CN104792827A - Self-powered humidity sensor adopting antimony doped zinc oxide nano array and preparation method of self-powered humidity sensor - Google Patents
Self-powered humidity sensor adopting antimony doped zinc oxide nano array and preparation method of self-powered humidity sensor Download PDFInfo
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- CN104792827A CN104792827A CN201510157994.2A CN201510157994A CN104792827A CN 104792827 A CN104792827 A CN 104792827A CN 201510157994 A CN201510157994 A CN 201510157994A CN 104792827 A CN104792827 A CN 104792827A
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- zinc oxide
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Abstract
The invention aims to solve the problem of low sensitivity of a pure zinc oxide sensor in the prior art, provides a self-powered humidity sensor adopting an antimony doped zinc oxide nano array and a preparation method of the self-powered humidity sensor, and belongs to the field of self-powered active gas sensors. The provided humidity sensor comprises a humidity sensing element, electrodes and frames, wherein the humidity sensing element adopts a zinc oxide nano array which grows on a titanium chip and has the antimony atom doping molar content of 0.8%-1.6%. The preparation method of the self-powered humidity sensor comprises the following steps: an antimony ion doping liquid is added to a zinc nitrate solution, and ammonia water is added dropwise; the clean titanium chip is immersed into the solution, and the humidity sensing element adopting the antimony doped zinc oxide nano array which grows on the titanium chip is obtained; finally, the crude antimony doped zinc oxide nano array, aluminum foil and polyimide films are assembled together. The sensitivity of the humidity sensor prepared with the method is improved substantially when compared with a zinc oxide nanowire, and the humidity sensor is a gas sensor which has the self-powered characteristic and does not require external electric energy.
Description
Technical field
The invention belongs to self energizing active gas sensor field, particularly a kind of stibium-doped zinc oxide nano-array self energizing humidity sensor and preparation method thereof.
Background technology
Humidity sensor is significant in commercial production and daily life, and traditional humidity sensor depends on the change of electric capacity or resistance usually, needs external power source to provide energy.Its wet sensitive original paper mainly contains hygristor and the large class of humicap two, but all there is the shortcoming of poor linearity, and measuring resistance or electric capacity generally need a Circuits System, and this makes whole moisture measurement need a lot of additional device, complex structure energy consumption high.Except resistance-type, capacitive moisture sensor, also have electrolyte ion type humidity-sensitive element, weight humidity-sensitive element (utilizing the change of humidity-sensitive film weight to change oscillation frequency), light intensity type humidity-sensitive element, surface acoustic wave humidity photosensitive elements etc.Under the overall background of 21 century energy crisis, a kind of can collect neighbouring environmental energy for self work provide the new ideas device of power supply to be suggested---self energizing sensor.Simultaneously under the theory economized on resources, a lot of product all towards miniaturization development, makes nanometer technology obtain develop rapidly.In recent years, by piezoelectricity and the gas sensing characteristics of coupled oxidation zinc nano-array, achieve a self energizing gas sensor without the need to any external electric energy first, the piezoelectricity output voltage of this device provides energy simultaneously also as gas sensing signal for devices function.
But this sensor still exists certain defect, as gas-selectively, piezoelectric voltage can further improve, and wherein comparing distinct issues is exactly that the susceptibility of pure zinc oxide sensor is also lower, is difficult to practical application.
Summary of the invention
The object of the invention is the problem that susceptibility in order to solve the pure zinc oxide sensor existed in above-mentioned prior art is low, provide a kind of stibium-doped zinc oxide nano-array self energizing humidity sensor and preparation method thereof, the humidity inductive original paper of this sensor is the zinc oxide nanowire of Sb doped, and its sensitivity comparatively zinc oxide nanowire is improved largely; And having self-energizing characteristic, is a kind of self energizing gas sensor without the need to any external electric energy.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework;
Wherein, described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 0.8% ~ 1.6% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton.
Present invention also offers the preparation method of above-mentioned humidity sensor, comprise the steps:
(1) get ethanol in proper amount acid, NaOH and antimony acetate, add deionized water, be mixed with antimony ion doping liquid; Get appropriate zinc nitrate hexahydrate again, add deionized water, after dissolving, in zinc nitrate solution, add antimony ion doping liquid, more dropwise add ammoniacal liquor;
Wherein, described antimony acetate molal quantity accounts for 0.8 ~ 1.6% of antimony acetate and zinc nitrate hexahydrate total mole number; The mol ratio of described glycollic acid and NaOH is 1:1, and is 10 ~ 14 times of antimony acetate molal quantity; In described antimony ion doping liquid, antimony ion concentration is 18 ~ 22mmol/L; Described zinc nitrate solution concentration is 0.035 ~ 0.045mol/L; The mol ratio of described ammoniacal liquor and zinc nitrate hexahydrate is 15 ~ 20:1;
(2) titanium sheet of cleaning is immersed in above-mentioned solution, again solution be heated to 70 ~ 80 DEG C and keep 24 ~ 36 hours, then taking out titanium sheet, with deionized water and ethanol purge, last dry under 50 ~ 70 DEG C of environment, obtain growing the stibium-doped zinc oxide nano-array in titanium sheet;
(3) namely humidity inductive original paper is grown the stibium-doped zinc oxide nano-array in titanium sheet, electrode aluminium foil and framework Kapton fit together.
