CN107144606A - A kind of zinc oxide nano rod CNT ethanol sensor and preparation method thereof - Google Patents
A kind of zinc oxide nano rod CNT ethanol sensor and preparation method thereof Download PDFInfo
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- CN107144606A CN107144606A CN201710242746.7A CN201710242746A CN107144606A CN 107144606 A CN107144606 A CN 107144606A CN 201710242746 A CN201710242746 A CN 201710242746A CN 107144606 A CN107144606 A CN 107144606A
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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
Abstract
The invention discloses a kind of zinc oxide nano rod CNT ethanol sensor and preparation method thereof, belong to gas detection technology field.Sensitive layer, test electrode and heating electrode of the ethanol sensor on earthenware, earthenware are constituted, and wherein sensitive layer is zinc oxide nano rod carbon nano tube compound material.The preparation process of sensor is divided into：1) zinc oxide nano rod carbon nano tube compound material is prepared；2) heater-type sintered-type gas sensor is prepared.Gas sensor has reached 2ppm to the Monitoring lower-cut of ethanol, while having shorter response time, stronger repetition stability and higher sensitivity.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method thereof, and in particular to a kind of zinc oxide nano rod-carbon nanometer
Pipe belongs to gas detection technology field as ethanol sensor of sensitive membrane and preparation method thereof.
Background technology
Highly sensitive and quick response the novel sensor of development, to environmental monitoring, the healthy of people, military and national defense etc.
Have great importance.ZnO is one of wider gas sensitive of current application, and many is based on ZnO nano-structure gas sensing
The research of device has some to report, however, single zinc oxide remains a series of bottleneck, including spirit as sensor
Sensitivity is low and responds the shortcomings of recovery characteristics are poor, limits its further application.It is therefore desirable to by zinc oxide with it is other
Material cladding, realizes that material is integrated with function, has given play to the advantage of two kinds of materials.
CNT belongs to nano material, and it has hollow tubular structure, with big specific surface area, can largely adsorb and treat
Gas is surveyed, its surface carries many active groups, is conducive to gas to detect, CNT also has unique physical chemistry in addition
Performance, such as high electron mobility and conductance, the nano-sensor research heat as field of nanometer devices is prepared using it
One of point.By two kinds of structure composites of nano structure of zinc oxide and CNT, many interesting structures and performance will be obtained, are utilized
The cooperative effect of two kinds of structures, can further improve the sensitivity of gas detection, accelerates its response recovery time.There is presently no
Relevant report in this respect.
The content of the invention
There is provided a kind of zinc oxide nano rod-composite structure of carbon nano tube for the deficiency in above-mentioned prior art by the present invention
Ethanol sensor as sensitive membrane and preparation method thereof, obtained sensor performance comes relative to zinc oxide nano rod sensor
Say, the sensitivity and response speed to alcohol gas all have increased significantly.
Technical scheme
Sensitive layer, test on a kind of zinc oxide nano rod-CNT ethanol sensor, including earthenware, earthenware
Electrode and heating electrode.Earthenware (being about 4.1 millimeters, about 1.0 millimeters of internal diameter, about 1.4 millimeters of external diameter) two ends have gold electrode,
4 Pt wires are drawn at gold electrode, test electrode is used as；A piece spiral helicine nichrome wire runs through earthenware, is used as heating
Electrode；Wherein, sensitive layer is zinc oxide nano rod-carbon nano tube compound material, is covered in ceramic pipe surface and two gold electricity
Between pole.The preparation of sensitive layer is divided into three steps：1) hydro-thermal method prepares ZnO nanorod；2) CVD prepares CNT；3) by two
Plant material mixing coating between electrodes.
Preferably, the mass fraction percentage of sensitive composition of layer is：50~95% zinc oxide nano rod, 5~50%
CNT.
The preparation method of the zinc oxide nano rod that the present invention is provided-CNT ethanol sensor is specific according to following steps
Carry out：
Step 1, zinc nitrate, methenamine, ammoniacal liquor, the mixed solution of polyethyleneimine, i.e. ZnO digestion solutions are configured.
Step 2, ZnO digestion solutions are poured into autoclave, digestion solution is no more than the 2/3 of autoclave, be positioned over true
Furnace cooling after hydro-thermal process in empty drying box, reaction.
Step 3, the ZnO digestion solutions after hydro-thermal method is handled pour into centrifuge tube, using centrifugal collection white precipitate, repeatedly
Cleaning, and dry in air atmosphere, obtain zinc oxide white powder.
