CN108333225A - A kind of preparation method of graphene tin oxide sensing material - Google Patents
A kind of preparation method of graphene tin oxide sensing material Download PDFInfo
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- CN108333225A CN108333225A CN201711412820.1A CN201711412820A CN108333225A CN 108333225 A CN108333225 A CN 108333225A CN 201711412820 A CN201711412820 A CN 201711412820A CN 108333225 A CN108333225 A CN 108333225A
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- 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
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Abstract
The invention discloses a kind of preparation method of graphene tin oxide sensing material, the present invention is combined three-dimensional grapheme with tin oxide, is contributed to the configuration of surface for improving tin oxide, is enhanced the sensitivity of sensor detection；This method preparation process is simple, improves response efficiency by improving material specific surface area and surface-active vacancy, reduces response temperature, keep application of the tin oxide in terms of gas sensor simpler.
Description
Technical field
The present invention relates to sensor manufacturing fields, and in particular to a kind of preparation method of graphene tin oxide sensing material.
Background technology
While science and technology and social economy's rapid development, white elephant is also brought to natural environment, air is dirty
Dye seriously restricts the sustainable development of the mankind.Industrial production produces a large amount of toxic, pernicious gas, not only pollute environment,
Ecology is destroyed, and jeopardizes health and life security.Therefore, the ingredient of toxic gas and concentration meaning weight in environment are detected
Greatly.
Metal oxide such as ZnO, SnO2、WO3Deng due to have have excellent performance, environment is friendly, resourceful, cheap
The advantages that, it is the relatively broad gas sensitive of research.But metal oxide has response to majority of gas, by building not
Same structure, crystal form metal oxide can improve sensitivity, response/recovery time etc..
Three-dimensional grapheme material has the excellent chemical property of two-dimensional graphene, while having the specific surface area and more of bigger
Add excellent flexibility, the distortion of general level not to interfere with the property and characteristic of material, is conducive to prepare stretchable, stable
The good sensor of property.
Invention content
The present invention provides a kind of preparation method of graphene tin oxide sensing material, and the present invention is by three-dimensional grapheme and aoxidizes
Tin combines, and contributes to the configuration of surface for improving tin oxide, enhances the sensitivity of sensor detection；This method preparation process letter
It is single, response efficiency is improved by improving material specific surface area and surface-active vacancy, response temperature is reduced, tin oxide is made to exist
Application in terms of gas sensor is simpler.
To achieve the goals above, the present invention provides a kind of preparation method of graphene tin oxide sensing material, the party
Method includes the following steps：
（1）Prepare three-dimensional grapheme material
Three-dimensional grapheme is prepared on foamed aluminium substrate, obtains graphene/foamed aluminium composite material；
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional graphite
Alkene material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5-5mol/L
（2）The three-dimensional grapheme material is scattered in spare in deionized water, obtains the outstanding mixed object of three-dimensional grapheme, hang in mixed object
Three-dimensional grapheme material quality accounting be 0.1-0.3%；
(1-3) in molar ratio:1 takes stannic chloride and Potassium dodecylbenzenesulfonate, is placed in dimethylformamide, the concentration of stannic chloride
For 0.5-0.8M, it is vigorously stirred 2-4 hours, obtains solution one；
Appropriate ammonium carbonate is taken to be premixed with dimethylformamide, the molar ratio of ammonium carbonate and the tin ion in stannic chloride is (1-2):1,
Stirring, the pH value for adjusting solution with ammonium hydroxide obtain solution two to 9-11；
Solution one is heated to 70-80 DEG C, and is slowly added to the outstanding mixed object of three-dimensional grapheme, it is above-mentioned to be vigorously stirred simultaneously, by solution
Two slowly instill in solution one, after reacting 3-5 hours, gained precipitation are repeatedly washed with deionized water, is placed in drying box 70-90
DEG C it is dried to obtain graphene tin oxide sensing material, the mass ratio of wherein graphene and tin oxide is（2-3）：50.
