CN107731550A - A kind of metal oxide/graphene composite material and its preparation method and application - Google Patents
A kind of metal oxide/graphene composite material and its preparation method and application Download PDFInfo
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- CN107731550A CN107731550A CN201711095948.XA CN201711095948A CN107731550A CN 107731550 A CN107731550 A CN 107731550A CN 201711095948 A CN201711095948 A CN 201711095948A CN 107731550 A CN107731550 A CN 107731550A
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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
- H01M4/362—Composites
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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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- 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
- 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
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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 functionalized nano field of material technology, is related to a kind of metal oxide/graphene composite material and its preparation method and application.Graphite, the concentrated sulfuric acid and sodium nitrate are mixed, the above-mentioned mixed liquor of potassium permanganate addition is weighed and continues to stir；Distilled water diluting stirring is added under ice-water bath；Add H2O2The aqueous solution stirs；Washed repeatedly with distilled water to neutrality, collect graphene oxide sample.Metal simple-substance is placed in graphene oxide water solution, room temperature collects the black solid product of washing generation after placing, metal oxide/graphene complex is obtained after freeze-drying.The inventive method is easy to operate, preparation condition is gentle, raw material are cheap and easy to get, and product is good as lithium ion battery negative material chemical property.It can also be applied to the fields such as solar cell, gas sensor, light emitting diode, laser diode, ultracapacitor, spin electric device, UV-detector, field-effect transistor, photocatalysis treatment sewage.
Description
Technical field
The invention belongs to functionalized nano field of material technology, be related to a kind of metal oxide/graphene composite material and
Its preparation method and application.
Background technology
The Colloidal particles that graphene is made up of monolayer carbon, it is the high-density raw sublayer that sp2 hydbridized carbon atoms are formed
The honeycomb network structure of arrangement form.Since first time in 2004 is reported, graphene is such as excellent just with its unique performance
Charge carrier mobility, the high grade of transparency, excellent pliability, outstanding electron mass and superior heating power and mechanical performance
The extensive concern of scientific circles is attracted.Graphene has the special Young mould of higher mechanical strength (＞ 1060GPa) and 1TPa
Amount.In addition, single-layer graphene is the most strong material tested since the dawn of human civilization, it also shows excellent hot property (≈ 5000W
m-1·K-1), electrical conductivity (up to 6000Scm-1) and high theoretical specific surface area (2630m2·g-1).These advantages are all graphite
The potential application of alkene provides wide prospect, in many technical fields, such as nanoelectronic, hydrogen storage, ultracapacitor and sensing
It can all be applied in device.Although graphene has many good performances, it also has special property, due between graphene layer
Van der Waals interact and stack and limit its application in every field.This shortcoming can pass through graphene and nanometer
Grain is compound to be eliminated.
In in the past few decades, the synthesis of nano transition metal oxides (TMO NPs) material causes extensive pass
Note, it has shape, size, crystallinity and function controllable, and good ecological environment is corrosion-resistant, and easily extension and relative cost benefit etc. is excellent
Point.Particularly, in all TMO NPs materials, titanium dioxide, manganese oxide, iron oxide and zinc oxide are with its unique performance
Received much concern with attribute.By changing the reaction condition in building-up process, as reaction time, reaction temperature and presoma are dense
Degree, TMO NPs form and size can be optimized, so as to make it have different particular features.These materials electronic product,
The fields such as optics, electrochemistry, solar energy acquisition suffer from being widely applied.In order to further improve their performance, can make
TMO NPs and graphene are compound so as to prepare composite, so that some shortcomings in TMO NPs are offset by graphene.
Prepare Fe2O3/ graphene composite material, usual way are used containing molysite as precursor, are gone back by using all kinds of
Former agent, redox graphene (RGO) prepared by graphene oxide (GO) using hydro-thermal method.These methods be typically it is complicated and
High cost.Metallic iron also has in acid condition in addition to the characteristics of stronger reproducibility, rich content and environmental protection
The characteristics of reducing GO.In addition, metallic iron is also the preferable presoma of ferriferous oxide.In the present invention, by room temperature using low
Cost feedstocks, γ-Fe are expeditiously prepared with simple one kettle way2O3/ RGO composites, wherein metallic iron as reducing agent and
γ-Fe2O3The presoma of nano particle.As a result show, γ-Fe2O3/ RGO samples show good form and structure, the sample
The negative material that product are used as lithium ion battery illustrates good cycle performance and high rate performance.