Step 4, the Zinc oxide powder that step 3 is obtained is mixed with CNT, pasty state is ground to form in mortar, be coated in
On earthenware, sintered after air-drying in Muffle furnace.
Step 5, using in the earthenware described in the careful inserting step 4 of a nichrome wire as heating electrode, and will
Electrode and test electrode welding are heated on a hexagonal pedestal, that is, heater-type sintered-type gas sensor has been made.
Step 6, gas sensor step 5 being made is inserted on WS-30A gas sensor testers, carries out aging, oxygen is made
Change zinc nanometer rods-CNT ethanol sensor.
Complete after above step, obtained ethanol sensor can carry out the test of air-sensitive performance, such as sensitivity is responded extensive
Multiple characteristic, least concentration etc..
Preferably, the content of each composition is in the ZnO digestion solutions：Zinc nitrate is 0.05mol/L, and methenamine is
0.05mol/L, ammoniacal liquor is 0.05mol/L, and polyethyleneimine is 0.002mol/L.
Preferably, the temperature of vacuum drying chamber is 100 DEG C, and the hydro-thermal time is 12h.
Preferably, step 3 is obtained white precipitate ultra-pure water or washes of absolute alcohol, dry under 60 DEG C of air atmospheres
It is dry.
Preferably, Zinc oxide powder and CNT are according to mass ratio 4:1 mixing, sintering temperature is 450 DEG C.
Preferably, aging temperature is 300 DEG C, and ageing time is 24h.
The preparation method of wherein CNT is：Substrate is done using P-type silicon piece, using magnetron sputtering method radio frequency nickel plating conduct
Catalyst, CNT is prepared using CVD.
Preferably, nickel plating power is 150W, and the time is 50s.
Preferably, the reaction time is 15min, CH4And H2Flow is respectively 10sccm and 40sccm.
Present invention process is simple, easy to operate and with low cost.The present invention has advantages below compared with prior art：This
Invention has big specific surface area using the hollow tubular structure of CNT, can largely adsorb under test gas.Its surface is carried
Many active groups, are conducive to gas to detect, CNT also has unique physical and chemical performance in addition, and such as high electronics is moved
Shifting rate and conductance.By the compound of zinc oxide nano rod and CNT, preparing gained composite air-sensitive sensing membrane has high table
Face adsorption capacity and the completely depleted of carrier can be reached, form double depletion layers, and then show higher sensitivity, faster
Response characteristic.
Brief description of the drawings
Fig. 1 is gas sensor configuration schematic diagram prepared by a preferred embodiment of the present invention；
Fig. 2 is gas sensor schematic diagram prepared by a preferred embodiment of the present invention；
Fig. 3 is the scanning electricity of zinc oxide nano rod-carbon nano tube compound material prepared by a preferred embodiment of the present invention
Mirror picture；
Fig. 4 is pure zinc oxide nanometer rods and zinc oxide nano rod-CNT prepared by a preferred embodiment of the present invention
Response recovery curve figure of the composite to 50ppm concentration ethanols；
Fig. 5 is sensitivity curve of the ethanol sensor to different concentration ethanol of a preferred embodiment of the present invention preparation
Figure.
Embodiment
The implementation to the present invention is described in detail below in conjunction with the accompanying drawings.The present embodiment with the technical scheme is that
Under the premise of implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
It is quick on zinc oxide nano rod-CNT ethanol sensor, including earthenware 1, earthenware as shown in Figure 1 and Figure 2
Feel layer 2, test electrode 3 and heating electrode 4.Earthenware (being about 4.1 millimeters, about 1.0 millimeters of internal diameter, about 1.4 millimeters of external diameter) two
End, which has, draws 4 Pt wires at gold electrode, gold electrode, be used as test electrode；A piece spiral helicine nichrome wire is through pottery
Porcelain tube, is used as heating electrode；Wherein, sensitive layer is zinc oxide nano rod-carbon nano tube compound material, is covered in ceramic pipe surface
And between two gold electrodes.
The preparation process of zinc oxide nano rod-CNT ethanol sensor is as follows：
The preparation of zinc oxide nano rod：First, zinc nitrate (0.05M), methenamine (0.05M), ammonia are prepared with ultra-pure water
The mixed solution of water (0.05M) and polyethyleneimine (2mM).Secondly, mixed solution is poured into 50mL autoclaves, sealed
Autoclave, in vacuum drying chamber after 100 DEG C of reaction 12h, cools to room temperature with the furnace, then removes solution.Finally, use
Centrifugal collection white precipitate, the white precipitate being collected into is cleaned multiple times with ultra-pure water and absolute ethyl alcohol, and in 50~70 DEG C of skies
Dried under gas atmosphere, obtain white powder, i.e. zinc oxide nano rod.