Preferably, using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put
Enter in vacuum reaction stove heating region, vacuumize, heat simultaneously, by hydrogen injection vacuum reaction stove, is heated to predetermined temperature
After 100-500 DEG C, then constant temperature 10-30 minutes anneals, after being heated to 900-1100 DEG C of predetermined temperature, carbon source is led to
Enter vacuum reaction stove, while keeping hydrogen flowing quantity constant, growth closes gas and is down to room temperature after 50-100 minutes, you can obtain
The substrate of Direct precipitation graphene, i.e. graphene/foamed aluminium composite material.
Specific implementation mode
Embodiment one
Using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put into vacuum reaction stove
It in heating region, vacuumizes, heats simultaneously, by hydrogen injection vacuum reaction stove, after being heated to 100 DEG C of predetermined temperature, constant temperature 10
Minute, it then anneals, after being heated to 900 DEG C of predetermined temperature, carbon source is passed through vacuum reaction stove, while keeping hydrogen stream
Measure constant, growth closes after 50 minutes and gas and is down to room temperature, you can obtain the substrate of Direct precipitation graphene, i.e., graphene/
Foamed aluminium composite material.
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional
Grapheme material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5mol/L.
The three-dimensional grapheme material is scattered in spare in deionized water, obtains the outstanding mixed object of three-dimensional grapheme, hang mixed object
In three-dimensional grapheme material quality accounting be 0.1；In molar ratio 1:1 takes stannic chloride and Potassium dodecylbenzenesulfonate, is placed in
In dimethylformamide, a concentration of 0.5M of stannic chloride is vigorously stirred 2-4 hours, obtains solution one；Take appropriate ammonium carbonate and two
Methylformamide premixes, and the molar ratio of ammonium carbonate and the tin ion in stannic chloride is 1:1, stirring adjusts the pH of solution with ammonium hydroxide
Value obtains solution two to 9-11.
Solution one is heated to 70 DEG C, and is slowly added to the outstanding mixed object of three-dimensional grapheme, it is above-mentioned to be vigorously stirred simultaneously, by solution
Two slowly instill in solution one, and after reacting 3 hours, gained precipitation is repeatedly washed with deionized water, and it is dry to be placed in 70 DEG C of drying box
Dry to obtain graphene tin oxide sensing material, the wherein mass ratio of graphene and tin oxide is 2：50.
Embodiment two
Using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put into vacuum reaction stove
It in heating region, vacuumizes, heats simultaneously, by hydrogen injection vacuum reaction stove, after being heated to 500 DEG C of predetermined temperature, constant temperature 30
Minute, it then anneals, after being heated to 1100 DEG C of predetermined temperature, carbon source is passed through vacuum reaction stove, while keeping hydrogen
Flow is constant, and growth closes gas and is down to room temperature after 100 minutes, you can obtain the substrate of Direct precipitation graphene, i.e. graphite
Alkene/foamed aluminium composite material.
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional
Grapheme material；The etching solution is iron nitrate solution, and the solution concentration is 5mol/L.
The three-dimensional grapheme material is scattered in spare in deionized water, obtains the outstanding mixed object of three-dimensional grapheme, hang mixed object
In three-dimensional grapheme material quality accounting be 0.3%；In molar ratio 3:1 takes stannic chloride and Potassium dodecylbenzenesulfonate, is placed in
In dimethylformamide, a concentration of 0.8M of stannic chloride is vigorously stirred 4 hours, obtains solution one；Take appropriate ammonium carbonate and diformazan
Base formamide premixes, and the molar ratio of ammonium carbonate and the tin ion in stannic chloride is 2:1, stirring adjusts the pH value of solution with ammonium hydroxide
To 9-11, solution two is obtained.
Solution one is heated to 80 DEG C, and is slowly added to the outstanding mixed object of three-dimensional grapheme, it is above-mentioned to be vigorously stirred simultaneously, it will be molten
Liquid two slowly instills in solution one, after reacting 5 hours, gained precipitation is repeatedly washed with deionized water, is placed in 90 DEG C of drying box
It is dried to obtain graphene tin oxide sensing material, the wherein mass ratio of graphene and tin oxide is 3：50.
