CN110373890A - The method of solvent hot preparation NiS CC nano material - Google Patents
The method of solvent hot preparation NiS CC nano material Download PDFInfo
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
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- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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Abstract
The present invention provides a kind of methods for preparing nanostructure NiS@CC material, the present invention is using carbon cloth as substrate, using six water nickel nitrates, nine water vulcanized sodium, urea as raw material, distilled water is solvent, the NiS@CC nano material with graded porous structure has been made using two step of solvent-thermal method, the nano material shows lower overpotential and biggish specific capacitance under alkaline condition, can be used as electrode material applied to the conversion of the energy such as electro-catalysis, supercapacitor and storage system.
Description
Technical field
The present invention relates to a kind of preparation method of NiS CC nano material more particularly to a kind of solvent hot preparation nanostructures
The method of NiS@CC material, is applied in the energy storage devices such as electro-catalysis, supercapacitor mainly as electrode material, is belonged to non-expensive
Metal nanometer composite material field.
Background technique
With the increasingly consumption of fossil fuel and increasingly sharpening for problem of environmental pollution, new energy conversion and storage skill
Art will play significant role in the following sustainable energy strategy, therefore study and design elctro-catalyst with high performance
It is instantly the most key project with energy storage material.Hydrogen Energy because have energy density is high, energy sources conversion cleaning is nontoxic,
The advantages that pollution-free, is considered as ideal clean energy resource.Usually industrial hydrogen production process mainly includes electrocatalytic decomposition water
Hydrogen manufacturing, photocatalytic hydrogen production by water decomposition, fossil fuel gasification and methane steam reforming etc., in numerous methods, electrocatalytic decomposition
Water hydrogen manufacturing is considered as a kind of method most with prospects.However, restrict its development main bottleneck be the absence of it is high performance
Base metal elctro-catalyst.The advantages that electric conductivity of transient metal sulfide Yin Qigao, good stability and Modulatory character,
Extensive research has been obtained in electrochemical energy conversion conversion and field of storage.In recent years, around transient metal sulfide
Research boom gradually rises, and brings more opportunities for the design of material of energy field.Compared to other traditional metal materials,
Transient metal sulfide has better electric conductivity, and its unique structural advantage makes it have more excellent electrochemistry
Energy.This provides feasible research approach for novel electro-catalytic agent and energy storage material, also setting for functional direction material
Meter and performance optimization provide a brand-new platform.
Summary of the invention
The object of the present invention is to provide a kind of methods of the preparation of NiS@CC nano material；
It is another object of the present invention to can be carried out analytic explanation to NiS CC nano material electrochemistry.
One, the preparation of nanostructure NiS@CC material
1, the processing of carbon cloth
Carbon cloth is multiple using successively being washed with acetone, distilled water and dehydrated alcohol before carbon cloth, the miscellaneous of carbon cloth surfaces is removed
Matter, it is dry.In order to improve carbon fiber hydrophily and expand interfibrous space interval, high-temperature calcination is used to the carbon cloth after removal of impurities
And acid treatment process；
The condition of high-temperature calcination: in nitrogen atmosphere, with 5 ~ 10 DEG C of min-1Rate be warming up to 800 ~ 1000 DEG C, keep 1 ~ 2h,
It is cooled to room temperature；
Acid treatment process: with concentrated hydrochloric acid (concentration 36% ~ 38%) impregnate 1.5 ~ 2.5h, with distilled water, dehydrated alcohol repeatedly wash to
Neutrality is dried in vacuo 6h at 60 DEG C.
2, the preparation of NiS@CC nano material
(1) six water nickel nitrates, urea are dissolved in distilled water (the molten concentration of six water nickel nitrates, urea is 40 ~ 50mg/mL), room
Temperature is lower to stir 0.5 ~ 1.5h；The mixed solution is transferred in ptfe autoclave, and the carbon cloth of processing is vertically put into
In mixed solution, reaction kettle is sealed, and in 100 ~ 130 DEG C of 10 ~ 13h of hydro-thermal；It is cooled to room temperature, is washed with distilled water, dehydrated alcohol
It washs, is dried in vacuo, obtains carrying precursor carbon cloth.
Urea keeps constant pH value of reaction system as precipitation from homogeneous solution agent, by slow release ammonia, promotes Ni2+And S2 +Homogeneous reaction.The mass ratio of six water nickel nitrates and urea is 1:5 ~ 1:7.
(2) nine water vulcanized sodium are dissolved in distilled water, stirring mixes them thoroughly (nine water vulcanization in mixed solution at room temperature
The amount of sodium is 0.005 ~ 0.007g/mL)；Mixed solution is transferred in ptfe autoclave, and by carrying precursor carbon cloth
It is vertically put into mixed liquor, reaction kettle is sealed, and in 80 ~ 100 DEG C of 7 ~ 9h of hydro-thermal reaction；It is cooled to room temperature, with distilled water, nothing
Water-ethanol washing is dried in vacuo 5 ~ 7h at 50 ~ 70 DEG C to get NiS@CC nano material.
