CN103862751A - Method for preparing composite nano film - Google Patents
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- CN103862751A CN103862751A CN201410061492.5A CN201410061492A CN103862751A CN 103862751 A CN103862751 A CN 103862751A CN 201410061492 A CN201410061492 A CN 201410061492A CN 103862751 A CN103862751 A CN 103862751A
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Abstract
The embodiment of the invention discloses a method for preparing a composite nano film. The method for preparing the composite nano film comprises the following steps: depositing a graphene oxide/ferric ion/nano ion composite LB membrane by adopting an LB film method; then reducing a ferrum ion into an oxidizing agent by a chemical method; then acquiring a conductive polymer layer on the oxidizing agent layer by adopting a chemical vapor phase polymerization method; finally, reducing oxidized graphene into reduction-oxidation graphene, thereby obtaining a composite nano film. The composite nano electrode prepared by the method is a reduction-oxidation graphene/conductive polymer/nano particle composite nano film, and has wide application in the aspect of high-specific-volume electrode and gas sensitive materials.
Description
Technical field
The present invention relates to nano film material technical field, especially relate to a kind of method of manufacturing composite nano film.
Background technology
Organic-inorganic nanocomposite is the important topic that in nanosecond science and technology field has basic research and using value.This material is combined in nanometer range by inorganic phase and organic phase, exists more by force or weak chemical bond between two-phase interface.After Organic-inorganic materials hybrid, can obtain the new material of the many characteristics that integrate inorganic, organic, nano particle.These new materials have new application in fields such as photoelectricity, heat, biology, environmental protection.
Utilizing nano material to carry out to polymer the polymer base inorganic nano-composite material that modification has a nano functional characteristic with exploitation is one of focus of polymeric material field research.It is functionalization and the large key factor of high performance two that realizes polymer based nanocomposites that the dispersed and inorganic nano-particle of nano material in polymeric matrix is combined with the excellent interface of polymeric matrix.Composite material interface is the very important microstructure of composite, and the character at interface directly affects the properties of composite.
The conducting polymer of nanostructured, as polyaniline, polypyrrole etc., has electricity and electro-chemical activity concurrently, aspect high-capacity electrochemical electrode and sensor sensing material, is being widely used.But mostly there is unstable properties in current conducting polymer, the imperfect shortcoming of mechanical performance.Graphene rich surface contains oxy radical, specific area is high, the interior electric conductivity of face is good and mechanical property is excellent, and suitable Graphene-conducting polymer combination electrode material of preparing is used as high performance electrochemical electrode and sensor sensing material.But how to realize conducting polymer mate with the good interface of grapheme material, and can effectively to introduce the cooperative effect that other inorganic nano structural material strengthens each component be to manufacture the key factor of high-performance inorganic-organic composite nanostructured.
Summary of the invention
One of object of the present invention is to provide a kind of method of manufacturing composite nano film, the composite of the composite nano film that wherein the method is manufactured based on redox graphene, conducting polymer and nano particle, by the good synergy between three, give full play to the advantage of each component, thereby having a good application prospect aspect Fabrication of High Specific Capacitance combination electrode and composite gas sensitive material.
Technical scheme disclosed by the invention comprises:
A kind of method of manufacturing composite nano film is provided, has it is characterized in that, having comprised: carboxylated graphene oxide and nano particle have been scattered in organic solvent, obtain carboxylated graphene oxide and nanoparticle dispersion liquid; At least a portion of described carboxylated graphene oxide and nanoparticle dispersion liquid is spread in to the iron content deionized water solution surface in LB film groove, form graphene oxide/ferric ion/Nanocomposites nano thin-film on described ferric chloride aqueous solutions surface; With LB become embrane method at least a portion of described graphene oxide/ferric ion/Nanocomposites nano thin-film is transferred to substrate surface; Ferric ion in described graphene oxide/ferric ion/Nanocomposites nano thin-film is replaced into ferric trichloride, obtains graphene oxide/ferric trichloride/Nanocomposites nano thin-film; Described graphene oxide/ferric trichloride/Nanocomposites nano thin-film is carried out to chemical gaseous phase aggregation deposition in conducting polymer monomer atmosphere, obtain graphene oxide/conducting polymer/Nanocomposites nano thin-film; Graphene oxide in described graphene oxide/conducting polymer/Nanocomposites nano thin-film is reduced to redox graphene, obtains redox graphene/conducting polymer/Nanocomposites nano thin-film.
