CN108133829B - Co(OH)2@CoMoO4The preparation method of composite nano plate - Google Patents
Co(OH)2@CoMoO4The preparation method of composite nano plate Download PDFInfo
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- CN108133829B CN108133829B CN201711396196.0A CN201711396196A CN108133829B CN 108133829 B CN108133829 B CN 108133829B CN 201711396196 A CN201711396196 A CN 201711396196A CN 108133829 B CN108133829 B CN 108133829B
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000002055 nanoplate Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910018864 CoMoO4 Inorganic materials 0.000 claims abstract description 66
- 239000006260 foam Substances 0.000 claims abstract description 39
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 39
- 239000000243 solution Substances 0.000 claims abstract description 30
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 15
- 239000010941 cobalt Substances 0.000 claims abstract description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 8
- 239000011684 sodium molybdate Substances 0.000 claims description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000001868 cobalt Chemical class 0.000 claims 1
- 150000002460 imidazoles Chemical class 0.000 claims 1
- 239000007772 electrode material Substances 0.000 abstract description 15
- 238000003860 storage Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 description 6
- 238000010276 construction Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910015667 MoO4 Inorganic materials 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- -1 oxo transition metal Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses Co (OH)2@CoMoO4The preparation method of composite nano plate, comprising: S1, processing nickel foam；S2, CoMoO is grown in nickel foam4Nanometer sheet: nickel foam being added in the mixed solution of divalent cobalt and sexavalence molybdate, after hydro-thermal reaction, is washed and dry；S3,Co(OH)2@CoMoO4The preparation of nanometer sheet: CoMoO4Nanometer sheet is put into 2-methylimidazole solution, and divalent cobalt solution is quickly poured into containing CoMoO4In the 2-methylimidazole solution of nanometer sheet, stirring, ultrasound is washed and dry.Compared with prior art, low in cost the beneficial effects of the present invention are: preparation method is simple, it can be used in being mass produced.Co(OH)2@CoMoO4Nanometer sheet has high specific capacity, and the ability of good storage charge can be used as electrode material application.
Description
Technical field
The invention belongs to supercapacitor technologies field, in particular to a kind of Co (OH)2@CoMoO4The system of composite nano plate
Preparation Method.
Background technique
Supercapacitor is that a kind of power density is big, the novel energy storage apparatus that has extended cycle life, in micro-capacitance sensor and new energy
It plays an important role in automobile.Supercapacitor is divided into pseudocapacitors and double layer capacitor from energy storage mechnism, and pseudocapacitors
There is higher energy density than double layer capacitor.Transition metal oxide is due to redox active with higher, more
The advantages that valence state, good physical/chemical stability and high temperature resistant, it is widely used in pseudocapacitors.But oxo transition metal
There is also many defects, such as redox reaction of electrode surface can reduce farad as the electrode material of supercapacitor for compound
The stability of capacitor, conductivity is low, and preparation cost height etc., to limit its large-scale application.
Research shows that the physicochemical properties of electrode material directly affect the performance of pseudocapacitors, meanwhile, electrode material
Structure largely influences energy storage behavior and the electrochemical behavior of electrode material.Therefore, many researchers are by different metal
Oxide carries out being compounded to form composite material, or the electrode material of exploitation different structure, it is expected to improve the electricity of electrode material
The performances such as appearance, energy, power density and ion diffusion rates.
In metal oxide, CoMoO4Nanometer sheet due to being served as electricity with high specific capacitance and electric conductivity extensively
The composite substrate of pole material.Co(OH)2With obvious reversible redox reaction, layer structure has biggish interlayer
Away from, biggish surface area, facilitate insertion/disengaging of electrolyte ion, and by Co (OH)2Energy again is combined on other materials
Enough increase the specific capacitance of composite material.Although CoMoO4With Co (OH)2The correlative study of compound be reported that however this
The preparation method of high performance combination electrode material often too complex, preparation cost is excessively high, and is unfavorable for being mass produced.
Summary of the invention
It is an object of the present invention to be directed to existing CoMoO4With Co (OH)2Compound preparation method present on it is above-mentioned
Problem provides a kind of Co (OH)2@CoMoO4The preparation method of composite nano plate.
