CN106504902A - A kind of CuO@MnO2Core shell structure porous nano wire material and preparation method thereof - Google Patents
A kind of CuO@MnO2Core shell structure porous nano wire material and preparation method thereof Download PDFInfo
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- CN106504902A CN106504902A CN201610836756.9A CN201610836756A CN106504902A CN 106504902 A CN106504902 A CN 106504902A CN 201610836756 A CN201610836756 A CN 201610836756A CN 106504902 A CN106504902 A CN 106504902A
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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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- 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
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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
- H01G11/24—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
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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
-
- 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
- H01G11/46—Metal oxides
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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
- H01G11/84—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
Abstract
The invention discloses a kind of CuO@MnO2Core shell structure porous nano wire material and preparation method thereof, the CuO@MnO2The stratum nucleare of core shell structure porous nano wire material is CuO nano wires, and shell is MnO2Nanometer sheet, and CuO nano wire dense growths are in substrate, and shell MnO2Grow nonparasitically upon another plant in CuO nanowire surfaces nanometer sheet dense uniform, and crisscross, loose structure is formed in nanowire surface.Preparation process includes that aoxidizing the prepared surface length of copper mesh has the copper mesh of CuO nano wires and pass through in KMnO4It is MnO that in solution, short time hydro-thermal process forms shell on CuO nano wires2Nanometer sheet, ultimately forms CuO@MnO2Core shell structure porous nano wire material.CuO@MnO obtained in of the invention2Generate new nanotopography, it is a kind of new heterojunction structure, and causes new interface, and huge specific surface area significantly increases the avtive spot of reaction, so as to the response characteristic of the nano composite material can be lifted, its application prospect in energy storage, catalysis and sensory field is expanded.
Description
Technical field
The present invention relates to a kind of field of core-shell nano material, more particularly to a kind of oxide core shell nanometer material and its system
Preparation Method.
Background technology
The rhythm of current social development is more and more faster, and its cost is built upon in the huge consumption to the energy and resource,
Nowadays it has been realized that this rough energy resource consumption mode may caused by various problems, the such as wasting of resources, money
Source exhaustion and environmental pollution etc..Therefore, the new energy and new energy storage and occupation mode are needed badly and are developed, to solve
Certainly existing crisis.In energy storage and energy supply, traditional battery and capacitor are due to cannot provide high-energy-density and height simultaneously
Power density, thus be restricted in actual applications, and ultracapacitor has this advantage, close with high power
Degree, it may have higher energy density, simultaneously because its long service life, the advantages of effect on environment is little so that super capacitor
Device is expected to the energy stores instrument for becoming a new generation.
Used as the electrode material of ultracapacitor, it is oxide material, wherein CuO and MnO that people research and develop most at present2
Be easy to get because of raw material, low cost, environmental protection the advantages of and receive much concern.If by CuO and MnO2Nano material is combined, and is formed
Composite nanostructure, then the beneficial property can simultaneously with both oxides, while composite construction can produce new heterogeneous
Structure, causes new interface, and the multilevel hierarchy that two kinds of nanostructureds are compounded to form can produce new nanotopography, multistage knot
The bigger serface that structure has can increase the avtive spot of reaction, so as to cause a series of new cooperative effects, make full use of
These collaborations are expected to obtain better performance, obtain more preferable material.Therefore, design and prepare CuO and MnO2Both
The composite nanostructure of material, is all significant in academic research and practical application.
Content of the invention
Present invention aims to practical application request, there is provided a kind of CuO@MnO2Core shell structure porous nano wire rod
Material and preparation method thereof.
The invention provides a kind of CuO@MnO2Core shell structure porous nano wire material, described CuO@MnO2Core shell structure
Porous nano wire material includes stratum nucleare and shell two parts, and wherein stratum nucleare is CuO nano wires, and CuO nano wire dense growths are in base
On bottom, shell is MnO2Nanometer sheet, and nanometer sheet dense uniform ground grows nonparasitically upon another plant in CuO nanowire surfaces, and crisscross, in nanometer
Line surface forms loose structure.The present invention by rational microstructure design, and employing effectively synthetic method by the nano junction
Structure realizes that this multistage nanometer nuclear shell nano-structure will likely produce multiple synergies.
Further, described CuO@MnO2Core shell structure porous nano wire material, stratum nucleare CuO nanowire lengths are 5 ~ 10
μm, about 300 nm of diameter, shell MnO2The thickness of nanometer sheet about 100nm, every MnO2The thickness of nanometer sheet is 3 ~ 7nm.
