
Gesture is given full play to simultaneously, thus has constructed the composite with multilevel hierarchy.
Nickelous selenide prepared by the present invention/hollow carbon fiber composite, can be used as high-performance liberation of hydrogen catalyst material and
The preferably electrode material such as sodium-ion battery, ultracapacitor.
Accompanying drawing explanation
Fig. 1 is the nickelous selenide/hollow carbon fiber composite SEM figure of the embodiment of the present invention 3, (A) low enlargement ratio, (B)
High magnification.
Fig. 2 is the XRD figure of the nickelous selenide/hollow carbon fiber composite of the embodiment of the present invention 3.
Fig. 3 be the nickelous selenide/hollow carbon fiber composite of the embodiment of the present invention 3 and nickel hydroxide/hollow carbon fiber multiple
The linear sweep voltammetry curve (LSV) of condensation material.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is expanded on further, it should be appreciated that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art
The present invention can make various change or amendment, and these equivalent form of values fall within what the application appended claims was limited equally
Scope.
Embodiment 1, the present embodiment comprise the following steps:
(1) being positioned in high pure nitrogen by Cotton Gossypii and carry out high temperature cabonization, high temperature cabonization temperature is 900 DEG C, and the high temperature cabonization time is 2
H, prepares hollow carbon fiber;
(2) carbamide of 1 mmol Nickelous nitrate hexahydrate and 3 mmol is dissolved in (volume ratio in the mixed liquor of 30 mL second alcohol and waters
2:1), stir a period of time, be allowed to be uniformly dispersed;
(3) after 5 mg hollow carbon fibers being immersed mixed liquor prepared by (4), heating in water bath to 80 DEG C, reacts 7 h, treats that nature drops
Wen Hou, takes out carbon fiber deionized water and ethanol repeatedly cleans repeatedly and is dried, and prepares nickel hydroxide/hollow carbon fiber
Composite, is designated as Ni (OH)2-HCF;
(4) nickel hydroxide prepared/hollow carbon fiber composite being placed in air port under tube furnace, mouth of being in the wind is placed
100 mg selenium powders carry out selenizing, and the programming rate of selenylation reaction is 2 DEG C/min, and temperature is 350 DEG C, and temperature retention time is 1 h, preparation
Obtain nickelous selenide/hollow carbon fiber composite, be designated as NiSe2-HCF-1。
Embodiment 2, changing the selenizing temperature in embodiment 1 into 400 DEG C, remaining is all with embodiment 1, and finally obtained answers
Condensation material is designated as NiSe2-HCF-2。
Embodiment 3, changing the selenizing temperature in embodiment 1 into 450 DEG C, remaining is all with embodiment 1, and finally obtained answers
Condensation material is designated as NiSe2-HCF-3。
Embodiment 4, changing the temperature of the Cotton Gossypii carbonization in embodiment 1 into 1000 DEG C, remaining is all with embodiment 1, final institute
The composite obtained is designated as NiSe2-HCF-4。
Fig. 1 is the nickelous selenide/hollow carbon fiber composite SEM figure of the embodiment of the present invention 3, (A) low enlargement ratio, (B)
High magnification.Fig. 2 is the XRD figure of the nickelous selenide/hollow carbon fiber composite of the embodiment of the present invention 3.Fig. 3 is that the present invention is real
Execute the nickelous selenide/hollow carbon fiber composite of example 3 and the linear sweep voltammetry song of nickel hydroxide/hollow carbon fiber composite
Line (LSV).Nickelous selenide prepared by remaining embodiment/hollow carbon fiber composite has similar pattern and character.
Claims (7)
1. the preparation method of nickelous selenide/hollow carbon fiber composite, it is characterised in that: prepared by high temperature cabonization Cotton Gossypii
Obtain hollow carbon fiber, then by chemical bath deposition growth in situ nickel hydroxide nano sheet on hollow carbon fiber, finally will
It carries out selenization, specifically comprises the following steps that
(1) by Cotton Gossypii high temperature cabonization under an inert atmosphere, hollow carbon fiber is obtained;
(2) Nickelous nitrate hexahydrate and carbamide being dissolved in the mixed liquor of water and ethanol, stirring makes it be uniformly dispersed;
(3) hollow carbon fiber is immersed mixed liquor prepared by step (2), then reacted by chemical bath deposition method, obtain hydrogen-oxygen
Change nickel/hollow carbon fiber composite;
(4) nickel hydroxide prepared/hollow carbon fiber composite is dried and as air port under air-flow in tube furnace, selenium
Powder is placed in air-flow uptake, heats so that nickel hydroxide/hollow carbon fiber carries out selenylation reaction in high pure nitrogen air-flow,
To nickelous selenide/hollow carbon fiber composite.
The preparation method of nickelous selenide the most according to claim 1/hollow carbon fiber composite, it is characterised in that step
(1) in, described noble gas is high-purity argon gas or high pure nitrogen, and high temperature cabonization temperature is 900-1200 DEG C, the high temperature cabonization time
It is 1 ~ 3 h.
The preparation method of nickelous selenide the most according to claim 1 and 2/hollow carbon fiber composite, it is characterised in that step
Suddenly in (2), described Nickelous nitrate hexahydrate consumption is 1-4mmol, and amount of urea is 3-12mmol, and mixeding liquid volume is 20-40
ML, in mixed liquor, water and ethanol volume ratio are 1:2-1:4, and the hollow carbon fiber that Cotton Gossypii carbonization prepares is soaked by mixed liquor completely
Not yet.
The preparation method of nickelous selenide the most according to claim 3/hollow carbon fiber composite, it is characterised in that step
(3), in, described chemical bath deposition method reaction, reaction temperature is 70-90 DEG C, and the response time is 6-8 h.
5. according to the preparation method of the nickelous selenide/hollow carbon fiber composite described in claim 1,2 or 4, it is characterised in that
In step (4), described selenylation reaction, selenium powder consumption is 50-150 mg, and the programming rate of heating is 1-10 DEG C/min, reaction
Temperature is 350-550 DEG C, is incubated 1-2 h.
6. one of claim 1-5 as described in nickelous selenide/graphene/carbon nano-tube composite wood of preparing of preparation method
Material.
7. nickelous selenide/Graphene/carbon nanotube composite material as claimed in claim 6 is as high-performance electric catalysis material, with
And the application of the electrode material of sodium-ion battery and ultracapacitor.
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CN107732116A (en) * | 2017-11-20 | 2018-02-23 | 南通百正电子新材料股份有限公司 | A kind of nickelous selenide film of graphene carbon nanotube two for lithium battery and preparation method thereof |
CN109092332A (en) * | 2018-09-30 | 2018-12-28 | 河北工业大学 | A method of carbon cloth load nickelous selenide is prepared based on solwution method |
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