In one embodiment of the invention, the described step that graphene oxide in described graphene oxide/conducting polymer/Nanocomposites nano thin-film is reduced to redox graphene comprises: described graphene oxide/conducting polymer/Nanocomposites nano thin-film is placed in to hydrazine hydrate and reduces.
In one embodiment of the invention, described nano particle is nm of gold, Nano Silver and/or nano titanium oxide.
In one embodiment of the invention, described conducting polymer monomer is aniline, thiophene or 3,4-rthylene dioxythiophene.
In one embodiment of the invention, described substrate is tin indium oxide or aluminium foil.
In one embodiment of the invention, described organic solvent is the deionized water solution of formamide or n-butanol.
In one embodiment of the invention, the described step that ferric ion in described graphene oxide/ferric ion/Nanocomposites nano thin-film is replaced into ferric trichloride comprises: described graphene oxide/ferric ion/Nanocomposites nano thin-film is placed in to hydrogen chloride gas environment and reacts.
In one embodiment of the invention, in described carboxylated graphene oxide and nanoparticle dispersion liquid, the concentration of described hydroxylating graphene oxide is 10 mg/ml to 20 mg/ml, and the concentration of described nano particle is 1 mg/ml to 5 mg/ml.
In one embodiment of the invention, in described ferric chloride aqueous solutions, the concentration of ferric trichloride is 2 mol/L to 4 mol/L.
In the method for the manufacture composite nano film that the embodiment of the present invention provides, adopt a kind of MULTILAYER COMPOSITE nanostructured, comprise redox graphene, conducting polymer, nano particle, by the good cooperative effect between c-based nanomaterial, conducting polymer and nano particle, can greatly increase the specific area in composite nano film; In addition, the many components in composite nano film can be realized the sensitivity to multiple gases, realize the high selectivity to gas response.Therefore this composite nano film is all having a good application prospect aspect Fabrication of High Specific Capacitance electrode and gas sensitive material.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the method for the manufacture composite nano film of one embodiment of the invention.
Fig. 2 is the schematic diagram that is deposited on the composite nano film structure of the manufacture of method according to an embodiment of the invention of flexible ITO.
Detailed description of the invention
Describe the concrete steps of the method for the manufacture composite nano film of embodiments of the invention in detail below in conjunction with accompanying drawing.
As shown in Figure 1, in one embodiment of the present of invention, a kind of method of manufacturing composite nano film comprises step 10, step 12, step 14 and step 16.
Step 10:LB embrane method is prepared graphene oxide/ferric ion/Nanocomposites nano thin-film.
In the method for embodiments of the invention, first carboxylated graphene oxide and nano particle are scattered in organic solvent, to obtain graphene oxide and nanoparticle dispersion liquid, are beneficial to it and sprawl at gas/liquid interface.
In embodiments of the invention, nano particle can be nm of gold, Nano Silver and/or nano titanium oxide.That is, in embodiments of the invention, these nanoparticle can be used separately, also can be wherein at least two kinds or all use simultaneously.
In embodiments of the invention, organic solvent can be formamide/deionized water solution or n-butanol/deionized water solution.
In embodiments of the invention, the concentration of carboxylated graphene oxide in organic solvent can be 10 mg/ml (mg/ml) to 20 mg/ml (mg/ml), the concentration of nano particle in organic solvent can be that 1 mg/ml (mg/ml) is to 5 mg/ml (mg/ml).
In embodiments of the invention, can use LB film-forming apparatus to form the film needing.In the LB film groove of LB film-forming apparatus, the aqueous solution can be ferric chloride aqueous solutions (for example, the deionized water solution of ferric trichloride).
