CN107271488A - A kind of preparation method of nano composite structure gas sensitive - Google Patents
A kind of preparation method of nano composite structure gas sensitive Download PDFInfo
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- CN107271488A CN107271488A CN201710452416.0A CN201710452416A CN107271488A CN 107271488 A CN107271488 A CN 107271488A CN 201710452416 A CN201710452416 A CN 201710452416A CN 107271488 A CN107271488 A CN 107271488A
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- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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Abstract
The invention discloses a kind of preparation method of nano composite structure gas sensitive, belong to sensitive material technical field.The preparation method of this method is different from existing use mixed solution system and prepares gas sensitive, the film that titania nanotube and graphene oxide quantum dot formation composite nanostructure are formed first on substrate is prepared by substep, then redox graphene quantum dot is irradiated by laser and obtains a case film, while avoiding graphene quantum dot from being difficult to the defect mixed with titania nanotube, RGO is caused to carry out effectively being compounded to form the material with various dimensions feature with titania nanotube based on physical expansion effect, so as to dramatically increase the surface area and opening of composite nanostructure, be conducive to absorption and the desorption of gas molecule, significantly improve the sensitivity of gas sensitive；Last redeposition ultrathin nanometer metal oxide layer, not only ensures the stability of composite nanostructure, and improve the selectivity of material for gaseous.
Description
Technical field
The invention belongs to sensitive material technical field, more particularly to a kind of preparation side of nano composite structure gas sensitive
Method.
Background technology
Gas sensitive is related to the interaction between sensitive material surface and gas molecule, or causes the electricity of sensitive material
Performance changes, and produces gas sensitive signal.And the generation of gas sensitive signal can be related to absorption of the gas on gas sensitive surface
And the electric charge transfer between gas molecule and gas sensitive.Sensitive material and gas are more crucially improved in above process
Action effect between body molecule.Therefore, how to develop a kind of new gas sensitive turns into this area to solve the above problems
Research emphasis.
Because the material system of nanostructured has, specific surface area is big, structure opening advantage, so in gas sensitive neck
Domain has extremely important application value.And the compound of nanostructured can not only improve the pattern and structure of material, and respectively
Cooperative effect between material is also expected to be lifted sensitivity and the selectivity of gas sensitive system.So, how to pass through stabilization
Assemble method causes the nanostructureds such as quantum dot, nano wire, nanotube to realize that the nanostucture system of various dimensions becomes ability
The focus in domain.However, due to there is skin effect between different nanostructureds, causing the stack effect of nano structural material tight
Weight, therefore realizing stable assembling also with larger difficulty.Therefore, effective preparation technology how is combined to obtain stable nanometer
Composite construction turns into this area urgent problem to be solved.
The content of the invention
Present invention solves the technical problem that being to provide one kind prepares redox graphene quantum dot and nano titania
The method that pipe forms stable sandwich, the present invention passes through physical expansion effect so that RGO enters with titania nanotube
Row is effectively compounded to form the material with various dimensions feature, so that the surface area and opening of composite nanostructure are dramatically increased,
Be conducive to absorption and the desorption of gas molecule, so as to greatly improve sensitivity and the selectivity of gas sensor.
To achieve these goals, the invention provides following technical scheme：
A kind of preparation method of nano composite structure gas sensitive, it is characterised in that including：Oxidation stone is formed on substrate
The film that black alkene quantum dot is mutually combined with titania nanotube, then using laser irradiation redox graphene quantum
Point, then form nano metal oxide on the composite construction of obtained redox graphene quantum dot and titania nanotube
Thing film, finally obtained redox graphene quantum dot, titania nanotube and nano-metal-oxide Film laminated are received
Rice structural material.
Further, form what graphene oxide quantum dot was mutually combined with titania nanotube in the present invention on substrate
Film is specifically using following operation：
By graphene oxide quantum dot dispersion liquid and both dispersion liquids of titania nanotube dispersion liquid using gas simultaneously
The mode of spray is sprayed at substrate surface film, and graphene oxide quantum dot and nano titania are then obtained after drying process
The material of pipe composite construction.
As the method that is preferable to carry out, the concentration of above-mentioned graphene oxide quantum dot dispersion liquid is 1.5mg/mL~2.0mg/
ML, the concentration of titania nanotube dispersion liquid is 0.5mg/mL~1.0mg/mL.
