CN109916965A - It is a kind of using FTO electro-conductive glass as the ZnO nano cluster gas sensor of electrode member - Google Patents
It is a kind of using FTO electro-conductive glass as the ZnO nano cluster gas sensor of electrode member Download PDFInfo
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- CN109916965A CN109916965A CN201811226084.5A CN201811226084A CN109916965A CN 109916965 A CN109916965 A CN 109916965A CN 201811226084 A CN201811226084 A CN 201811226084A CN 109916965 A CN109916965 A CN 109916965A
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Abstract
The present invention relates to a kind of FTO electro-conductive glass handled using laser ablation as the ZnO nano cluster gas sensor of electrode member, belongs to gas sensor technical field.This gas sensor is made of gas sensing electrode element and gas sensitive two parts, it is characterized in that: the gas sensing electrode element is as being carried out obtained by the laser ablation processing of specific pattern and line width to FTO electro-conductive glass, wherein etching pattern is interdigitated, interdigital width of fringe is 300 ~ 500 μm, and interdigital fringe spacing is 20 ~ 80 μm；The gas sensitive material is the ZnO nano cluster array of hexagonal wurtzite structure, and the diameter of nano wire is 70 ~ 100 nm, and length is 2 ~ 3.5 μm.FTO gas sensing electrode element of the present invention has many advantages, such as that at low cost, stability is good, is easy to gas sensitive growth in situ；The gases such as ethyl alcohol, methanol, hydrogen sulfide are shown excellent responding ability by many advantages, such as sensor has low in cost, simple process, gas sensing property excellent, and stability is good, are the novel gas sensors of a kind of great development and application prospect.
Description
Technical field
The present invention relates to a kind of using the FTO electro-conductive glass of photoetching treatment as the ZnO nano cluster gas sensor of electrode member,
Belong to gas sensor technical field.
Background technique
It is good for it is well known that excessive poisonous and harmful and flammable explosive gas will cause serious environmental pollution and endanger the mankind
Health.Currently, having caused a large amount of casualties because the major accident that poisonous and harmful and flammable explosive gas causes is commonplace
And property loss.How to realize the real-time monitoring to hazardous gas, and then avoid the generation of potential safety accident, and is dangerous gas
The subsequent processing of body, which provides, to be ensured early period, and the great difficult problem and technological challenge that current social is faced have been become.
In recent years, based on the chemical-electrical resistive gas sensor of metal oxide semiconductor material because its production cost is low,
The advantages that manufacture craft is simple, means of testing is flexible, sensitivity is higher, in industry manufacture, the detection of family life public safety etc.
Field has obtained extensive exploitation and application.But based on the application demand increasingly promoted, the sensitivity of existing gas sensor is also
To be improved, novel air-sensitive electrode member and gas sensitive are urgently excavated.Currently, people are based on chemical-electrical resistive gas sensor
Working principle: by measure material surface electronics and ambient enviroment in object gas occur redox reaction caused by
Resistance variations are detected the concentration of object gas indirectly, the exploitation of gas sensing electrode element and the size of gas sensitive, pattern and
Structure regulating etc. has carried out many work, such as develops silver (Ag) the electrode gas sensor of noble metal, is prepared for specific surface
Biggish porous, flower-shaped, the isostructural TiO of nucleocapsid of product2、ZnO、SnO2Gas sensitive etc., to promote the sensitivity of gas sensor
With service life.However, common Ag electrode member remains the disadvantages of at high cost, oxidizable, stability is poor now, especially
It is difficult to realize that the growth in situ of gas sensitive and detection are applied on its surface.In addition, gas sensitive usually requires to grind by dispersion
Mill, manual film to Ag electrode surface, decrepitation etc. are handled, and just can be carried out the detection and application of gas-sensitive property.But at this
In the process, grinding normally results in the destruction of material morphology, manual film normally results in the uneven thickness and and electrode of material
Contact it is bad, calcining will lead to reunion and surface oxidation of Ag electrode of material etc., the appearance of these problems all can serious shadow
The performance for ringing gas sensitive device, significantly reduces the precision and service life of its gasmetry.
