CN107271488B - Preparation method of gas-sensitive material with nano composite structure - Google Patents
Preparation method of gas-sensitive material with nano composite structure Download PDFInfo
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- CN107271488B CN107271488B CN201710452416.0A CN201710452416A CN107271488B CN 107271488 B CN107271488 B CN 107271488B CN 201710452416 A CN201710452416 A CN 201710452416A CN 107271488 B CN107271488 B CN 107271488B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- 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
Abstract
The invention discloses a preparation method of a gas sensitive material with a nano composite structure, and belongs to the technical field of sensitive materials. The preparation method of the method is different from the existing method of preparing the gas-sensitive material by adopting a mixed solution system, the film with the composite nano structure is formed by firstly forming the titanium dioxide nanotube and the graphene oxide quantum dot on the substrate through step preparation, then the graphene oxide quantum dot is reduced through laser irradiation to obtain the cluster patterned film, the defect that the graphene quantum dot and the titanium dioxide nanotube are difficult to mix is avoided, and simultaneously the RGO and the titanium dioxide nanotube are effectively compounded to form the material with the multi-dimensional characteristic based on the physical expansion effect, so that the surface area and the openness of the composite nano structure are remarkably increased, the adsorption and the desorption of gas molecules are facilitated, and the sensitivity of the gas-sensitive material is remarkably improved; and finally, an ultrathin nano metal oxide layer is deposited, so that the stability of the composite nano structure is ensured, and the selectivity of the material to gas is improved.
Description
Technical Field
The invention belongs to the technical field of sensitive materials, and particularly relates to a preparation method of a gas sensitive material with a nano composite structure.
Background
The gas sensitive material relates to the interaction between the surface of the sensitive material and gas molecules, or causes the electrical property of the sensitive material to change, so as to generate a gas sensitive signal. The generation of the gas-sensitive signal involves the adsorption of gas on the surface of the gas-sensitive material and the charge transfer between gas molecules and the gas-sensitive material. The key in the process is to improve the effect between the sensitive material and the gas molecules. Therefore, how to develop a novel gas sensitive material to solve the above problems has become a research focus in the art.
The nano-structured material system has the advantages of large specific surface area and open structure, so the nano-structured material system has extremely important application value in the field of gas sensitive materials. The compounding of the nano structure can improve the morphology and the structure of the material, and the synergistic effect among the materials is expected to improve the sensitivity and the selectivity of the gas sensitive material system. Therefore, how to realize a multi-dimensional nanostructure system of quantum dots, nanowires, nanotubes and other nanostructures through a stable assembly method becomes a hot spot in the field. However, due to the existence of surface effect between different nanostructures, the stacking effect of the nanostructure material is serious, and therefore, it is difficult to achieve stable assembly. Therefore, how to combine efficient preparation processes to obtain stable nanocomposite structures becomes an urgent problem to be solved in the art.
Disclosure of Invention
The invention solves the technical problem of providing a method for preparing a material with a stable composite structure formed by reduced graphene oxide quantum dots and titanium dioxide nanotubes.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a gas sensitive material with a nano composite structure is characterized by comprising the following steps: forming a film compounded by graphene oxide quantum dots and titanium dioxide nanotubes on a substrate, reducing the graphene oxide quantum dots by adopting a laser irradiation method, forming a nano metal oxide film on the prepared composite structure of the reduced graphene oxide quantum dots and the titanium dioxide nanotubes, and finally preparing the reduced graphene oxide quantum dots, the titanium dioxide nanotubes and the nano metal oxide film composite nano structure material.
Further, the method specifically comprises the following steps of forming the graphene oxide quantum dot and titanium dioxide nanotube composite film on the substrate:
and spraying the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid on the surface of the substrate by adopting a simultaneous air spraying mode to prepare a membrane, and then drying to obtain the material with the graphene oxide quantum dot and titanium dioxide nanotube composite structure.
In a preferred embodiment, the graphene oxide quantum dot dispersion has a concentration of 1.5mg/mL to 2.0mg/mL, and the titanium dioxide nanotube dispersion has a concentration of 0.5mg/mL to 1.0 mg/mL.
Further, the method for preparing the metal oxide thin film in the present invention includes, but is not limited to: atomic layer deposition, chemical vapor deposition, and molecular beam epitaxy.