In step 10, at least a portion of carboxylated graphene oxide and nanoparticle dispersion liquid is spread in to the surface of the iron content deionized water solution in the LB film groove of LB film-forming apparatus, thus on this iron content deionized water solution surface (being the gas/liquid interface in LB film groove) upper one deck graphene oxide/ferric ion/Nanocomposites nano thin-film that forms.
In one embodiment of the present of invention, this iron content deionized water solution can be ferric chloride aqueous solutions or toluene sulfonic acide molten iron solution, can be also other solution containing iron ion being applicable to.
In one embodiment of the present of invention, in this ferric chloride aqueous solutions, the concentration of ferric trichloride can be that 2 mol/L (mol/l) are to 4 mol/L (mol/l).Ferric ion in solution can produce electrostatic interaction with the carboxyl that ionizes in graphene oxide.
Formed graphene oxide/ferric ion/Nanocomposites nano thin-film in LB film groove after, in step 10, can use LB to become embrane method that the graphene oxide/ferric ion/Nanocomposites nano thin-film in LB film groove is transferred on applicable substrate.
For example, in an embodiment, can control sliding barrier compressed oxygen functionalized graphene/ferric ion/Nanocomposites nano thin-film of LB film-forming apparatus, and adopt the mode of vertical film forming that at least a portion of this graphene oxide/ferric ion/Nanocomposites nano thin-film is transferred to substrate surface.
In embodiments of the invention, substrate can be tin indium oxide (ITO) (flexible ITO) or aluminium foil.
In the other embodiment of the present invention, above-mentioned steps 10 can be repeatedly, thereby on substrate, form multilayer graphene oxide/ferric ion/Nanocomposites nano thin-film basal body structure.
Here, the concrete structure of LB film-forming apparatus can become the structure of membrane structure identical with LB conventional in this area, is not described in detail in this.
Step 12: chemical method is prepared graphene oxide/ferric trichloride/Nanocomposites nano thin-film
On substrate, form after graphene oxide/ferric ion/Nanocomposites nano thin-film, in step 12, ferric ion in this composite nano film is replaced into ferric trichloride, obtain graphene oxide/ferric trichloride/Nanocomposites nano thin-film, thereby make this composite nano film there is certain oxidation characteristic, be beneficial to the polymerization of follow-up conducting polymer monomer.
In an embodiment of the present invention, step 12 can be used chemical method to complete.For example, in an embodiment, can be for for example, to react being placed in the substrate of graphene oxide/ferric ion/Nanocomposites nano thin-film in hydrogen chloride gas environment (, the closed environment that contains hydrogen chloride gas), thus ferric ion is become to ferric trichloride.
Step 14: adopt chemical gaseous phase aggregation deposition method to prepare graphene oxide/ferric trichloride/Nanocomposites nano thin-film.
On substrate, the ferric ion in graphene oxide/ferric ion/Nanocomposites nano thin-film is become after ferric trichloride, in step 14, graphene oxide/ferric trichloride/Nanocomposites nano thin-film is carried out to chemical gaseous phase aggregation deposition in conducting polymer monomer atmosphere, thereby obtain graphene oxide/conducting polymer/Nanocomposites nano thin-film.
In embodiments of the invention, the conducting polymer monomer in step 14 can be aniline, thiophene or 3,4 ethene dioxythiophenes etc.Correspondingly, the conducting polymer in graphene oxide/conducting polymer/Nanocomposites nano thin-film can be polyaniline, polythiophene or poly-3,4-rthylene dioxythiophene, etc.