Present invention also offers described CuO@MnO2The preparation method of core shell structure porous nano wire material, its step is such as
Under：
1）Prepare one piece of copper mesh, be cleaned by ultrasonic in acetone, deionized water, 1mol/L watery hydrochloric acid, deionized water successively, Ran Hou
Dry in vacuum drying chamber；
2）By step 1）The copper mesh for processing is put into tube furnace, is passed through the O of 5 ~ 25sccm2, and react under the conditions of 300 DEG C
30min, takes out copper mesh after furnace temperature natural cooling, and obtaining surface length has the copper mesh of CuO nano wires；
3）Weigh KMnO4And deionized water is dissolved in, stir to all dissolvings, then by KMnO4Solution is transferred to polytetrafluoroethylene (PTFE)
In the reactor of liner
4）By step 2）In the length that the obtains copper mesh that has CuO nano wires be immersed in the solution in reactor, be then placed into 150
0.5-1h is reacted in ~ 170 DEG C of baking oven, and reaction is taken out substrate and cleaned and dries after terminating, obtain CuO@MnO2Core shell structure is more
Hole nano-material.
The useful achievement of the present invention is：
（1）The growing method of CuO nano wires is extremely simple, it is only necessary to the copper mesh for cleaning up is placed in tube furnace and is heat-treated one
The section time, you can obtain substantial amounts of CuO nano wires, CuO@MnO2The preparation of core shell structure is also easy to realize, it is only necessary to have length
The copper mesh of CuO nano wires is in KMnO4Short time hydro-thermal process in solution, thus CuO@MnO2Core shell structure porous nano line
Material can achieve effective controllable standby.
（2）CuO@MnO of the present invention2Core shell structure porous nano wire material is a kind of composite, can have concurrently
Co3O4And MnO2The advantage of two oxides, and a series of new cooperative effects are formed, obtain more preferably combination property.
（3）CuO@MnO of the present invention2Core shell structure porous nano wire material is by CuO nano wires stratum nucleare and MnO2Nanometer
Piece shell two parts are constituted, and are grown nonparasitically upon another plant in the MnO on CuO nano-pillars surface2The crisscross formation loose structure of nanometer sheet, two kinds are received
Rice structure has been compounded to form multilevel hierarchy, generates new nanotopography, is a kind of new heterojunction structure, and causes new boundary
Face, and huge specific surface area significantly increases the avtive spot of reaction, so as to the reaction of the nano composite material can be lifted
Characteristic, expands its application prospect in energy storage, catalysis and sensory field.
（4）CuO@MnO of the present invention2Core shell structure porous nano wire material, this CuO@MnO2Core shell structure synthesis
CuO and MnO2Two kinds of electric capacity active materials, and package assembly is formed in nanoscale so that the electric capacity of two kinds of active materials is special
Property can be obtained by simultaneously, additionally, CuO@MnO2Nuclear shell structure nano line is grown directly upon on copper mesh, and copper mesh can be made then
Directly use for collector, deducted the flow process that active material in industrial production needs to be coated to collector, and because copper mesh
The composite of upper direct growth forms entirety with copper mesh, does not deposit the active material for producing in the industrial production because of coating procedure
The contact resistance problem formed between collector, therefore CuO@MnO2Core shell structure porous nano wire material is in ultracapacitor
Field is expected with unique advantage.
（5）The preparation method of the present invention includes two methods of thermal oxide and hydro-thermal method, and equipment is simple, raw materials used inexpensive,
Technique is simple and clear and easily operated, can achieve large-scale industrial production.
Description of the drawings
The low power ESEM of stratum nucleare CuO nano wires obtained in Fig. 1 embodiments 2（SEM）Figure.
The high power ESEM of stratum nucleare CuO nano wires obtained in Fig. 2 embodiments 2（SEM）Figure.
CuO@MnO obtained in Fig. 3 embodiments 22The high power ESEM of core shell structure porous nano wire material（SEM）Figure.
Specific embodiment
Below in conjunction with instantiation, the present invention is further illustrated.
Chemical raw material acetone used in following examples, hydrochloric acid, KMnO4Pure for analyzing, deionized water resistance is 18.2M
Ω.
Example 1
1）Prepare one piece of copper mesh, be cleaned by ultrasonic in acetone, deionized water, 1mol/L watery hydrochloric acid, deionized water successively, Ran Hou
Dry in vacuum drying chamber.