Further, the method that metal-oxide film is prepared in the present invention includes but is not limited to：Atomic layer deposition method,
Chemical vapour deposition technique and molecular beam epitaxy.
Further, the material of nano-metal-oxide film is nano aluminium oxide, nano oxidized ruthenium, nanometer in the present invention
Iron oxide, nano tin dioxide, nano zircite or nano zine oxide；
Further, the thickness of metal-oxide film is 5~10nm in the present invention.
The present invention is different from existing use solution mixed system and prepares gas sensitive, and the first shape on substrate is prepared by substep
Into graphene oxide and the film of titania nanotube composite construction, then irradiated again using laser and cause graphene oxide amount
Son point is reduced to reduced graphene quantum dot, and during laser reduction, quantum dot produces physics bulking effect and forms projection
Structure so can with titania nanotube effectively be combined, so as to dramatically increase surface area and the opening of composite nanostructure
Property, be conducive to absorption and the desorption of gas molecule, improve selectivity and the sensitivity of gas sensitive；The present invention is in reduction-oxidation
Ultra thin metal oxide layer is formed on the composite construction of graphene quantum dot and titania nanotube, it is ensured that form various dimensions
The structural stability of material, and metal-oxide film also improves selection of the composite nanostructure to gas molecule simultaneously
Property.
Compared with prior art, the invention has the advantages that：
(1) using gas blowout graphene oxide quantum dot simultaneously, laser reduction is aoxidized the present invention again with titania nanotube
The technological means of graphene quantum dot, effectively prevent the defect that graphene quantum dot and titania nanotube are difficult to mix,
Meanwhile, during laser reduction, because physical expansion effect causes quantum dot to be effectively combined with nanotube, so as to dramatically increase
The surface area and opening of composite nanostructure, are conducive to absorption and the desorption of gas molecule, improve the selection of gas sensitive
Property and sensitivity.
(2) the present invention forms ultra-thin on the composite construction of redox graphene quantum dot and titania nanotube
Nano-metal-oxide layer, not only ensure that the stability of quantum dot and nanotube phase surface, and metal is aoxidized
The introducing of thing is conducive to strengthening selectivity of the composite air-sensitive material for gas.
(3) has simple controllable, environmentally friendly advantage with preparation method of the present invention, and laser reduction process can be realized multiple
The patterning of nanostructured is closed, and is advantageously implemented the direct-assembling of device.
Embodiment
Present invention process flow is described in detail below in conjunction with specific embodiment：
Embodiment 1：
Step 1：
Weigh graphene quantum dot 15mg to be dissolved in 9.8ml deionized waters, preparation obtains 10mL concentration for 1.5mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 10mg to be dissolved in 9.6ml ethanol, preparation obtains 10mL
Concentration is 1.0mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nano oxidized zinc layers for 5nm are spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano zine oxide formation composite nanostructure.
Embodiment 2：
Step 1：
Weigh graphene quantum dot 20mg to be dissolved in 9.6ml deionized waters, preparation obtains 10mL concentration for 2.0mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 10mg to be dissolved in 9.6ml ethanol, preparation obtains 10mL
Concentration is 1.0mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nano oxidized zirconium layer for 5nm is spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano zircite formation composite nanostructure.
Embodiment 3：
Step 1：
Weigh graphene quantum dot 15mg to be dissolved in 9.8ml deionized waters, preparation obtains 10mL concentration for 1.5mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 5.0mg to be dissolved in 9.8ml ethanol, preparation is obtained
10mL concentration is 0.5mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nano oxidized aluminium lamination for 5nm is spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano aluminium oxide formation composite nanostructure.
Embodiment 4：
Step 1：
Weigh graphene quantum dot 15mg to be dissolved in 9.8ml deionized waters, preparation obtains 10mL concentration for 1.5mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 10mg to be dissolved in 9.6ml ethanol, preparation obtains 10mL
Concentration is 1.0mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nano oxidized layer of ruthenium for 5nm is spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano oxidized ruthenium formation composite nanostructure.
Embodiment 5：
Step 1：
Weigh graphene quantum dot 15mg to be dissolved in 9.8ml deionized waters, preparation obtains 10mL concentration for 1.5mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 10mg to be dissolved in 9.6ml ethanol, preparation obtains 10mL
Concentration is 1.0mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nano oxidized iron layer for 5nm is spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano-sized iron oxide formation composite nanostructure.