To achieve the goals above, the technical solution that the application uses are as follows: Co (OH)2@CoMoO4The preparation of composite nano plate
Method includes the following steps:
Co(OH)2@CoMoO4The preparation method of composite nano plate, which comprises the steps of:
S1, processing nickel foam: firstly, nickel foam is cut slabbing, and by sheet-formed foam nickel successively 2.5moL/L~
The hydrochloric acid of 3.5moL/L, acetone are respectively ultrasonically treated 10min~20min in ethyl alcohol；Then, then with deionized water clean 3~5 times；
Finally, cleaned sheet-formed foam nickel is dried 10h~14h under 55 DEG C~65 DEG C of vacuum condition, for use；
S2, CoMoO is grown in nickel foam4Nanometer sheet: firstly, divalent cobalt is dissolved in second together with sexavalence molybdate
The in the mixed solvent of two pure and mild deionized waters, obtains mixed solution after mixing evenly, wherein the substance of cobalt element and molybdenum element
The ratio between amount is 1:1, and the volume ratio of in the mixed solvent ethylene glycol and deionized water is 1:6；Then, by the sheet-formed foam nickel after drying
It is added in mixed solution, and hydro-thermal reaction 3h~5h at 90 DEG C~110 DEG C, is cooled to room temperature；Finally, by hydrothermal product point
After not cleaned with deionized water and ethyl alcohol, dry 10h~14h, obtains CoMoO under conditions of 55 DEG C~65 DEG C4Nanometer sheet；
S3、Co(OH)2@CoMoO4The preparation of composite nano plate: firstly, divalent cobalt and 2-methylimidazole difference is each molten
Solution obtains divalent cobalt solution and 2-methylimidazole solution in the in the mixed solvent of methanol and distilled water, wherein cobalt element and 2-
The ratio between amount of substance of methylimidazole is 1:4, and the volume ratio of in the mixed solvent methanol and distilled water is 1:1；Then, by CoMoO4
Nanometer sheet is put into 2-methylimidazole solution, after stirring 10min~20min at room temperature, divalent cobalt solution is quickly poured into and is contained
There is CoMoO4In the 2-methylimidazole solution of nanometer sheet, 10min~20min is stirred at room temperature；Finally, successively with deionized water,
After ethyl alcohol and deionized water distinguish ultrasound 3min~8min, dry 4h~8h, obtains Co under conditions of 55 DEG C~65 DEG C
(OH)2@CoMoO4Composite nano plate.
Further, the sheet-formed foam nickel that it is 1.5cm × 1cm that sheet-formed foam nickel, which is cut out, in the S1.
Further, the divalent cobalt is Co (NO3)2·6H2O, the sexavalence molybdate are Na2MoO4·2H2O。
Compared with prior art, the beneficial effects of the present invention are:
(1) preparation method of the invention is simple, low in cost, can be used in being mass produced.
(2) Co (OH) of the preparation method preparation prepared through the invention2@CoMoO4Nanometer sheet with a thickness of Nano grade,
And after passage capacity test, Co prepared by the present invention (OH) is found2@CoMoO4Nanometer sheet has high specific capacity, good storage electricity
The ability of lotus can be used as electrode material application.
Detailed description of the invention
Fig. 1 is the Co (OH) of the specific embodiment of the invention 22@CoMoO4The XRD spectra of nanometer sheet；
Fig. 2 is the Co (OH) of the specific embodiment of the invention 22@CoMoO4The SEM image of nanometer sheet；
Fig. 3 is the Co (OH) of the specific embodiment of the invention 22@CoMoO4The cyclic voltammetric CV curve of composite construction nanometer sheet
Figure；
Fig. 4 is the Co (OH) of the specific embodiment of the invention 22@CoMoO4The constant current charge-discharge GCPL of composite construction nanometer sheet is bent
Line chart.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
Technical solution of the present invention is clearly and completely described in specific embodiments of the present invention.