In view of the above-mentioned problems, the gas sensing electrode element that development cost is low and performance is stable, and air-sensitive is realized on this basis
Growth in situ of the material on electrode member is the key that further promotion gas sensitive device sensitivity and service life.FTO is conductive
Glass, conducting surface are the tin dioxide thin film of one layer of F element heavy doping, have good electric conductivity, stability and crystallinity,
It is commonly used for the growth substrate of nano material, is low cost, the good selection for stablizing the preparation of gas sensing electrode element.Binding isotherm mould
Quasi- and experimental analysis, suitable interdigitated laser ablation is carried out to FTO electro-conductive glass, off state needed for forming it into detection
With distribution of electrodes, the electrode member in gas sensor just can be used as.More importantly being based on FTO electro-conductive glass air-sensitive
Electrode member, it can be achieved that a variety of gas-sensitive nano materials growth in situ, and then realize gas sensitive in situ detection and application, from
And it is obviously improved the detection accuracy and service life of gas sensor.ZnO has and protrudes as a kind of typical semiconductor material
Gas-sensitive property (fast, high sensitivity, multiple gases response of response etc.), and preparation process simple (such as hydro-thermal method), it is low in cost,
Morphology controllable (such as nano wire, nanotube, nanometer rods) is a kind of very excellent gas sensitive.Therefore, the present invention is with photoetching
The FTO electro-conductive glass of processing is gas sensing electrode element, and growth in situ ZnO nano cluster array on this basis, and then is obtained
Gas sensor at low cost, precision is high, performance is excellent, stability is good.
Summary of the invention
For existing gas sensing electrode element and gas sensitive cost, stability, in terms of existing for deficiency,
Invention demonstrates a method a kind of using the FTO electro-conductive glass of photoetching treatment as gas sensing electrode element growth in situ ZnO nano cluster array
Gas sensor and preparation method thereof.The present invention is conducive to air-sensitive using the FTO electro-conductive glass of photoetching treatment as gas sensing electrode element
The enhancing of the growth in situ and device stability of material；ZnO nano cluster array with big aspect ratio provides big ratio table
Area and direct electron transport channel, are conducive to the air-sensitive performance for being obviously improved material；By by gas sensitive growth in situ
In overcoming on gas sensing electrode element, destructible material morphology existing for knife coating, coating thickness in traditional air-sensitive test are uneven
Even, material contacts the disadvantages of bad, material is easy to reunite, electrode is oxidizable with electrode.Gas sensing utensil prepared by the present invention
There is many advantages, such as at low cost, high sensitivity, response resume speed is fast, stability is good.
The obtained gas sensor of the present invention using the FTO electro-conductive glass of photoetching treatment as gas sensing electrode element, it is characterized in that:
This electrode member is to carry out special pattern, line width, depth to FTO electro-conductive glass conductive layer by theoretical modeling and experimental analysis
Laser ablation obtain, wherein
The litho pattern is interdigitated；
The interdigital fringe spacing of the figure is 20 ~ 80 μm；
The interdigital width of fringe of the figure is 300 ~ 500 μm；
The laser ablation depth of the figure is 0.5-1 μm；
The material of the electrode member is FTO electro-conductive glass.
The obtained gas sensor of the present invention using ZnO nano cluster array as gas sensitive, it is characterized in that
The ZnO nano cluster array is equably grown on gas sensing electrode surface；
The morphological rules of the ZnO nano cluster array is orderly, and surface is smooth；
The diameter of the ZnO nano cluster is 70 ~ 100 nm, and length is 2 ~ 3.5 μm；
The crystal structure of the ZnO nano cluster array is hexagonal wurtzite structure.
In addition, gas sensor of the present invention is obtained by following preparation methods:
(1) 0.05 M Zinc diacetate dihydrate, 0.05 M ethylene glycol amine and appropriate ethanol solution is taken to prepare laminar solution；
(2) electrode member is passed in and out into laminar solution twice with the speed of 1 ~ 3 mm/s using self-control lifting motor, it then will be electric
Pole element is being to be dried overnight at room temperature, is then placed in Muffle furnace and is annealed at 400 DEG C with the heating rate of 5 DEG C/min
10 min, the above process, which is repeated twice, obtains uniform ZnO seed layer；
(3) polyethyleneimine of the zinc nitrate hexahydrate compound of 0.05 M, the hexamethylenetetramine of 0.055 M, 0.018 M are taken
(molecular weight 600) and suitable deionized water solution configure hydro-thermal reaction precursor liquid；
(4) the FTO electrode member for growing seed layer and reaction precursor liquid are moved into polytetrafluoroethylliner liner, then puts liner
Enter in water heating kettle and be sealed, water heating kettle is put into drying box at 95 DEG C and reacts 6 h.It is cooled to room temperature to the end of reacting,
FTO electrode member is taken out to be placed into 60 DEG C of 2 h of drying in drying box with deionized water and ethyl alcohol repeated flushing, can be carried out
Gas-sensitive property test in situ；
(5) prepared gas sensor is placed on the pedestal of air-sensitive test macro, adjust test probe position, make its with
Gas sensor both ends well contact and form access.Then test temperature is set, the tested gas for being passed through suitable concentration can be into
The quick test of promoting the circulation of qi.