Further, the nano metal oxide film is made of nano aluminum oxide, nano ruthenium oxide, nano iron oxide, nano tin oxide, nano zirconium oxide or nano zinc oxide;
furthermore, the thickness of the metal oxide film is 5-10 nm.
The method is different from the existing method for preparing the gas-sensitive material by adopting a solution mixing system, a film with a graphene oxide and titanium dioxide nanotube composite structure is firstly formed on a substrate through step preparation, then the graphene oxide quantum dots are reduced into reduced graphene quantum dots by adopting laser irradiation, and in the laser reduction process, the quantum dots generate a physical expansion effect to form a convex structure so as to be effectively compounded with the titanium dioxide nanotube, so that the surface area and the openness of the composite nanostructure are obviously increased, the adsorption and the desorption of gas molecules are facilitated, and the selectivity and the sensitivity of the gas-sensitive material are improved; according to the invention, the ultrathin metal oxide layer is formed on the composite structure of the reduced graphene oxide quantum dot and the titanium dioxide nanotube, so that the structural stability of the formed multi-dimensional material is ensured, and the selectivity of the composite nanostructure to gas molecules is improved by the metal oxide film.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts the technical means of simultaneously air-spraying the graphene oxide quantum dots and the titanium dioxide nanotube and then reducing the graphene oxide quantum dots by laser, thereby effectively avoiding the defect that the graphene quantum dots and the titanium dioxide nanotube are difficult to mix, and simultaneously, in the laser reduction process, the quantum dots and the nanotube are effectively compounded due to the physical expansion effect, thereby obviously increasing the surface area and the openness of the composite nanostructure, being beneficial to the adsorption and desorption of gas molecules and improving the selectivity and the sensitivity of the gas sensitive material.
(2) According to the invention, the ultrathin nano metal oxide layer is formed on the composite structure of the reduced graphene oxide quantum dot and the titanium dioxide nanotube, so that the stability of the composite surface structure of the quantum dot and the nanotube is ensured, and the introduction of the metal oxide is favorable for enhancing the selectivity of the composite gas-sensitive material to gas.
(3) The preparation method has the advantages of simplicity, controllability and environmental protection, and the patterning of the composite nano structure can be realized by the laser reduction process, and the direct assembly of devices is favorably realized.
Detailed Description
The process flow of the invention is explained in detail below with reference to specific examples:
example 1:
step 1:
weighing 15mg of graphene quantum dots, dissolving the 15mg of graphene quantum dots in 9.8mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 1.5 mg/mL; weighing 10mg of titanium dioxide nanotube, dissolving in 9.6mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 1.0 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a nano zinc oxide layer with the thickness of 5nm on the surface of the film, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano zinc oxide on the interdigital electrode surface.
Example 2:
step 1:
weighing 20mg of graphene quantum dots, dissolving the graphene quantum dots in 9.6mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 2.0 mg/mL; weighing 10mg of titanium dioxide nanotube, dissolving in 9.6mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 1.0 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a nano zirconia layer with the thickness of 5nm on the surface of the film, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano zirconia on the interdigital electrode surface.
Example 3:
step 1:
weighing 15mg of graphene quantum dots, dissolving the 15mg of graphene quantum dots in 9.8mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 1.5 mg/mL; weighing 5.0mg of titanium dioxide nanotube, dissolving in 9.8mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 0.5 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a nano aluminum oxide layer with the thickness of 5nm on the surface of the film, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano aluminum oxide on the interdigital electrode surface.
Example 4:
step 1:
weighing 15mg of graphene quantum dots, dissolving the 15mg of graphene quantum dots in 9.8mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 1.5 mg/mL; weighing 10mg of titanium dioxide nanotube, dissolving in 9.6mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 1.0 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a layer of nano ruthenium oxide with the thickness of 5nm on the film surface, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano ruthenium oxide on the interdigital electrode surface.
Example 5:
step 1:
weighing 15mg of graphene quantum dots, dissolving the 15mg of graphene quantum dots in 9.8mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 1.5 mg/mL; weighing 10mg of titanium dioxide nanotube, dissolving in 9.6mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 1.0 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a nano iron oxide layer with the thickness of 5nm on the surface of the film, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano iron oxide on the interdigital electrode surface.