Two, the structural characterization of nanostructure NiS@CC material
The microstructure of material prepared is characterized by field emission scanning electron microscope, and crystal structure is to pass through powder
X-ray diffractometer (XRD；Cu target: λ=1.5418,40 kV of tube voltage, tube current 60 mA, sweep speed 5omin-1) carry out
Analysis.
1, field emission scanning electron microscope (SEM) is analyzed
Fig. 1 is field emission scanning electron microscope (SEM) picture of nanostructure NiS@CC material prepared by the present invention.It is observed from figure
Nanostructure NiS@CC material is the network nano structure being cross-linked with each other, and pattern is orderly regular, and has open and porous spy
Property.
2, X diffraction spectrogram (XRD) is analyzed
Fig. 2 is the X diffraction spectrogram (XRD) of nanostructure NiS@CC material prepared by the present invention.In Fig. 2, NiS@CC material is in 2 θ
Peak of the angle about at 25 ° and 45 ° belongs to (002) and (101) crystal face of carbon cloth, is the characteristic peak of carbon cloth.NiS@in figure
For the principal character peak of CC material at 31.0,45.2 and 53.8 °, corresponding crystal face is (100), (102) and (110)
(PDF50-1791), show the presence of NiS in material.
Three, chemical property
Chemical property is to test in three-electrode system at room temperature, and electrochemical workstation is CHI 760E(occasion China, Shanghai, in
State).Below by electrochemical workstation CHI 760E to the chemical property of nanostructure NiS@CC material prepared by the present invention
It is described in detail.(all electrochemical datas with reversible hydrogen electrode (RHE) potential inversion of phases, in the conversion of alkaline condition
Equation is E (RHE)=EΘ(Ag/AgCl)+0.059 × pH)
1, the HER electro-catalysis of material is tested under alkaline condition
Fig. 3 is the HER performance correlation figure of NiS@CC nano material prepared by the present invention.Wherein, (a) is the LSV curve of NiS@CC:
When current density is 10 mA cm-2When, the overpotential of NiS@CC-2 is 295mV；(b) the Tafel slope for being NiS@CC: afel is oblique
Rate is 156 mV dec-1, small Tafel slope shows that NiS@CC catalyst keeps HER reaction rate relatively fast；It (c) is NiS@
The C of the ECSA:NiS@CC electrode of CCdlFor 10 mF cm-2, biggish CdlIt is living that value means that NiS@CC electrode has reached electrochemistry
The level of property surface area；(d) the LSV curve for NiS@CC electrode after initial and 1000 circle CV circulations, illustrates the HER of the material
Performance is very excellent；(e) the EIS curve for being NiS@CC: its obvious diameter is smaller, it is meant that occurs on porous electrode quick
HER reaction；It (f) be NiS@CC electrode in current density is 10 mA cm-2When i-t curve, show its brilliant stability.
2, the OER electro-catalysis of material is tested under alkaline condition
Fig. 4 is the OER performance correlation figure that the present invention prepares NiS@CC nano material.Wherein, (a) is the LSV curve of NiS@CC, when
Current density is 12mA cm-2When, the overpotential of NiS@CC is only 299mV, illustrates that the material has brilliant OER performance；
(b) the LSV curve for NiS@CC electrode after initial and 1000 circle CV circulations；(c) the Tafel slope for being NiS@CC, Tafel
Slope is 136 mV dec-1, lesser Tafel slope show NiS@CC catalyst make OER reaction rate accelerate；It (d) is NiS@
The EIS curve of CC, it is clear that its diameter is smaller, it is meant that quick OER reaction occurs on porous electrode；It (e) is NiS@CC electricity
Pole is 12 mA cm in current density-2When i-t curve, curve shows its excellent stability there is no significant change.
3, the all-hydrolytic electro-catalysis of material is tested under alkaline condition
Fig. 5 is the all-hydrolytic performance correlation figure of NiS@CC nano material prepared by the present invention.The LSV that wherein (a) is NiS@CC is bent
Line, when current density is 10 mA cm-2When, the permanent potential of NiS@CC is only 1.69V, illustrates that the material has brilliant electrification
Learn performance；(b) it is i-t curve of the NiS@CC electrode when permanent potential is 1.69V, shows its excellent stability.