The method of the invention, which is removed, is applied to γ-Fe2O3Outside the preparation of/RGO composites, zinc, magnesium, aluminium etc. are applied also for
The preparation of other metal oxide/graphene composite materials.Metal oxide/graphene composite material prepared by this method removes
It is outer in field of lithium ion battery application, apply also for solar cell, gas sensor, light emitting diode, laser diode,
The fields such as ultracapacitor, spin electric device, UV-detector, field-effect transistor, photocatalysis treatment sewage.
The content of the invention
It is a primary object of the present invention to provide a kind of metal oxide/graphene composite material and preparation method thereof and answer
With.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of metal oxide/graphene composite material, comprises the following steps：
Step (1)：Graphite, the concentrated sulfuric acid and sodium nitrate are mixed to obtain mixed liquor；
Step (2)：The mixed liquor that potassium permanganate is added obtained by step (1) is weighed to continue to stir；
Step (3)：Distilled water diluting stirring is added under ice-water bath into step (2) resulting solution；
Step (4)：Aqueous hydrogen peroxide solution stirring is added to step (3) resulting solution；
Step (5)：The bottom sediment thing and supernatant liquor in mixture obtained by removing step (4) are centrifuged, in collection
Interbed light color product, washed repeatedly with distilled water to neutrality, it is standby to collect GO；
Step (6)：Metal simple-substance is placed in the GO suspension after dilution, room temperature collects washing life after placing a period of time
Into black solid product, obtain metal oxide/graphene composite material after freeze-drying.
Metal simple-substance described in step (6) is one kind in metallic iron, metallic zinc, metallic aluminium, magnesium metal.
Graphite 5.0g, 98% concentrated sulfuric acid 120mL, sodium nitrate 2.5g are mixed into 30min in step (1).
The potassium permanganate added in step (2) is 15g, mixing time 24h.
The distilled water added in step (3) is 150mL, mixing time 24h.
The hydrogenperoxide steam generator added in step (4) is 50mL, 30wt%, mixing time 24h.
A kind of metal oxide/graphene composite material prepared such as above-mentioned method.
A kind of application of metal oxide/graphene composite material in lithium ion battery negative material.
A kind of metal oxide/graphene composite material solar cell, gas sensor, light emitting diode,
In laser diode, ultracapacitor, spin electric device, UV-detector, field-effect transistor or photocatalysis treatment sewage
Application.
The invention has the advantages that：
Process existing in terms of for metal oxide in the prior art/graphene complex technology of preparing is complicated, cost
The shortcomings of higher, severe reaction conditions, the present invention provide a kind of preparation method of metal oxide/graphene composite material, should
Method is easy to operate, preparation condition is gentle, raw material are cheap and easy to get, and product is as lithium ion battery negative material chemical property
Well.
Brief description of the drawings
Fig. 1 is γ-Fe2O3/ RGO powder X ray diffracting spectrum (XRD and compareed with standard substance PDF cards)；
The powder X ray diffracting spectrum (XRD and compareed with standard substance PDF cards) that Fig. 2 is ZnO/RGO；
Fig. 3 is γ-Fe2O3/ RGO circulating battery figure；
Fig. 4 is γ-Fe2O3/ RGO high rate performance figure；
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
Embodiment 1
5.0g graphite, the 120mL98% concentrated sulfuric acids and 2.5g sodium nitrate are mixed into 30min, 15g potassium permanganate is weighed and adds
Enter above-mentioned mixed liquor to continue to stir 24h；150mL distilled water dilutings stirring 24h is added under ice-water bath；Add 50mL 30wt%'s
H2O2The aqueous solution stirs 24h；The bottom black bulk sediment and supernatant liquor removed in gained mixture is centrifuged, is received
Collect intermediate layer light color product, washed repeatedly with distilled water to neutrality, it is standby to collect GO suspension (3mg/mL).