Step 16: graphene oxide is reduced to redox graphene
In composite nano film, obtain after conducting polymer, in step 16, graphene oxide in graphene oxide/conducting polymer/Nanocomposites nano thin-film is reduced to redox graphene, thereby obtains redox graphene/conducting polymer/Nanocomposites nano thin-film.For example, in an embodiment, adopt hydrazine hydrate to process the graphene oxide/conducting polymer/Nanocomposites nano thin-film obtaining, being placed in hydrazine hydrate by graphene oxide/conducting polymer/Nanocomposites nano thin-film reduces, thereby graphene oxide is wherein reduced to redox graphene, make film there is good electric conductivity, and there is good MULTILAYER COMPOSITE nanostructured
Particularly, in one embodiment of the present of invention, a kind of concrete steps of the method for manufacturing composite nano film are as follows:
1. carboxylated graphene oxide and nano particle are scattered in n-butanol/deionization solution, the concentration of carboxylated graphene oxide material is 10-20mg/ml, and the concentration of nanometer particle material is carboxylated graphene oxide and the nano silver dispersion that 1-5mol/ml is formed for LB film preparation;
2. adopt microsyringe to extract the 1. middle nano structural material dispersion liquid obtaining of 500-1200 μ l, be added on respectively the ferric trichloride/deionized water surface in two grooves of LB film device, carboxylated graphene oxide and nano particle sprawl and form orderly layer (film) at gas/liquid interface;
3. control the sliding barrier of LB film device and compress respectively carboxylated graphene oxide film and film of nanoparticles to mould 18-25 MN/m (mN/m) and 12-25 MN/m (mN/m) with the speed of 0.5-1 mm/min (mm/min), the mode of the horizontal film forming of employing is alternately transferred to carboxylated graphene oxide/ferric ion and nano particle on substrate, and rate of film build is 0. 05 ~ 0.1 mm/min (mm/min);
4. the substrate that has deposited graphene oxide/ferric ion/film of nanoparticles is placed in to the closed environment that contains hydrogen chloride gas, the processing time is 60-80 minute;
5. the substrate 4. obtaining is inserted in the atmosphere that contains conducting polymer monomer, adopt chemical gaseous phase aggregation deposition method to obtain conductive polymer coating;
6. the substrate 5. obtaining is inserted in hydrazine hydrate, graphene oxide is reduced to redox graphene.
By 1.-6. step has obtained a kind of Fabrication of High Specific Capacitance electrode film of redox graphene/conducting polymer/nano particle.
Several concrete examples below.
Example 1:
1. carboxylated graphene oxide and Nano Silver are scattered in n-butanol/deionization solution, the concentration of carboxylated graphene oxide is 16mg/ml, and the concentration of Nano Silver is 3mol/ml, is formed for graphene oxide and the nano silver dispersion of LB film preparation;
2. adopt microsyringe to extract carboxylated graphene oxide and Nano silver solution that 1. 800 μ l obtain, be added on respectively ferric trichloride/deionized water surface in LB film groove, the concentration of ferric trichloride is 3 mol/L (mol/l), and order thin film is sprawled and formed to carboxylated graphene oxide and Nano Silver at gas/liquid interface;
3. control the sliding barrier of LB film device and compress respectively carboxylated graphene oxide film and nanometer silverskin to mould 20 mN/m and 17mN/m with the speed of 1 mm/min, the mode that employing replaces horizontal film forming is transferred to carboxylated graphene oxide/ferric ion/nanometer silverskin on substrate, and rate of film build is 0.06 mm/min;
4. the substrate that has deposited carboxylated graphene oxide/ferric ion/nanometer silverskin is placed in to hydrogen chloride gas closed environment, the processing time is 60 minutes.
5. the airtight cavity that the substrate 4. obtaining is placed in to thiophene atmosphere carries out chemical vapour deposition (CVD).
6. the substrate 5. obtaining is placed in to hydrazine hydrate, graphene oxide is reduced to redox graphene.
By 1.-6. step has obtained a kind of composite nano film of redox graphene/polythiophene/Nano Silver.
Example 2:
In example 2, metal nanoparticle is nm of gold, similar in all the other materials and manufacturing process and enforcement 1, thereby obtains the composite nano film of redox graphene/polythiophene/nm of gold.