In conclusion the present invention is using carbon cloth as substrate, and using six water nickel nitrates, nine water vulcanized sodium, urea as raw material, distilled water
For solvent, the NiS@CC nano material with graded porous structure is made using two step of solvent-thermal method, the nano material is in alkali
Property under the conditions of show lower overpotential and biggish specific capacitance, can be used as electrode material applied to electro-catalysis, super capacitor
The conversion of the energy such as device and storage system.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope figure (SEM) of present invention preparation nanostructure NiS@CC material.
Fig. 2 is the X diffraction spectrogram (XRD) of present invention preparation nanostructure NiS@CC material.
Fig. 3 is the HER performance correlation figure of NiS@CC nano material prepared by the present invention.
Fig. 4 is the OER performance correlation figure that the present invention prepares NiS@CC nano material.
Fig. 5 is the all-hydrolytic performance correlation figure of NiS@CC nano material prepared by the present invention.
Specific embodiment
Below by specific embodiment to the preparation of nanostructure NiS@CC material of the present invention and its chemical property make into
One step detailed description.
Embodiment 1
(1) processing of carbon cloth: business carbon cloth is successively washed repeatedly with acetone, distilled water and dehydrated alcohol respectively, dry at 60 DEG C
Dry 6h.Carbon cloth after cleaning is put into porcelain boat, is then placed it in tube furnace, with 8 DEG C of min in nitrogen atmosphere-1Rate
900 DEG C of holding 1.5h are warming up to, are cooled to room temperature；2h is impregnated with concentrated hydrochloric acid, is repeatedly washed into distilled water, dehydrated alcohol
Property, 6h is dried in vacuo at 60 DEG C；
(2) preparation of NiS@CC nano material: by 1 mmol(290.79mg), six water nickel nitrate, 6mmol(360mg) urea is dissolved in
In 15mL distilled water, 1h is stirred at room temperature.The carbon that the mixed solution is transferred in ptfe autoclave, and will be handled well
Cloth (cm of 2 cm × 2) is vertically put into mixed solution, and reaction kettle is sealed and is placed in drying box in 120 DEG C of hydro-thermal reactions
12h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C, obtain carrying precursor carbon cloth；It will
Nine water vulcanized sodium of 90mg is dissolved in 15mL distilled water, stirs 0.5h at room temperature；It is anti-that the mixed solution is transferred to polytetrafluoroethylene (PTFE)
It answers in kettle, and the carbon cloth of carrying precursor carbon cloth is vertically put into mixed liquor, reaction kettle is sealed and is placed in drying box in 90
DEG C hydro-thermal 8h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C to get sample NiS@
CC-1 nano material；
(3) electrochemical property test: as reference electrode, carbon-point is used as to electrode Ag/AgCl under alkaline condition, and 0.5 × 0.5
cm2NiS@CC-1 directly as working electrode.It is mapped using 8.0 software of origin.Test result shows that NiS@CC-1 receives
Rice material is 10,20 mA cm in current density-2When, overpotential is respectively 67,109 mV；Its Tafel slope is 98 mVdec-1；The C of NiS@CC-1 electrodedlFor 13 mF cm-2, illustrate that the material has excellent HER performance, have as HER electro-catalysis material
The potential of material.
Embodiment 2
(1) processing of carbon cloth: with embodiment 1；
(2) preparation of nanostructure NiS@CC-2 material: by 1 mmol(290.79mg), six water nickel nitrate, 6mmol(360mg) urine
Element is dissolved in 15mL distilled water, stirs 1h at room temperature.The mixed solution is transferred in ptfe autoclave, and will processing
Good carbon cloth (cm of 2 cm × 2) is vertically put into mixed solution, and reaction kettle is sealed and is placed in drying box in 120 DEG C of hydro-thermals
React 12h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C, obtain carrying precursor carbon
Cloth；Nine water vulcanized sodium of 100mg is dissolved in 15ml distilled water, stirs 0.5h at room temperature；The mixed solution is transferred to polytetrafluoro
In ethylene reaction kettle, and the carbon cloth of carrying precursor carbon cloth is vertically put into mixed liquor, reaction kettle is sealed and is placed in drying box
In in 90 DEG C of hydro-thermal 8h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C to get sample
Product NiS@CC-2 nano material；
(3) electrochemical property test: as reference electrode, carbon-point is used as to electrode Ag/AgCl under alkaline condition, and 0.5 × 0.5
cm2NiS@CC-2 directly as working electrode.It is mapped using 8.0 software of origin.Test result shows to work as current density
For 10 mA cm-2When, overpotential 295mV(HER)；When current density is 12 mA cm-2When, overpotential is 299 mV
(OER), illustrate that NiS@CC-2 has lower overpotential；And when current density is 12mA cm-2When, the perseverance electricity of NiS@CC-2
Gesture is only 1.69V, illustrates that the material has brilliant chemical property, and have the potential for making multi-functional electrocatalysis material.