Embodiment 1
Co(OH)2@CoMoO4The preparation method of composite nano plate, includes the following steps:
S1, processing nickel foam: firstly, nickel foam to be cut into the sheet of 1.5cm × 1cm, and sheet-formed foam nickel is distinguished
Successively 10min is respectively ultrasonically treated in 2.5mol/L hydrochloric acid, acetone and ethyl alcohol；Then, then with deionized water clean 3 times；Finally,
Cleaned sheet-formed foam nickel is dried into 10h under 55 DEG C of vacuum environment, for use；
S2, CoMoO is grown in nickel foam4Nanometer sheet: firstly, weighing the Co (NO of 0.1274g3)2·6H2O and
The Na of 0.1059g2MoO4·2H2O, i.e. Co (NO3)2·6H2O and Na2MoO4·2H2The ratio between amount of substance of O is 1:1, by Co
(NO3)2·6H2O and Na2MoO4·2H2O is dissolved in the in the mixed solvent of 2.5mL ethylene glycol and 15mL deionized water together, stirring
Mixed solution is obtained after uniformly；Then, the sheet-formed foam nickel after drying is added in mixed solution, and hydro-thermal is anti-at 90 DEG C
3h is answered, is cooled to room temperature；Finally, hydrothermal product is cleaned 3 times with deionized water, then cleaned 3 times with ethyl alcohol, by the water after cleaning
Hot dry 10h under conditions of 55 DEG C, obtains CoMoO4Nanometer sheet；
S3、Co(OH)2@CoMoO4The preparation of composite nano plate: firstly, weighing the Co (NO of 0.1455g3)2·6H2O and
The 2-methylimidazole of 0.1642g, i.e. Co (NO3)2·6H2The ratio between amount of substance of O and 2-methylimidazole is 1:4, and by Co
(NO3)2·6H2O and 2-methylimidazole are dissolved separately in the in the mixed solvent of 5mL distilled water and 5mL methanol, obtain Co (NO3)2It is molten
Liquid and 2-methylimidazole solution；Then, by CoMoO4Nanometer sheet is put into 2-methylimidazole solution, after stirring 10min at room temperature,
By Co (NO3)2Solution is quickly poured into containing CoMoO4In the 2-methylimidazole solution of nanometer sheet, 10min is stirred at room temperature；Finally,
Successively with after deionized water, ethyl alcohol and deionized water respectively ultrasound 3min, dry 4h, obtains Co (OH) under conditions of 55 DEG C2@
CoMoO4Composite nano plate.
Embodiment 2
Co(OH)2@CoMoO4The preparation method of composite nano plate, includes the following steps:
S1, processing nickel foam: firstly, nickel foam to be cut into the sheet of 1.5cm × 1cm, and sheet-formed foam nickel is distinguished
Successively 3mol/L hydrochloric acid, acetone are respectively ultrasonically treated 15min in ethyl alcohol；Then, then with deionized water clean 4 times；Finally, by clear
Washed sheet-formed foam nickel dry 12h under 60 DEG C of vacuum environment, for use；
S2, CoMoO is grown in nickel foam4Nanometer sheet: firstly, weighing the Co (NO of 0.2547g3)2·6H2O and
The Na of 0.2117g2MoO4·2H2O, i.e. Co (NO3)2·6H2O and Na2MoO4·2H2The ratio between amount of substance of O is 1:1, by Co
(NO3)2·6H2O and Na2MoO4·2H2O is dissolved in the in the mixed solvent of 5mL ethylene glycol and 30mL deionized water together, stirring
Mixed solution is obtained after uniformly；Then, the sheet-formed foam nickel after drying is added in mixed solution, and the hydro-thermal at 100 DEG C
4h is reacted, is cooled to room temperature；Finally, hydrothermal product is cleaned 5 times with deionized water, then cleaned 5 times with ethyl alcohol, and will be after cleaning
Hydrothermal product under conditions of 60 DEG C dry 12h, obtain CoMoO4Nanometer sheet；
S3、Co(OH)2@CoMoO4The preparation of composite nano plate: firstly, weighing the Co (NO of 0.291g3)2·6H2O and
The 2-methylimidazole of 0.3283g, i.e. Co (NO3)2·6H2The ratio between amount of substance of O and 2-methylimidazole is 1:4, and by Co
(NO3)2·6H2O and 2-methylimidazole are dissolved separately in the in the mixed solvent of 10mL distilled water and 10mL methanol, obtain Co (NO3)2
Solution and 2-methylimidazole solution；Then, by CoMoO4Nanometer sheet is put into 2-methylimidazole solution, stirs 15min at room temperature
Afterwards, by Co (NO3)2Solution is quickly poured into containing CoMoO4In the 2-methylimidazole solution of nanometer sheet, 15min is stirred at room temperature；Most
Afterwards, successively with after deionized water, ethyl alcohol and deionized water respectively ultrasound 5min, dry 6h, obtains Co under conditions of 60 DEG C
(OH)2@CoMoO4Composite nano plate.