By zinc oxide nano rod and CNT according to mass ratio 4:1 is mixed in mortar, pours into a small amount of alcohol grinding, does
After, alcohol grinding is added again, and repeating half an hour (grinding direction is identical) is tuned into pasty state, is coated in ceramic pipe surface.Will
Coated earthenware natural air drying, is subsequently placed in 450~550 DEG C of sintering 2h in Muffle furnace, is taken out after furnace cooling.
By in the insertion earthenware of a nichrome wire carefully, and will heating electrode and test electrode welding at one
On hexagonal pedestal, that is, heater-type sintered-type gas sensor is made.The gas sensor is inserted into WS-30A gas sensor testers
On, using working stability as 200~300 DEG C of progress 18~24h of aging, zinc oxide nano rod-CNT ethanol sensor is made.
Complete after above step, obtained ethanol sensor can carry out the test of air-sensitive performance, such as sensitivity responds recovery characteristics,
Least concentration etc..
Fig. 1 is sensor of the invention structural representation, describes the biography of zinc oxide nano rod-carbon nano tube compound material
Feel principle, resistance variations during by detecting that composite and ethanol are acted on realize the response to ethanol.
Fig. 2 is the gas sensor schematic diagram of the present invention, describes zinc oxide nano rod-CNT ethanol sensor and six
The welding relation of angle pedestal, wherein, 5 be test electrode pin, and 6 be heating electrode pin.
Fig. 3 is the scanning electron microscopic picture of zinc oxide nano rod-carbon nano tube compound material, it can be seen that CNT is uniform
And be closely compounded on zinc oxide nano rod.
Fig. 4 is the sound of pure zinc oxide nanometer rods and zinc oxide nano rod-carbon nano tube compound material to 50ppm concentration ethanols
Answer recovery curve figure.By contrast it can be found that the sensor of composite construction is extensive with higher sensitivity and shorter response
The multiple time.
Fig. 5 is sensitivity curve figure of the zinc oxide nano rod-CNT ethanol sensor to different concentration ethanol, with
The increase of concentration of alcohol, the sensitivity of gas sensor gradually increases, and minimum response concentration can reach 2ppm.
Embodiment 2
Structure and the preparation process such as embodiment 1 of zinc oxide nano rod-CNT ethanol sensor, by zinc-oxide nano
The mass fraction content of CNT in rod-carbon nano tube compound material falls below 10% by 25%, and gas sensor is made
8 are reduced to by 16 to the sensitivity of 50ppm concentration ethanols.
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without
Need creative work just can make many modifications and variations according to the design of the present invention.Therefore, all technologies in the art
Personnel under this invention's idea on the basis of existing technology by logic analysis, reasoning or it is limited realize it is available
Technical scheme all should be in the protection domain being defined in the patent claims.
Claims (8)
1. sensitive layer, test electricity on a kind of zinc oxide nano rod-CNT ethanol sensor, including earthenware, earthenware
Pole and heating electrode；Earthenware two ends, which have, draws 4 Pt wires at gold electrode, gold electrode, be used as test electrode；A piece spiral
The nichrome wire of shape runs through earthenware, is used as heating electrode；The sensitive layer is zinc oxide nano rod-carbon nanotube composite
Material, is covered between ceramic pipe surface and two gold electrodes..
2. a kind of zinc oxide nano rod-CNT ethanol sensor according to claim 1, it is characterised in that described
The mass fraction percentage of sensitive composition of layer is：50~95% zinc oxide nano rod, 5~50% CNT.
3. the preparation method of zinc oxide nano rod-CNT ethanol sensor described in claim 1 or 2, it is characterised in that
The preparation method is followed the steps below：
Step 1, the mixed solution of configuration zinc nitrate, methenamine, ammoniacal liquor and polyethyleneimine, i.e. ZnO digestion solutions；
Step 2, ZnO digestion solutions are poured into autoclave, is positioned over hydro-thermal process in vacuum drying chamber, it is cold with stove after reaction
But；
Step 3, the ZnO digestion solutions after hydro-thermal method is handled pour into centrifuge tube, using centrifugal collection white precipitate, repeatedly clear
Wash, and dry in air atmosphere, obtain zinc oxide white powder；
Step 4, the Zinc oxide powder that step 3 is obtained is mixed with CNT, pasty state is ground to form in mortar, be coated in ceramics
Guan Shang, is sintered after air-drying in Muffle furnace；
Step 5, using in the earthenware described in a nichrome wire inserting step 4 as heating electrode, and will heating electrode and
Electrode welding is tested on a plastic base, that is, heater-type sintered-type gas sensor has been made；
Step 6, gas sensor step 5 being made is inserted on WS-30A gas sensor testers, carries out aging, and zinc oxide is made
Nanometer rods-CNT ethanol sensor.