Embodiment 3
(1) business carbon cloth: successively being used acetone, distilled water and each ultrasound 2h of dehydrated alcohol by the processing of carbon cloth respectively, dry at 60 DEG C
Dry 6h；
(2) preparation of nanostructure NiS@CC-3 material: by 1 mmol(290.79mg), six water nickel nitrate, 6mmol(360mg) urine
Element is dissolved in 15mL distilled water, stirs 1h at room temperature.The mixed solution is transferred in ptfe autoclave, and will processing
Good carbon cloth (cm of 2 cm × 2) is vertically put into mixed solution, and reaction kettle is sealed and is placed in drying box in 120 DEG C of hydro-thermals
React 12h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C, obtain carrying precursor carbon
Cloth；Nine water vulcanized sodium of 90mg is dissolved in 15mL distilled water, stirs 0.5h at room temperature；The mixed solution is transferred to polytetrafluoroethyl-ne
In alkene reaction kettle, and the carbon cloth of carrying precursor carbon cloth is vertically put into mixed liquor, reaction kettle is sealed and is placed in drying box
In 90 DEG C of hydro-thermal 8h；It is cooled to room temperature, is repeatedly washed with distilled water, dehydrated alcohol, be dried in vacuo 6h at 60 DEG C to get sample
NiS@CC-3 nano material；
(3) electrochemical property test: saturated calomel electrode (SCE) is reference electrode under alkaline condition, and platinum guaze is used as to electrode,
0.5×0.5 cm2NiS@CC-3 directly as working electrode.It is mapped using 8.0 software of origin.Test result show when
When current density is 1A/g, the specific capacitance of electrode material is up to 569F/g, illustrates material specific capacitance with higher, there is work electricity
The potential of container electrode material.
Claims (8)
1. the method for solvent hot preparation NiS CC nano material, comprising the following steps:
(1) six water nickel nitrates, urea are dissolved in distilled water, stir 0.5 ~ 1.5h at room temperature；The mixed solution is transferred to poly-
In tetrafluoroethene reaction kettle, and the carbon cloth of processing is vertically put into mixed solution, seals reaction kettle, and in 100 ~ 130 DEG C of water
10 ~ 13h of heat；It is cooled to room temperature, is washed with distilled water, dehydrated alcohol, be dried in vacuo, obtain carrying precursor carbon cloth；
(2) nine water vulcanized sodium are dissolved in distilled water, stirring mixes them thoroughly at room temperature；Mixed solution is transferred to polytetrafluoro
In ethylene reaction kettle, and carrying precursor carbon cloth is vertically put into mixed liquor, reaction kettle is sealed, and anti-in 80 ~ 100 DEG C of hydro-thermals
Answer 7 ~ 9h；It is cooled to room temperature, is washed with distilled water, dehydrated alcohol, 5 ~ 7h is dried in vacuo at 50 ~ 70 DEG C and is received to get NiS@CC
Rice material.
2. the method for solvent hot preparation NiS CC nano material as described in claim 1, it is characterised in that: in step (1), six water
The mass ratio of nickel nitrate and urea is 1:5 ~ 1:7.
3. the method for solvent hot preparation NiS CC nano material as described in claim 1, it is characterised in that: in step (1), six water
It is 40 ~ 50mg/mL that nickel nitrate, urea, which are dissolved in the concentration in distilled water,.
4. the method for solvent hot preparation NiS CC nano material as described in claim 1, it is characterised in that: the mixing of step (2)
In solution, the amount of nine water vulcanized sodium is 5 ~ 7mg/mL.
5. the method for solvent hot preparation NiS CC nano material as described in claim 1, it is characterised in that: carbon cloth is using it
Before, the impurity for repeatedly removing carbon cloth surfaces is successively washed with acetone, distilled water and dehydrated alcohol, it is dry.
6. the method for solvent hot preparation NiS CC nano material as claimed in claim 5, it is characterised in that: to the carbon cloth after removal of impurities
Carry out high-temperature calcination and acid processing.
7. the method for solvent hot preparation NiS CC nano material as claimed in claim 6, it is characterised in that: high-temperature calcination is in nitrogen
In gas atmosphere, with 5 ~ 10 DEG C of min-1Rate be warming up to 800 ~ 1000 DEG C, keep 1 ~ 2h, be cooled to room temperature.
8. the method for solvent hot preparation NiS CC nano material as claimed in claim 6, it is characterised in that: acid processing is with dense salt
1.5 ~ 2.5h of acid soak is repeatedly washed with distilled water, dehydrated alcohol to neutrality, vacuum drying.
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Cited By (1)
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| CN115832222A (en) * | 2022-12-29 | 2023-03-21 | 楚能新能源股份有限公司 | Flexible sodium-ion battery cathode, preparation method thereof and flexible sodium-ion battery |
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