Example 3:
In example 3, nano particle is nano titanium oxide, similar in all the other materials and manufacturing process and enforcement 1, thereby obtains the composite nano film of redox graphene/polythiophene/nano titanium oxide.
Example 4:
In example 4, conducting polymer is for poly-3,4-rthylene dioxythiophene, similar in all the other materials and manufacturing process and enforcement 1, thereby obtains the composite nano film of redox graphene/poly-3,4-rthylene dioxythiophene/Nano Silver.
Example 5:
In example 5, conducting polymer is polyaniline, similar in all the other materials and manufacturing process and enforcement 1, thereby obtains the composite nano film of redox graphene/polyaniline/Nano Silver.
Example 6:
In example 6, conducting polymer is polyaniline, and nano particle is nano titanium oxide, similar in all the other materials and manufacturing process and enforcement 1, thereby obtains the composite nano film of redox graphene/polyaniline/nano titanium oxide.
In the method for the manufacture composite nano film that the embodiment of the present invention provides, adopt a kind of MULTILAYER COMPOSITE nanostructured, comprise redox graphene, conducting polymer, nano particle, by the good cooperative effect between c-based nanomaterial, conducting polymer and nano particle, can greatly increase the specific area in composite nano film.This good structural stability derives from LB film deposition has increased the degree of coupling between each component greatly.In addition, the many components in composite nano film can be realized the sensitivity to multiple gases, realize the high selectivity to gas response.Therefore this composite nano film is all having a good application prospect aspect Fabrication of High Specific Capacitance electrode and gas sensitive material.And this manufacture method is rationally simple, easy operating.
The laminated film of the method manufacture of embodiments of the invention can be realized large area deposition, and can be prepared in flexible substrates surface and realize the manufacture of flexible electrode and sensitive thin film.
For example, as shown in Figure 2, wherein 1 is flexible ITO to the schematic diagram that composite nano film made according to the method for the present invention is prepared in flexible ITO electrode film, and 2 is redox graphene, and 3 is nano particle, and 4 is conducting polymer.
Describe the present invention by specific embodiment above, but the present invention is not limited to these specific embodiments.It will be understood by those skilled in the art that and can also make various amendments to the present invention, be equal to replacement, change etc., these conversion, all should be within protection scope of the present invention as long as do not deviate from spirit of the present invention.In addition, " embodiment " described in above many places represents different embodiment, can certainly be by its all or part of combination in one embodiment.
Claims (10)
1. a method of manufacturing composite nano film, is characterized in that, comprising:
Carboxylated graphene oxide and nano particle are scattered in organic solvent, obtain carboxylated graphene oxide and nanoparticle dispersion liquid;
At least a portion of described carboxylated graphene oxide and nanoparticle dispersion liquid is spread in to the iron content deionized water solution surface in LB film groove, form graphene oxide/ferric ion/Nanocomposites nano thin-film on described iron content deionized water solution surface;
With LB become embrane method at least a portion of described graphene oxide/ferric ion/Nanocomposites nano thin-film is transferred to substrate surface;
Ferric ion in described graphene oxide/ferric ion/Nanocomposites nano thin-film is replaced into ferric trichloride, obtains graphene oxide/ferric trichloride/Nanocomposites nano thin-film;
Described graphene oxide/ferric trichloride/Nanocomposites nano thin-film is carried out to chemical gaseous phase aggregation deposition in conducting polymer monomer atmosphere, obtain graphene oxide/conducting polymer/Nanocomposites nano thin-film;
Graphene oxide in described graphene oxide/conducting polymer/Nanocomposites nano thin-film is reduced to redox graphene, obtains redox graphene/conducting polymer/Nanocomposites nano thin-film.
2. the method for claim 1, it is characterized in that, the described step that graphene oxide in described graphene oxide/conducting polymer/Nanocomposites nano thin-film is reduced to redox graphene comprises: described graphene oxide/conducting polymer/Nanocomposites nano thin-film is placed in to hydrazine hydrate and reduces.
3. the method for claim 1, is characterized in that: described nano particle is nm of gold, Nano Silver and/or nano titanium oxide.