The specific technical solution of the present invention is as follows:
All reagent purities are that analysis is pure；The lifting motor is commercially available.
In step (2), the FTO electro-conductive glass gas sensing electrode element of photoetching treatment is before lifting obtains seed layer, first by it
For surface clean to cleaning, concrete operations are as follows, go appropriate electrode member to be put into beaker A, the hydrochloric acid water for the use of volume ratio being 1:1
Solution, acetone, isopropanol, dehydrated alcohol, deionized water difference 30 min of ultrasound successively take out electrode member in beaker A simultaneously
It is put into beaker B with deionized water flushing, then deionized water sealer is injected into beaker B and saves.The electrode member of cleaning
Before use, rinsing and drying the liquid of removal surface residual well using deionized water, dehydrated alcohol.
In step (2), electrode member conducting surface slowly enters in solution perpendicular to solution surface, when solution is just by electrode
Electrode member is slowly left into solution when being totally submerged.
In step (3), preferentially beaker is placed on weighing balance and weighs 0.018 M polyethyleneimine, then in magnetic force
Under stirring, 40 ml deionized waters are injected into beaker, then successively weigh 0.055 M hexamethylenetetramine and 0.05 M six directions water
Zinc nitrate is added in solution, and 30 min are stirred under 600 r/min revolving speeds, obtains uniform clear solution.
The beneficial effects of the present invention are: the FTO electro-conductive glass of photoetching treatment has cost as gas sensing electrode element
It is low, stability is good, is easy to the advantages that gas sensitive growth in situ；The ZnO nano cluster array growth in situ of morphological rules is in electrode
Element surface overcomes traditional knife coating and carries out that destructible material morphology when air-sensitive test, coating thickness is uneven, particle is easy
Reunion, material contact the disadvantages of bad with electrode；Gained gas sensor is had excellent performance, and is shown to multiple gases higher
Sensitivity and quickly response resume speed, and there is good repeated (i.e. long service life).Prepared by the present invention with
Photoetching treatment FTO electro-conductive glass is that the ZnO nano cluster gas sensor of electrode member is low with production cost, preparation process is simple
Many advantages, such as single, air-sensitive performance protrudes, and stability is good, is a kind of novel gas sensor with applications well prospect.
Detailed description of the invention
Fig. 1 be embodiment 1 in photoetching treatment FTO electro-conductive glass structural schematic diagram, wherein 1 for by theoretical modeling with
The litho pattern of interdigital shape designed by experimental analysis；2 be the interdigital width of fringe of litho pattern；3 be the fork of litho pattern
Refer to fringe spacing.
Fig. 2 is X-ray diffraction (XRD) spectrogram of ZnO nano cluster array prepared by embodiment 1.
Fig. 3 is that the scanning electron microscope (SEM) of 1000 multiple of amplification of ZnO nano cluster array prepared by embodiment 1 is shone
Piece.
Fig. 4 is scanning electron microscope (SEM) photo of the partial enlargement of ZnO nano cluster array prepared by embodiment 1.
Fig. 5 is response of the gas sensor at 390 DEG C of operating temperature to 100 ppm gas with various prepared by embodiment 1
Recovery curve figure.
Fig. 6 is that gas sensor prepared by embodiment 1 is tested to the difference of 100 ppm concentration at 390 DEG C of operating temperature
The sensitivity of gas.
Specific embodiment
Embodiment 1, using the FTO electro-conductive glass of photoetching treatment as the preparation process of electrode member growth in situ ZnO nano cluster
And its air-sensitive performance test.