2）The copper mesh that step 1 was processed is put into tube furnace, the O of 5sccm is passed through2, and react under the conditions of 300 DEG C
30min, takes out copper mesh after furnace temperature natural cooling, and obtaining surface length has the copper mesh of CuO nano wires.
3）Weigh KMnO4And deionized water is dissolved in, stir to all dissolvings, then by KMnO4Solution is transferred to polytetrafluoroethyl-ne
In the reactor of alkene liner.
4）By step 2）In the length that the obtains copper mesh that has CuO nano wires be immersed in the solution in reactor, then place
0.5h is reacted in 150 DEG C of baking oven.Reaction is taken out substrate and is cleaned and dries after terminating, obtain CuO@MnO2Core shell structure porous
Nano-material.
Example 2
1）Prepare one piece of copper mesh, be cleaned by ultrasonic in acetone, deionized water, 1mol/L watery hydrochloric acid, deionized water successively, Ran Hou
Dry in vacuum drying chamber.
2）The copper mesh that step 1 was processed is put into tube furnace, the O of 15sccm is passed through2, and react under the conditions of 300 DEG C
30min, takes out copper mesh after furnace temperature natural cooling, and obtaining surface length has the copper mesh of CuO nano wires.
3）Weigh KMnO4And deionized water is dissolved in, stir to all dissolvings, then by KMnO4Solution is transferred to polytetrafluoroethyl-ne
In the reactor of alkene liner.
4）By step 2）In the length that the obtains copper mesh that has CuO nano wires be immersed in the solution in reactor, then place
0.8h is reacted in 170 DEG C of baking oven.Reaction is taken out substrate and is cleaned and dries after terminating, obtain CuO@MnO2Core shell structure porous
Nano-material.
Example 3
1）Prepare one piece of copper mesh, be cleaned by ultrasonic in acetone, deionized water, 1mol/L watery hydrochloric acid, deionized water successively, Ran Hou
Dry in vacuum drying chamber.
2）The copper mesh that step 1 was processed is put into tube furnace, leads to the O of 25sccm2, and react under the conditions of 300 DEG C
30min, takes out copper mesh after furnace temperature natural cooling, and obtaining surface length has the copper mesh of CuO nano wires.
3）Weigh KMnO4And deionized water is dissolved in, stir to all dissolvings, then by KMnO4Solution is transferred to polytetrafluoroethyl-ne
The reactor of alkene liner.
4）By step 2）In the length that the obtains copper mesh that has CuO nano wires be immersed in the solution in reactor, then place
1h is reacted in 160 DEG C of baking oven.Reaction is taken out substrate and is cleaned and dries after terminating, obtain CuO@MnO2Core shell structure porous is received
Nanowire material.
To stratum nucleare CuO nano wires obtained in each embodiment step 2 and last obtained CuO@MnO2Core shell structure porous is received
Nanowire material is scanned Electronic Speculum（SEM）Morphology analysis.As Fig. 1 and Fig. 2 is respectively stratum nucleare CuO nano wires obtained in embodiment 2
Low power and high power ESEM（SEM）Figure, as we can see from the figure：Stratum nucleare CuO be nano wire, CuO nano wire dense growths
In substrate, length is 5 ~ 10 μm, about 300 nm of diameter.If Fig. 3 is CuO@MnO obtained in embodiment 22Core shell structure porous is received
The high power ESEM of nanowire material（SEM）Figure, as seen from the figure：The MnO of shell2For nanometer sheet, and the nanometer sheet is fine and close
Grown nonparasitically upon another plant in the CuO nanowire surfaces of stratum nucleare evenly, and crisscross, loose structure is formed in nanowire surface；And shell MnO2
The thickness of nanometer sheet about 100nm, every MnO2The thickness of nanometer sheet is 3 ~ 7nm.
Claims (4)
1. a kind of CuO@MnO2Core shell structure porous nano wire material, it is characterised in that：The CuO@MnO2Core shell structure porous is received
The stratum nucleare of nanowire material is CuO nano wires, and shell is MnO2Nanometer sheet, and CuO nano wire dense growths are in substrate, and shell
Layer MnO2Grow nonparasitically upon another plant in CuO nanowire surfaces nanometer sheet dense uniform, and crisscross, porous knot is formed in nanowire surface
Structure.
2. a kind of CuO@MnO according to claim 12Core shell structure porous nano wire material, it is characterised in that：The CuO
Nanowire length is 5 ~ 10 μm, diameter about 300 nm, MnO2The thickness of nanometer sheet about 100nm, every MnO2The thickness of nanometer sheet
For 3 ~ 7nm.