Embodiment 3
Co(OH)2@CoMoO4The preparation method of composite nano plate, includes the following steps:
S1, processing nickel foam: firstly, nickel foam to be cut into the sheet of 1.5cm × 1cm, and sheet-formed foam nickel is distinguished
Successively 15min is respectively ultrasonically treated in the hydrochloric acid of 3.5mol/L, acetone and ethyl alcohol；Then, then with deionized water clean 5 times；Most
Afterwards, cleaned sheet-formed foam nickel is dried to 14h under 65 DEG C of vacuum environment, for use；
S2, CoMoO is grown in nickel foam4Nanometer sheet: firstly, weighing the Co (NO of 0.5094g3)2·6H2O and
The Na of 0.4235g2MoO4·2H2O, i.e. Co (NO3)2·6H2O and Na2MoO4·2H2The ratio between amount of substance of O is 1:1, by Co
(NO3)2·6H2O and Na2MoO4·2H2O is dissolved in the in the mixed solvent of 10mL ethylene glycol and 60mL deionized water together, stirring
Mixed solution is obtained after uniformly；Then, the sheet-formed foam nickel after drying is added in mixed solution, and the hydro-thermal at 110 DEG C
5h is reacted, is cooled to room temperature；Finally, hydrothermal product is cleaned 8 times with deionized water, then cleaned 8 times with ethyl alcohol, and will be after cleaning
Hydrothermal product under conditions of 65 DEG C dry 14h, obtain CoMoO4Nanometer sheet；
S3、Co(OH)2@CoMoO4The preparation of composite nano plate: firstly, weighing the Co (NO of 0.5529g3)2·6H2O and
The 2-methylimidazole of 0.6239g, i.e. Co (NO3)2·6H2The ratio between amount of substance of O and 2-methylimidazole is 1:4, and by Co
(NO3)2·6H2O and 2-methylimidazole are dissolved separately in the in the mixed solvent of 20mL distilled water and 20mL methanol, obtain Co (NO3)2
Solution and 2-methylimidazole solution；Then, by CoMoO4Nanometer sheet is put into 2-methylimidazole solution, stirs 20min at room temperature
Afterwards, by Co (NO3)2Solution is quickly poured into containing CoMoO4In the 2-methylimidazole solution of nanometer sheet, 20min is stirred at room temperature；Most
Afterwards, successively with after deionized water, ethyl alcohol and deionized water respectively ultrasound 8min, dry 8h, obtains Co under conditions of 65 DEG C
(OH)2@CoMoO4Composite nano plate.
In order to further detect Co prepared by the embodiment of the present invention 1~3 (OH)2@CoMoO4The surface shape of composite nano plate
Looks and performance, Co (OH) is prepared with embodiment 2 in we2@CoMoO4For composite nano plate, it is tested for the property and analyzes,
Particular content is as follows:
Fig. 1 is Co (OH)2@CoMoO4The XRD spectra of nanometer sheet, as we can see from the figure CoMoO4The diffraction maximum of nanometer sheet
It is matched with standard spectrogram JCPDS:15-439, wherein highest peak is the characteristic peak of nickel foam, it was demonstrated that is successfully prepared single-phase
CoMoO4；Co(OH)2@CoMoO4Diffraction maximum and standard spectrogram JCPDS:15-439 and standard spectrogram JCPDS:3-913 combination
Match, wherein highest peak is the characteristic peak of nickel foam.Therefore, XRD spectrum illustrates successfully to be compounded with Co (OH)2And CoMoO4。
Fig. 2 is Co (OH)2@CoMoO4The SEM image of composite construction nanometer sheet, it can be seen that have the nano junction of a large amount of sheets
The thickness size of structure, nanometer sheet is about 10nm, and nanometer sheet is intertwined to form porous structure, illustrates that present invention success is compound
Co(OH)2And CoMoO4For nano-lamellar structure.