The preparation process of gas sensor carries out as steps described below:
(1) 0.05 M Zinc diacetate dihydrate, 0.05 M ethylene glycol amine and appropriate ethanol solution is taken to prepare laminar solution；
(2) electrode member is passed in and out into laminar solution twice with the speed of 1 ~ 3 mm/s using self-control lifting motor, it then will be electric
Pole element is being to be dried overnight at room temperature, is then placed in Muffle furnace and anneals 10 at 400 DEG C with the heating rate of 5 DEG C/min
Min, the above process, which is repeated twice, obtains uniform ZnO seed layer；
(3) polyethyleneimine of the zinc nitrate hexahydrate compound of 0.05 M, the hexamethylenetetramine of 0.055 M, 0.018 M are taken
(molecular weight 600) and suitable deionized water solution configure hydro-thermal reaction precursor liquid；
(4) the FTO electrode member for growing seed layer and reaction precursor liquid are moved into polytetrafluoroethylliner liner, then puts liner
Enter in water heating kettle and be sealed, water heating kettle is put into drying box at 95 DEG C and reacts 6 h.It is cooled to room temperature to the end of reacting,
It takes out FTO electrode member and places into 60 DEG C of 2 h of drying in drying box with deionized water and ethyl alcohol repeated flushing；
(5) prepared gas sensor is placed on the pedestal of air-sensitive test macro, adjust test probe position, make its with
Gas sensor both ends well contact and form access.Then test temperature is set, the tested gas for being passed through suitable concentration can be into
The quick test of promoting the circulation of qi.
Fig. 2 gives the XRD spectra for the ZnO nano cluster being grown on FTO electrode, it can be seen that each diffraction maximum is sharper
Sharp, this illustrates that ZnO nano cluster has good crystallinity, and the JCPDS 36- of the position of XRD diffraction maximum and hexagonal phase ZnO
1451 cards are corresponding, it was demonstrated that the ZnO nano cluster of preparation has hexagonal phase crystal structure.Fig. 3, Fig. 4 give ZnO nano cluster
The SEM of low power and partial enlargement figure, it can be seen that prepared ZnO material has tufted pattern, they are mutual by more roots and tops
The ZnO nanorod of contact is constituted, and hexagonal phase ZnO nano cluster has the top of hexagon, and diameter and distribution of lengths are uniform, table
Face is smooth, and corner angle are clearly demarcated, has aspect ratio outstanding and specific surface area.Fig. 5, Fig. 6 give gas sensing prepared by the present invention
Device is at 390 DEG C of operating temperature to the response recovery curve figure and sensitivity map of 500 ppm gas with various, it can be seen that this hair
Bright prepared gas sensor responds multiple gases with air-sensitive, and sensitivity with higher and quickly response restore speed
Degree, and highest sensitivity is shown to H2S gas, these excellent performances show it will well in gas sensing field
Development and application prospect.
Embodiment 2, using the FTO electro-conductive glass that photoetching fringe spacing is 30 μm as electrode member growth in situ ZnO nano cluster
Preparation process and its air-sensitive performance test.
The preparation process of gas sensor carries out as steps described below:
(1) 0.05 M Zinc diacetate dihydrate, 0.05 M ethylene glycol amine and appropriate ethanol solution is taken to prepare laminar solution；
(2) electrode member is passed in and out into laminar solution twice with 1 mm/s speed using self-control lifting motor, it then will be electric
Pole element is being to be dried overnight at room temperature, is then placed in Muffle furnace and anneals 10 at 400 DEG C with the heating rate of 5 DEG C/min
Min, the above process, which is repeated twice, obtains uniform ZnO seed layer；
(3) polyethyleneimine of the zinc nitrate hexahydrate compound of 0.05 M, the hexamethylenetetramine of 0.055 M, 0.018 M are taken
(molecular weight 600) and suitable deionized water solution configure hydro-thermal reaction precursor liquid；
(4) the FTO electrode member for growing seed layer and reaction precursor liquid are moved into polytetrafluoroethylliner liner, then puts liner
Enter in water heating kettle and be sealed, water heating kettle is put into drying box at 95 DEG C and reacts 6 h.It is cooled to room temperature to the end of reacting,
It takes out FTO electrode member and places into 60 DEG C of 2 h of drying in drying box with deionized water and ethyl alcohol repeated flushing.