Claims (2)
1. a kind of preparation method of graphene tin oxide sensing material, this method comprises the following steps：
（1）Prepare three-dimensional grapheme material
Three-dimensional grapheme is prepared on foamed aluminium substrate, obtains graphene/foamed aluminium composite material；
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional graphite
Alkene material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5-5mol/L
（2）The three-dimensional grapheme material is scattered in spare in deionized water, obtains the outstanding mixed object of three-dimensional grapheme, hang in mixed object
Three-dimensional grapheme material quality accounting be 0.1-0.3%；
(1-3) in molar ratio:1 takes stannic chloride and Potassium dodecylbenzenesulfonate, is placed in dimethylformamide, the concentration of stannic chloride
For 0.5-0.8M, it is vigorously stirred 2-4 hours, obtains solution one；
Appropriate ammonium carbonate is taken to be premixed with dimethylformamide, the molar ratio of ammonium carbonate and the tin ion in stannic chloride is (1-2):1,
Stirring, the pH value for adjusting solution with ammonium hydroxide obtain solution two to 9-11；
Solution one is heated to 70-80 DEG C, and is slowly added to the outstanding mixed object of three-dimensional grapheme, it is above-mentioned to be vigorously stirred simultaneously, by solution
Two slowly instill in solution one, after reacting 3-5 hours, gained precipitation are repeatedly washed with deionized water, is placed in drying box 70-90
DEG C it is dried to obtain graphene tin oxide sensing material, the mass ratio of wherein graphene and tin oxide is（2-3）：50.
2. the method as described in claim 1, which is characterized in that use chemical vapour deposition technique graphene/foamed aluminium composite wood
Material, the specific steps are：Foamed aluminium is put into vacuum reaction stove heating region, vacuumizes, heats simultaneously, hydrogen injection vacuum is anti-
It answers in stove, after being heated to 100-500 DEG C of predetermined temperature, then constant temperature 10-30 minutes anneals, is heated to predetermined temperature
After 900-1100 DEG C, carbon source is passed through vacuum reaction stove, while keeping hydrogen flowing quantity constant, growth closes gas after 50-100 minutes
Body is simultaneously down to room temperature, you can obtains the substrate of Direct precipitation graphene, i.e. graphene/foamed aluminium composite material.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764779A (en) * | 2015-04-09 | 2015-07-08 | 山东师范大学 | Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure |
| CN105067670A (en) * | 2015-07-07 | 2015-11-18 | 南京信息工程大学 | Ordered Cu-doped nano-porous tin oxide sensing device |
| CN106501449A (en) * | 2016-10-17 | 2017-03-15 | 上海理工大学 | A kind of gas sensitive and element and preparation method for detecting formaldehyde gas |
| CN106564938A (en) * | 2016-10-26 | 2017-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Ag-modified SnO2 nano-material for gas sensor as well as preparation method and application of Ag-modified SnO2 nano-material |
| CN106770492A (en) * | 2016-11-10 | 2017-05-31 | 合肥铭志环境技术有限责任公司 | A kind of composite nano fiber gas sensitive of Graphene doped stannum oxide modification and preparation method thereof |
-
2017
- 2017-12-24 CN CN201711412820.1A patent/CN108333225A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764779A (en) * | 2015-04-09 | 2015-07-08 | 山东师范大学 | Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure |
| CN105067670A (en) * | 2015-07-07 | 2015-11-18 | 南京信息工程大学 | Ordered Cu-doped nano-porous tin oxide sensing device |
| CN106501449A (en) * | 2016-10-17 | 2017-03-15 | 上海理工大学 | A kind of gas sensitive and element and preparation method for detecting formaldehyde gas |
| CN106564938A (en) * | 2016-10-26 | 2017-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Ag-modified SnO2 nano-material for gas sensor as well as preparation method and application of Ag-modified SnO2 nano-material |
| CN106770492A (en) * | 2016-11-10 | 2017-05-31 | 合肥铭志环境技术有限责任公司 | A kind of composite nano fiber gas sensitive of Graphene doped stannum oxide modification and preparation method thereof |
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