Fig. 3 is CoMoO4Nanometer sheet and Co (OH)2@CoMoO4Composite nano plate is as electrode material, in scanning speed
5mVs-1, voltage window is the cyclic voltammetry curve test chart of 0.1V~0.6V.Co (OH) as can also be seen from Figure2@CoMoO4
The area under the curve that composite nano plate surrounds is bigger, illustrates Co (OH)2@CoMoO4Have more when composite nano plate is as electrode material
High specific capacity, the charge storage with higher electricity.
Fig. 4 is CoMoO4Nanometer sheet and Co (OH)2@CoMoO4Composite nano plate is as electrode material, in scanning speed
5mAcm-2Constant current charge-discharge curve test figure.Co (OH) as can also be seen from Figure2@CoMoO4Nanometer sheet is closed as electrode material
Material has longer discharge time, further illustrates Co (OH)2@CoMoO4Composite construction nanometer sheet has more as electrode material
High specific capacity, charge storage with higher.
In conclusion the beneficial effects of the present invention are:
(1) preparation method of the invention is simple, low in cost, can be used in being mass produced.
(2) Co (OH) prepared by the present invention2@CoMoO4Nanometer sheet with a thickness of Nano grade, and after passage capacity test,
It was found that Co (OH) prepared by the present invention2@CoMoO4Nanometer sheet has high specific capacity, and the ability of good storage charge being capable of conduct
Electrode material application.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (3)
1.Co(OH)2@CoMoO4The preparation method of composite nano plate, which comprises the steps of:
S1, processing nickel foam: firstly, nickel foam is cut slabbing, and by sheet-formed foam nickel successively 2.5moL/L~
10min~20min is respectively ultrasonically treated in the hydrochloric acid of 3.5moL/L, acetone and ethyl alcohol；Then, then with deionized water clean 3~5
It is secondary；Finally, cleaned sheet-formed foam nickel is dried 10h~14h under 55 DEG C~65 DEG C of vacuum condition, for use；
S2, CoMoO is grown in nickel foam4Nanometer sheet: firstly, divalent cobalt is dissolved in ethylene glycol together with sexavalence molybdate
With the in the mixed solvent of deionized water, obtain mixed solution after mixing evenly, wherein the amount of the substance of cobalt element and molybdenum element it
Than for 1:1, the volume ratio of in the mixed solvent ethylene glycol and deionized water is 1:6；Then, the sheet-formed foam nickel after drying is added
Into mixed solution, and hydro-thermal reaction 3h~5h at 90 DEG C~110 DEG C, it is cooled to room temperature；Finally, hydrothermal product is used respectively
After deionized water and ethyl alcohol cleaning, dry 10h~14h, obtains CoMoO under conditions of 55 DEG C~65 DEG C4Nanometer sheet；
S3、Co(OH)2@CoMoO4The preparation of composite nano plate: firstly, divalent cobalt and 2-methylimidazole are respectively dissolved in respectively
The in the mixed solvent of methanol and distilled water obtains divalent cobalt solution and 2-methylimidazole solution, wherein cobalt element and 2- methyl
The ratio between amount of substance of imidazoles is 1:4, and the volume ratio of in the mixed solvent methanol and distilled water is 1:1；Then, by CoMoO4Nanometer
Piece is put into 2-methylimidazole solution, at room temperature stir 10min~20min after, by divalent cobalt solution be quickly poured into containing
CoMoO4In the 2-methylimidazole solution of nanometer sheet, 10min~20min is stirred at room temperature；Finally, successively using deionized water, second
Pure and mild deionized water is respectively after ultrasound 3min~8min, and dry 4h~8h, obtains Co (OH) under conditions of 55 DEG C~65 DEG C2@
CoMoO4Composite nano plate.
2. Co (OH) as described in claim 12@CoMoO4The preparation method of composite nano plate, which is characterized in that in the S1
The sheet-formed foam nickel that it is 1.5cm × 1cm that sheet-formed foam nickel, which is cut out,.
3. Co (OH) as described in claim 12@CoMoO4The preparation method of composite nano plate, which is characterized in that the divalent
Cobalt salt is Co (NO3)2·6H2O, the sexavalence molybdate are Na2MoO4·2H2O。
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| "Construction of Hierarchical Ni(OH)2@CoMoO4 Nanoflake Composite for High-Performance Supercapacitors";Xueqing Li等;《Nano》;20160310;第11卷(第5期);第1650050:1-7页 |
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