We are successfully prepared for ZnO nano cluster as electrode member using the FTO electro-conductive glass that photoetching fringe spacing is 30 μm
Array gas sensor, and achieve preferable air-sensitive performance.
Embodiment 3, the FTO electro-conductive glass for being 30 μm using photoetching fringe spacing change ZnO seed layer as electrode member
Pull rate in preparation process grows the preparation process and its air-sensitive performance test of ZnO nano cluster.
The preparation process of gas sensor carries out as steps described below:
(1) 0.05 M Zinc diacetate dihydrate, 0.05 M ethylene glycol amine and appropriate ethanol solution is taken to prepare laminar solution；
(2) electrode member is passed in and out into laminar solution twice with the speed of 3 mm/s using self-control lifting motor, then by electrode
Element is being to be dried overnight at room temperature, is then placed in Muffle furnace and anneals 10 at 400 DEG C with the heating rate of 5 DEG C/min
Min, the above process, which is repeated twice, obtains uniform ZnO seed layer；
(3) polyethyleneimine of the zinc nitrate hexahydrate compound of 0.05 M, the hexamethylenetetramine of 0.055 M, 0.018 M are taken
(molecular weight 600) and suitable deionized water solution configure hydro-thermal reaction precursor liquid；
(4) the FTO electrode member for growing seed layer and reaction precursor liquid are moved into polytetrafluoroethylliner liner, then puts liner
Enter in water heating kettle and be sealed, water heating kettle is put into drying box at 95 DEG C and reacts 6 h.It is cooled to room temperature to the end of reacting,
It takes out FTO electrode member and places into 60 DEG C of 2 h of drying in drying box with deionized water and ethyl alcohol repeated flushing.
The FTO electro-conductive glass that we are 30 μm using photoetching fringe spacing is 3 mm/s feelings in pull rate as electrode member
Under condition, it is successfully prepared for ZnO nano cluster array gas sensor, which is likewise supplied with good air-sensitive performance.
Claims (4)
1. a kind of using the FTO electro-conductive glass of photoetching treatment as the ZnO nano cluster gas sensor of electrode member, it is characterised in that:
The gas sensor is by situ on carrying out the FTO conductive glass electrode element after specific pattern and line width photoetching treatment
ZnO nano cluster array is grown to obtain, wherein ZnO nano cluster array is uniform, is grown on FTO gas sensing electrode element surface in an orderly manner,
A diameter of 70 ~ 100 nm, length are 2 ~ 3.5 μm, and crystal structure is hexagonal wurtzite structure.
2. gas sensing electrode element according to claim 1, it is characterized in that: the material of the electrode member is Fluorin doped dioxy
Change tin electro-conductive glass (FTO electro-conductive glass).
3. gas sensing electrode element according to claim 1, the laser ablation figure is interdigitated, wherein between interdigital striped
Away from being 20 ~ 80 μm, interdigital width of fringe is 300 ~ 500 μm, and laser ablation depth is 0.5 ~ 1 μm.
4. the preparation method of gas sensor according to claim 1, it is characterized in that:
Using 0.5 M Zinc diacetate dihydrate and the ethanol solution of 0.5 M ethylene glycol amine as laminar solution；Motor is lifted using self-control
It twice with the speed disengaging laminar solution of 1 ~ 3 mm/s by electrode member, is being then to do overnight at room temperature by electrode member
It is dry, it is then placed in Muffle furnace and is annealed at 400 DEG C 10 min with the heating rate of 5 DEG C/min, the above process is repeated twice
Obtain uniform ZnO seed layer；With the zinc nitrate hexahydrate compound of 0.05 M, the hexamethylenetetramine and 0.018 M of 0.055 M
Polyethyleneimine (molecular weight 600) aqueous solution be hydro-thermal reaction precursor liquid；By grow seed layer FTO electrode member and
Reaction precursor liquid moves into polytetrafluoroethylliner liner, and then liner is put into water heating kettle and is sealed, water heating kettle is put into dry
6 h are reacted in dry case at 95 DEG C；It is cooled to room temperature to the end of reacting, FTO electrode member is taken out, with deionized water and ethyl alcohol
Repeated flushing places into 60 DEG C of 2 h of drying in drying box, can carry out air-sensitive test.
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Application publication date: 20190621 |
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