Example 6:
step 1:
weighing 15mg of graphene quantum dots, dissolving the 15mg of graphene quantum dots in 9.8mL of deionized water, and preparing 10mL of graphene oxide quantum dot dispersion liquid with the concentration of 1.5 mg/mL; weighing 10mg of titanium dioxide nanotube, dissolving in 9.6mL of ethanol, and preparing 10mL of titanium dioxide nanotube dispersion liquid with the concentration of 1.0 mg/mL;
step 2:
respectively measuring 2ml of each of the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid, adding the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid into a cavity of air-jet equipment, depositing the graphene oxide quantum dot and the titanium dioxide nanotube on the surface of the interdigital electrode subjected to hydrophilic treatment in a simultaneous air-jet mode, and then placing the interdigital electrode in a vacuum drying oven at the temperature of 60 ℃ for drying for 2 hours to obtain a film with a composite nanostructure formed by the graphene oxide quantum dot and the titanium dioxide nanotube;
and step 3:
placing the interdigital electrode surface film prepared in the step 2 under a laser beam, adjusting the power to be 100mW, and adjusting the stepping rate of a laser head to be 15mm/min, so that the graphene oxide quantum dots are reduced to reduced graphene oxide quantum dots, and finally obtaining a patterned film;
and 4, step 4:
and (3) placing the interdigital electrode surface film prepared in the step (3) in atomic layer deposition equipment, depositing a nano tin oxide layer with the thickness of 5nm on the surface of the film, and finally preparing the film with the composite nano structure formed by the reduced graphene oxide quantum dots, the titanium dioxide nanotube and the nano tin oxide on the interdigital electrode surface.
The foregoing detailed description is to be construed as illustrative only and not limiting, and, although preferred embodiments of the invention have been set forth, other changes and modifications to the described embodiments will occur to those skilled in the art once they learn of the basic inventive concepts. The scope of the claims of the present invention should therefore be construed to cover the preferred embodiments and all variations and modifications that fall within the scope of the present invention.
Claims (6)
1. A preparation method of a gas sensitive material with a nano composite structure is characterized by comprising the following steps: forming a film compounded by graphene oxide quantum dots and titanium dioxide nanotubes on a substrate, reducing the graphene oxide quantum dots by adopting a laser irradiation method, forming a nano metal oxide film on the prepared composite structure of the reduced graphene oxide quantum dots and the titanium dioxide nanotubes, and finally preparing the gas-sensitive material with the composite nano structure of the reduced graphene oxide quantum dots, the titanium dioxide nanotubes and the nano metal oxide film.
2. The method for preparing the gas sensitive material with the nano composite structure according to claim 1, wherein the specific operation of forming the thin film compounded by the graphene oxide quantum dots and the titanium dioxide nanotubes on the substrate is as follows:
and spraying the graphene oxide quantum dot dispersion liquid and the titanium dioxide nanotube dispersion liquid on the surface of the substrate in a simultaneous air spraying manner, and drying to obtain the film with the composite nanostructure formed by the graphene oxide quantum dots and the titanium dioxide nanotubes.
3. The method for preparing the gas sensitive material with the nano composite structure according to claim 2, wherein the concentration of the graphene oxide quantum dot dispersion liquid is 1.5 mg/ml-2.0 mg/ml.
4. The method for preparing the gas sensitive material with the nano-composite structure according to claim 2, wherein the concentration of the titanium dioxide nanotube dispersion liquid is 0.5mg/ml to 1.0 mg/ml.
5. The method for preparing the gas sensitive material with the nano-composite structure according to claim 1, wherein the nano-metal oxide film is made of nano aluminum oxide, nano ruthenium oxide, nano iron oxide, nano tin oxide, nano zirconium oxide or nano zinc oxide.
6. The method for preparing the gas sensitive material with the nano composite structure according to claim 5, wherein the thickness of the nano metal oxide film is 5-10 nm.
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| CN111380818B (en) * | 2018-12-28 | 2021-06-18 | Tcl科技集团股份有限公司 | Thin film and preparation method thereof and detection method of free cadmium ions |
| CN110736722B (en) * | 2019-10-29 | 2022-04-08 | 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 |
| CN112014439B (en) * | 2020-08-31 | 2022-05-31 | 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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| CN101589173A (en) * | 2007-02-07 | 2009-11-25 | Imra美国公司 | A method for depositing crystalline titania nanoparticles and films |
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