4. the preparation method of zinc oxide nano rod according to claim 3-CNT ethanol sensor, its feature exists
In the content of each composition of ZnO digestion solutions is：Zinc nitrate is 0.05mol/L, and methenamine is 0.05mol/L, and ammoniacal liquor is
0.05mol/L, polyethyleneimine is 0.002mol/L.
5. the preparation method of zinc oxide nano rod according to claim 3-CNT ethanol sensor, its feature exists
In the injection rate of ZnO digestion solutions is no more than the 2/3 of autoclave in step 2, and the temperature of vacuum drying chamber is 100 DEG C, hydro-thermal
Time is 12h.
6. the preparation method of zinc oxide nano rod according to claim 3-CNT ethanol sensor, its feature exists
In white precipitate ultra-pure water or washes of absolute alcohol that step 3 is obtained are dried under 50~70 DEG C of air atmospheres.
7. the preparation method of zinc oxide nano rod according to claim 3-CNT ethanol sensor, its feature exists
In Zinc oxide powder is with CNT according to mass ratio 4:1 mixing, sintering temperature is 450~550 DEG C.
8. the preparation method of zinc oxide nano rod according to claim 3-CNT ethanol sensor, its feature exists
In aging temperature is 200~300 DEG C, and ageing time is 18~24h.
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Cited By (6)
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|---|---|---|---|---|
| CN108760836A (en) * | 2018-09-01 | 2018-11-06 | 罗杰敏 | A kind of cold ethanol detection unit |
| CN108918630A (en) * | 2018-05-16 | 2018-11-30 | 天津理工大学 | A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material |
| CN109060893A (en) * | 2018-07-05 | 2018-12-21 | 太原理工大学 | It is a kind of based on carbon nanotube/zinc oxide/chitosan complex film humidity sensor |
| CN114235900A (en) * | 2021-12-22 | 2022-03-25 | 浙江大学 | Device and method for measuring orientation degree of carbon nano tube for terahertz device |
| CN114354724A (en) * | 2022-01-11 | 2022-04-15 | 山西大学 | Metal oxide semiconductor gas sensor and preparation method and application thereof |
| WO2024027486A1 (en) * | 2022-08-02 | 2024-02-08 | 杭州三花研究院有限公司 | Measurement assembly, sensing apparatus, and manufacturing method for sensing apparatus |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918630A (en) * | 2018-05-16 | 2018-11-30 | 天津理工大学 | A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material |
| CN109060893A (en) * | 2018-07-05 | 2018-12-21 | 太原理工大学 | It is a kind of based on carbon nanotube/zinc oxide/chitosan complex film humidity sensor |
| CN109060893B (en) * | 2018-07-05 | 2020-11-13 | 太原理工大学 | Humidity sensor based on carbon nanotube/zinc oxide/chitosan composite membrane |
| CN108760836A (en) * | 2018-09-01 | 2018-11-06 | 罗杰敏 | A kind of cold ethanol detection unit |
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| CN114235900A (en) * | 2021-12-22 | 2022-03-25 | 浙江大学 | Device and method for measuring orientation degree of carbon nano tube for terahertz device |
| CN114235900B (en) * | 2021-12-22 | 2024-02-27 | 浙江大学 | Device and method for measuring orientation degree of carbon nano tube for terahertz device |
| CN114354724A (en) * | 2022-01-11 | 2022-04-15 | 山西大学 | Metal oxide semiconductor gas sensor and preparation method and application thereof |
| CN114354724B (en) * | 2022-01-11 | 2022-11-22 | 山西大学 | Metal oxide semiconductor gas sensor and preparation method and application thereof |
| WO2024027486A1 (en) * | 2022-08-02 | 2024-02-08 | 杭州三花研究院有限公司 | Measurement assembly, sensing apparatus, and manufacturing method for sensing apparatus |
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Application publication date: 20170908 |