GO suspension (25.0mL, 1.0mg/mL) after dilution is transferred in 25mL sample bottles.By fritter rectangle iron plate
It is positioned over after ultrasonic wave cleans 30min, absolute ethyl alcohol washing in sample bottle.After 24h, yellowish brown suspension becomes transparent, obtains
To the block black solid being attached on iron plate.Black solid is collected, is washed 2 times with ethanol, deionized water is washed 2 times.Freezing
After drying, γ-Fe are obtained2O3/RGO。
Embodiment 2
5.0g graphite, the 120mL98% concentrated sulfuric acids and 2.5g sodium nitrate are mixed into 30min, 15g potassium permanganate is weighed and adds
Enter above-mentioned mixed liquor to continue to stir 24h；150mL distilled water dilutings stirring 24h is added under ice-water bath；Add 50mL 30wt%'s
H2O2The aqueous solution stirs 24h；The bottom black bulk sediment and supernatant liquor removed in gained mixture is centrifuged, is received
Collect intermediate layer light color product, washed repeatedly with distilled water to neutrality, it is standby to collect GO suspension (3mg/mL).
GO suspension (25.0mL, 1.0mg/mL) after dilution is transferred in 25mL sample bottles.By fritter rectangle zinc metal sheet
It is positioned over after ultrasonic wave cleans 30min, absolute ethyl alcohol washing in sample bottle.After 24h, yellowish brown suspension becomes transparent, obtains
To the block black solid being attached on zinc metal sheet.Black solid is collected, is washed 2 times with ethanol, deionized water is washed 2 times.Freezing
After drying, ZnO/RGO is obtained.
Embodiment 3
5.0g graphite, the 120mL98% concentrated sulfuric acids and 2.5g sodium nitrate are mixed into 30min, 15g potassium permanganate is weighed and adds
Enter above-mentioned mixed liquor to continue to stir 24h；150mL distilled water dilutings stirring 24h is added under ice-water bath；Add 50mL 30wt%'s
H2O2The aqueous solution stirs 24h；The bottom black bulk sediment and supernatant liquor removed in gained mixture is centrifuged, is received
Collect intermediate layer light color product, washed repeatedly with distilled water to neutrality, it is standby to collect GO suspension (3mg/mL).
GO suspension (25.0mL, 1.0mg/mL) after dilution is transferred in 25mL sample bottles.By fritter rectangle aluminium flake
It is positioned over after ultrasonic wave cleans 30min, absolute ethyl alcohol washing in sample bottle.After 24h, yellowish brown suspension becomes transparent, obtains
To the block black solid being attached on zinc metal sheet.Black solid is collected, is washed 2 times with ethanol, deionized water is washed 2 times.Freezing
After drying, Al is obtained2O3/RGO。
Embodiment 4
5.0g graphite, the 120mL98% concentrated sulfuric acids and 2.5g sodium nitrate are mixed into 30min, 15g potassium permanganate is weighed and adds
Enter above-mentioned mixed liquor to continue to stir 24h；150mL distilled water dilutings stirring 24h is added under ice-water bath；Add 50mL 30wt%'s
H2O2The aqueous solution stirs 24h；The bottom black bulk sediment and supernatant liquor removed in gained mixture is centrifuged, is received
Collect intermediate layer light color product, washed repeatedly with distilled water to neutrality, it is standby to collect GO suspension (3mg/mL).
GO suspension (25.0mL, 1.0mg/mL) after dilution is transferred in 25mL sample bottles.By fritter rectangle magnesium sheet
It is positioned over after ultrasonic wave cleans 30min, absolute ethyl alcohol washing in sample bottle.After 24h, yellowish brown suspension becomes transparent, obtains
To the block black solid being attached on magnesium sheet.Black solid is collected, is washed 2 times with ethanol, deionized water is washed 2 times.Freezing
After drying, MgO/RGO is obtained.
Fig. 1 is γ-Fe2O3/ RGO powder X ray diffracting spectrum (XRD and compareed with standard substance PDF cards), from γ-
Fe2O3It can be seen that, stacked in multi-layers is derived from the broad peak about in 2 θ=25.6 ° in/RGO powder X ray diffracting spectrum
RGO, in 2 θ=30.2 °, 35.6 °, 43.3 °, 57.3 ° and 62.8 ° of spike corresponds respectively to γ-Fe2O3(220), (311),
(400), (511) and (440) diffraction crystal face, this and standard gamma-Fe2O3(JCPDS#39-1346) characteristic peak matches, so as to
It is RGO and γ-Fe to demonstrate product2O3Compound.