3. a kind of CuO@MnO described in claim 1 or 2 are prepared2The method of core shell structure porous nano wire material, its feature exist
In including step：
1）Prepare one piece of copper mesh, be cleaned by ultrasonic in acetone, deionized water, 1mol/L watery hydrochloric acid, deionized water successively, Ran Hou
Dry in vacuum drying chamber；
2）By step 1）The copper mesh for processing is put into tube furnace, is passed through the O of 5-25sccm2, and react under the conditions of 300 DEG C
30min, takes out copper mesh after furnace temperature natural cooling, and obtaining surface length has the copper mesh of CuO nano wires；
3）Weigh KMnO4And deionized water is dissolved in, stir to all dissolvings, then by KMnO4Solution is transferred in polytetrafluoroethylene (PTFE)
In the reactor of lining；
4）By step 2）In the length that the obtains copper mesh that has CuO nano wires be immersed in the solution in reactor, be then placed into drying
React in case；Reaction is taken out substrate and is cleaned and dries after terminating, obtain CuO@MnO2Core shell structure porous nano wire material.
4. CuO@MnO according to claims 32The preparation method of core shell structure porous nano wire material, its feature exist
In：Step 4）The temperature that reacts in baking oven is 150-170 DEG C, the reaction time is 0.5-1h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107731561A (en) * | 2017-09-26 | 2018-02-23 | 四川大学 | A kind of straightforward procedure of doped metallic oxide manganese bioxide electrode material |
| CN108671923A (en) * | 2018-05-10 | 2018-10-19 | 宁波大学 | Cu oxide/cobalt/cobalt oxide catalyst with core-casing structure and preparation method thereof for electrolysis water |
| CN108956735A (en) * | 2018-05-07 | 2018-12-07 | 西北工业大学 | A kind of cobalt black of core-shell structure-copper nano-wire combination electrode material and preparation method |
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN111115690A (en) * | 2019-12-20 | 2020-05-08 | 江苏大学 | Wearable MnO2Nanowire hybrid membrane and preparation method thereof |
| CN112233907A (en) * | 2020-09-03 | 2021-01-15 | 吉林大学 | CuO/MnO2Composite nano material and preparation method thereof |
| CN112951619A (en) * | 2021-01-29 | 2021-06-11 | 多助科技(武汉)有限公司 | Iron oxide @ manganese dioxide core-shell structure material and preparation and application thereof |
-
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- 2016-09-21 CN CN201610836756.9A patent/CN106504902A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107731561A (en) * | 2017-09-26 | 2018-02-23 | 四川大学 | A kind of straightforward procedure of doped metallic oxide manganese bioxide electrode material |
| CN108956735A (en) * | 2018-05-07 | 2018-12-07 | 西北工业大学 | A kind of cobalt black of core-shell structure-copper nano-wire combination electrode material and preparation method |
| CN108956735B (en) * | 2018-05-07 | 2020-05-12 | 西北工业大学 | Cobalt monoxide-copper nanowire composite electrode material with shell-core structure and preparation method thereof |
| CN108671923A (en) * | 2018-05-10 | 2018-10-19 | 宁波大学 | Cu oxide/cobalt/cobalt oxide catalyst with core-casing structure and preparation method thereof for electrolysis water |
| CN108671923B (en) * | 2018-05-10 | 2021-06-29 | 宁波大学 | Copper oxide/cobalt oxide core-shell structure catalyst for water electrolysis and preparation method thereof |
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN110514700B (en) * | 2019-09-27 | 2021-09-07 | 西安电子科技大学 | Copper oxide and cobaltosic oxide heterostructure nanowire composite sensitive material, ethylene glycol sensor and preparation method |
| CN111115690A (en) * | 2019-12-20 | 2020-05-08 | 江苏大学 | Wearable MnO2Nanowire hybrid membrane and preparation method thereof |
| CN111115690B (en) * | 2019-12-20 | 2022-04-26 | 江苏大学 | Wearable MnO2Nanowire hybrid membrane and preparation method thereof |
| CN112233907A (en) * | 2020-09-03 | 2021-01-15 | 吉林大学 | CuO/MnO2Composite nano material and preparation method thereof |
| CN112951619A (en) * | 2021-01-29 | 2021-06-11 | 多助科技(武汉)有限公司 | Iron oxide @ manganese dioxide core-shell structure material and preparation and application thereof |
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