Embodiment 6：
Step 1：
Weigh graphene quantum dot 15mg to be dissolved in 9.8ml deionized waters, preparation obtains 10mL concentration for 1.5mg/mL
Graphene oxide quantum dot dispersion liquid；Weigh titania nanotube 10mg to be dissolved in 9.6ml ethanol, preparation obtains 10mL
Concentration is 1.0mg/mL titania nanotube dispersion liquid；
Step 2：
Graphene oxide quantum dot dispersion liquid and each 2ml of titania nanotube dispersion liquid are measured respectively, are added gas blowout and are set
In standby cavity, graphene oxide quantum dot and titania nanotube are deposited on by hydrophilic place by the way of gas blowout simultaneously
The interdigital electrode surface of reason, is subsequently placed in the vacuum drying chamber that temperature is 60 DEG C and dries 2 hours, obtain graphene oxide quantum
The film of point and titania nanotube formation composite nanostructure；
Step 3：
Step 2 is made into interdigital electrode surface film to be placed under laser beam, adjustment power is 100mW, laser head stepping
Speed is 15mm/min so that graphene oxide quantum dot is reduced to redox graphene quantum dot, finally gives patterning
Film；
Step 4：
Step 3 is made into interdigital electrode surface film to be placed in atomic layer deposition apparatus, a thickness is deposited in film surface
The nm tin oxide layer for 5nm is spent, redox graphene quantum dot, nano titania finally is made on interdigital electrode surface
The film of pipe and nano tin dioxide formation composite nanostructure.
Above-mentioned embodiment is only schematical, rather than restricted, although having elaborated that the present invention's is excellent
Embodiment is selected, but those skilled in the art once know basic creative concept, you can above-described embodiment is made separately
Outer change and modification.Therefore the scope of the claim of the present invention should cover preferred embodiment and fall into the scope of the invention
Have altered and change.
Claims (6)
1. a kind of preparation method of nano composite structure gas sensitive, it is characterised in that including：Graphite oxide is formed on substrate
The film that alkene quantum dot is mutually combined with titania nanotube, then using laser irradiation redox graphene quantum dot,
Again nano-metal-oxide is formed on the composite construction of obtained redox graphene quantum dot and titania nanotube
Film, is finally made redox graphene quantum dot, titania nanotube and nano-metal-oxide Film laminated nanometer
Structure gas sensitive.
2. the preparation method of a kind of nano composite structure gas sensitive according to claim 1, it is characterised in that in substrate
The upper concrete operations for forming the film that graphene oxide quantum dot is mutually combined with titania nanotube are as follows：
Graphene oxide quantum dot dispersion liquid and titania nanotube dispersion liquid are sprayed at base by the way of gas blowout simultaneously
Piece surface, then obtains graphene oxide quantum dot after drying process and titania nanotube forms composite nanostructure
Film.
3. a kind of preparation method of nano composite structure gas sensitive according to claim 2, it is characterised in that oxidation stone
The concentration of black alkene quantum dot dispersion liquid is 1.5mg/ml~2.0mg/ml.
4. a kind of preparation method of nano composite structure gas sensitive according to claim 2, it is characterised in that titanium dioxide
The concentration of titanium nanotube dispersion liquid is 0.5mg/ml~1.0mg/ml.
5. a kind of preparation method of nano composite structure gas sensitive according to claim 1, it is characterised in that nanogold
Belong to sull material for nano aluminium oxide, nano oxidized ruthenium, nano-sized iron oxide, nano tin dioxide, nano zircite or
Person's nano zine oxide.
6. a kind of preparation method of nano composite structure gas sensitive according to claim 5, it is characterised in that nanogold
The thickness for belonging to sull is 5~10nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110736722A (en) * | 2019-10-29 | 2020-01-31 | 广州特种承压设备检测研究院 | Manufacturing method of graphene quantum dot composite material optical fiber gas sensor |
| CN111380818A (en) * | 2018-12-28 | 2020-07-07 | Tcl集团股份有限公司 | Thin film and preparation method thereof and detection method of free cadmium ions |
| CN112014439A (en) * | 2020-08-31 | 2020-12-01 | 南京信息工程大学 | Graphene quantum dot functionalization-based composite nano film material and gas-sensitive sensing element |
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