The powder X ray diffracting spectrum (XRD and compareed with standard substance PDF cards) that Fig. 2 is ZnO/RGO, from ZnO/RGO
Powder X ray diffracting spectrum in it can be seen that, the RGO of stacked in multi-layers is derived from the broad peak about in 2 θ=25.6 °, in 2 θ
=31.7 °, 34.4 °, 36.3 °, 47.6 °, 56.6 °, 62.9 °, 66.3 °, 67.9 °, 69.1 ° and 72.7 ° of spike corresponds to respectively
In ZnO (100), (002), (101), (102), (110), (103), (200), (112), (201) and (004) diffraction crystal face
This matches with the characteristic peak of standard ZnO (JCPDS#36-1451), so as to demonstrate the compound that product is RGO and ZnO.
Fig. 3 is γ-Fe2O3/ RGO is 1000mAg in current density as lithium ion battery negative material-1Under pass through 300
The cycle performance figure of secondary discharge and recharge；Fig. 4 is γ-Fe2O3The high rate performance figures of/RGO as lithium ion battery negative material.From figure
In as can be seen that γ-Fe2O3/ RGO possesses good cycle performance and high rate performance as lithium ion battery negative material.
Claims (9)
1. a kind of preparation method of metal oxide/graphene composite material, it is characterised in that comprise the following steps：
Step (1)：Graphite, the concentrated sulfuric acid and sodium nitrate are mixed to obtain mixed liquor；
Step (2)：The mixed liquor that potassium permanganate is added obtained by step (1) is weighed to continue to stir；
Step (3)：Distilled water diluting stirring is added under ice-water bath into step (2) resulting solution；
Step (4)：Aqueous hydrogen peroxide solution stirring is added to step (3) resulting solution；
Step (5)：The bottom sediment thing and supernatant liquor in mixture obtained by removing step (4) are centrifuged, collects intermediate layer
Light product, washed repeatedly with distilled water to neutrality, it is standby to collect GO；
Step (6)：Metal simple-substance is placed in the GO suspension after dilution, room temperature collects washing generation after placing a period of time
Black solid product, metal oxide/graphene composite material is obtained after freeze-drying.
2. preparation method according to claim 1, it is characterised in that metal simple-substance described in step (6) is metallic iron, gold
Belong to one kind in zinc, metallic aluminium, magnesium metal.
3. preparation method according to claim 1 or 2, it is characterised in that by graphite 5.0g, 98% dense sulphur in step (1)
Sour 120mL, sodium nitrate 2.5g mix 30min.
4. preparation method according to claim 1 or 2, it is characterised in that the potassium permanganate added in step (2) is 15g,
Mixing time is 24h.
5. preparation method according to claim 1 or 2, it is characterised in that the distilled water added in step (3) is 150mL,
Mixing time is 24h.
6. preparation method according to claim 1 or 2, it is characterised in that the hydrogenperoxide steam generator of addition is in step (4)
50mL, 30wt%, mixing time 24h.
A kind of 7. metal oxide/graphene composite material prepared such as claim 1-6 methods describeds.
A kind of 8. answering in lithium ion battery negative material of metal oxide/graphene composite material as claimed in claim 7
With.
9. a kind of metal oxide/graphene composite material as claimed in claim 7 is in solar cell, gas sensor, hair
At optical diode, laser diode, ultracapacitor, spin electric device, UV-detector, field-effect transistor or photocatalysis
Manage the application in sewage.
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Cited By (5)
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| CN108622885A (en) * | 2018-07-06 | 2018-10-09 | 青岛大学 | A kind of preparation method of graphene film |
| CN108666555A (en) * | 2018-05-25 | 2018-10-16 | 北京理工大学 | A kind of multistage γ-Fe2O3The preparation method of/C nano piece negative material |
| CN108823601A (en) * | 2018-07-06 | 2018-11-16 | 青岛大学 | A kind of preparation method of metal oxide/graphene composite film |
| CN108949102A (en) * | 2018-07-20 | 2018-12-07 | 青岛大学 | A kind of nano zine oxide/graphene composite material and preparation method thereof |
| CN109741974A (en) * | 2019-02-28 | 2019-05-10 | 重庆文理学院 | A kind of flexible compound film and preparation method thereof for supercapacitor |
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| CN109741974A (en) * | 2019-02-28 | 2019-05-10 | 重庆文理学院 | A kind of flexible compound film and preparation method thereof for supercapacitor |
| CN109741974B (en) * | 2019-02-28 | 2020-09-01 | 重庆文理学院 | Flexible composite film for super capacitor and preparation method thereof |
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Application publication date: 20180223 |