4. the method for claim 1, is characterized in that: described conducting polymer monomer is aniline, thiophene or 3,4-rthylene dioxythiophene.
5. the method for claim 1, is characterized in that: described substrate is tin indium oxide or aluminium foil.
6. the method for claim 1, is characterized in that: described organic solvent is the deionized water solution of formamide or n-butanol.
7. the method as described in any one in claim 1 to 6, it is characterized in that, the described step that ferric ion in described graphene oxide/ferric ion/Nanocomposites nano thin-film is replaced into ferric trichloride comprises: described graphene oxide/ferric ion/Nanocomposites nano thin-film is placed in to hydrogen chloride gas environment and reacts.
8. the method for claim 1, it is characterized in that: in described carboxylated graphene oxide and nanoparticle dispersion liquid, the concentration of described hydroxylating graphene oxide is 10 mg/ml to 20 mg/ml, and the concentration of described nano particle is 1 mg/ml to 5 mg/ml.
9. method as claimed in any of claims 1 to 8 in one of claims, is characterized in that: described iron content deionized water solution is ferric chloride aqueous solutions or toluene sulfonic acide molten iron solution.
10. method as claimed in claim 9, is characterized in that: in described ferric chloride aqueous solutions, the concentration of ferric trichloride is 2 mol/L to 4 mol/L.
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| CN104210168A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Preparation method for graphene and metal composite electromagnetic shielding film |
| CN104638256A (en) * | 2015-02-03 | 2015-05-20 | 中国科学院合肥物质科学研究院 | Nanocomposite, method for preparing nanocomposite, and lithium ion battery |
| CN105092646A (en) * | 2015-08-19 | 2015-11-25 | 电子科技大学 | Graphene/metal oxide composite film gas sensor and preparation method |
| CN107973621A (en) * | 2017-11-03 | 2018-05-01 | 东南大学 | A kind of reaction island based on graphene/nanometer gold plating and its preparation method and application |
| TWI754247B (en) * | 2020-03-20 | 2022-02-01 | 義守大學 | Manufacturing method of a gas sensor |
| CN115172065A (en) * | 2022-06-16 | 2022-10-11 | 宁德师范学院 | Three-dimensional capacitance electrode material with graphene surface grafted with polyaniline/titanium dioxide |
| WO2023282736A1 (en) * | 2021-07-07 | 2023-01-12 | University Of Malaya | An electrochemical biosensor comprising carboxylated reduced graphene oxide-titanium dioxide nanocomposite, a method of producing and a use thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104210168A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Preparation method for graphene and metal composite electromagnetic shielding film |
| CN104638256A (en) * | 2015-02-03 | 2015-05-20 | 中国科学院合肥物质科学研究院 | Nanocomposite, method for preparing nanocomposite, and lithium ion battery |
| CN105092646A (en) * | 2015-08-19 | 2015-11-25 | 电子科技大学 | Graphene/metal oxide composite film gas sensor and preparation method |
| CN107973621A (en) * | 2017-11-03 | 2018-05-01 | 东南大学 | A kind of reaction island based on graphene/nanometer gold plating and its preparation method and application |
| TWI754247B (en) * | 2020-03-20 | 2022-02-01 | 義守大學 | Manufacturing method of a gas sensor |
| WO2023282736A1 (en) * | 2021-07-07 | 2023-01-12 | University Of Malaya | An electrochemical biosensor comprising carboxylated reduced graphene oxide-titanium dioxide nanocomposite, a method of producing and a use thereof |
| CN115172065A (en) * | 2022-06-16 | 2022-10-11 | 宁德师范学院 | Three-dimensional capacitance electrode material with graphene surface grafted with polyaniline/titanium dioxide |
| CN115172065B (en) * | 2022-06-16 | 2023-04-25 | 宁德师范学院 | Three-dimensional capacitance electrode material with polyaniline/titanium dioxide grafted on graphene surface |
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Application publication date: 20140618 |