The principle of work of stibium-doped zinc oxide nano-array self energizing humidity sensor is that under low humidity, hydrone is chemisorbed on nanowire surface rapidly, and creates hydroxide ion on surface.Sb
3+ion causes high concentration charged region and the highfield of local, and many Lacking oxygen are Water Molecular Adsorption provides good position.After the water molecule layer of ground floor chemisorption is formed, the hydrone of next absorption is physisorption.Because chemisorbed layer has highfield, the hydrone of physisorption is ionized to H
3o
+and OH
-ion.By Grote recklessly this chain reaction and proton by H
3o
+be discharged on contiguous hydrone and can carry out charge-conduction.H
3o
+be present in the effect that act as charge carrier in the hydrone of physisorption on nano wire.When device is under pressure, H in water layer
3o
+with the piezoelectric polarization electric charge in the free electron meeting displacement screen nano line of nano wire inside, the voltage reducing device further exports.When device at high humidity, more Water Molecular Adsorption is in nanowire surface.Define physisorption water layer, its impact by chemisorption internal layer weakens.As a result, can freely move in physisorption water layer according to this principle proton of Grote Hu.When the device under high humility is under pressure, the H of water layer middle and high concentration
3o
+/ H
+ion can produce a very strong shielding action, and the piezoelectricity of device exports can significant step-down.
Sb doped amount prepared by said method is the zinc oxide nano array self energizing humidity sensor of 1.6%, detected by test macro, in humidity 20%, 30%, 40%, 50%, 60%, 70% situation, humidity sensor sensitivity is respectively 20.0,34.8,44.4,60.0,71.9 and 83.7.
The present invention compared with prior art, has following advantage:
1, the sensitivity of stibium-doped zinc oxide nano-array comparatively zinc oxide nanowire be improved largely.So excellent performance can owing to the gas piezoelectricity coupling mechanism of zinc oxide nanowire and antimony (Sb
3+) adulterate a large amount of Lacking oxygen caused, when pressure acts on zinc oxide nano array, the piezoelectric polarization electric charge produced by c-axis deformation can drive electron motion in external loop (piezoelectricity output), the free electron of zinc oxide nanowire inside can reduce piezoelectricity and exports by the piezoelectric polarization electric charge (piezoelectricity shielding effect) in partly shielding effect nano wire, because Sb doped creates more Lacking oxygen, a large amount of Lacking oxygen can provide more position for the absorption of hydrone, thus improves sensitivity.
2, stibium-doped zinc oxide nano-array of the present invention is by wet-layer preparation, and the method technique is simple, easy and simple to handle, pollutes little, is applicable to suitability for industrialized production.
3, the sensing elements prepared due to the present invention has nanoscale structures, and the diameter of nanometer rods is tens nanometers.Make device have the activity on sizable specific surface area and these surfaces very high, than initial devices, there is higher susceptibility, can light concentration gas be detected.
4, humidity sensor of the present invention is using piezoelectric voltage as gas sensing signal, the size of the direct corresponding charge carrier of output voltage values and gas concentration, the good fast response time of the linearity.
Accompanying drawing explanation
Fig. 1, stibium-doped zinc oxide nanometer self energizing humidity sensor structural representation;
Wherein, 1, Kapton, 2, aluminium foil, 3, the stibium-doped zinc oxide nano-array grown in titanium sheet, 4, copper conductor, 5, hydrone;
Fig. 2, stibium-doped zinc oxide nanometer self energizing humidity sensor schematic front view
Fig. 3, humidity sensor test macro sketch;
Wherein, 6, step motor, 7, hammer;
Fig. 4, the embodiment of the present invention 3 pictorial diagram;
Fig. 5, scanning electron microscope vertical view;
Wherein, Fig. 5 a is pure zinc oxide nano-array, Fig. 5 b to be Sb doped concentration be 0.8% zinc oxide nano array, Fig. 5 c to be Sb doped concentration be 1.6% zinc oxide nano array;
Fig. 6, Sb doped concentration are the zinc oxide nano array sectional drawing of 1.6%;
Fig. 7, Sb doped concentration are the single zinc oxide nano rod transmission electron microscope figure of 1.6%;
Fig. 8, Sb doped concentration are high-resolution-ration transmission electric-lens and the electronics selected diffraction figure of the single zinc oxide nano rod of 1.6%;
Fig. 9, Sb doped concentration are the energy spectrogram of the zinc oxide nano array of 1.6%;
Figure 10, Sb doped concentration are the X-ray diffractogram of the zinc oxide nano array of 1.6%;
Figure 11, pure zinc oxide and Sb doped concentration are the spectrogram of the zinc oxide nano array of 1.6%;
Under Figure 12, different humidity, Sb doped concentration is the voltage output of the zinc oxide nano array humidity sensor of 1.6%;
Under Figure 13, different humidity, Sb doped concentration is the voltage output enlarged drawing of the zinc oxide nano array humidity sensor of 1.6%;
Wherein, Figure 13 a is that under 10% humidity, voltage exports enlarged drawing, and Figure 13 b is that under 70% humidity, voltage exports enlarged drawing;
Figure 14, pure zinc oxide and Sb doped concentration are the sensitivity of zinc oxide nano array humidity sensor under different humidity of 1.6%.
Embodiment
The raw material used in following examples is commercial, and Kapton is Du Pont Kapton film, and ammonia concn is with NH
3count 13.8mol/L.
Test macro, as Fig. 3, connects copper conductor at sensor two ends, and applied on a sensor by pressure (34N, 2.7Hz) by stepper motor, piezoelectricity output voltage is measured by low-noise preamplifier (model SR560, Stamford Study system).
Embodiment 1
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework; Described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 0.8% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton film.This humidity sensor structural drawing as depicted in figs. 1 and 2.
Its preparation method is:
(1) first get 0.76g glycollic acid to be dissolved in 50mL deionized water, then add 0.40g NaOH and 0.30g antimony acetate and be mixed with antimony ion doping liquid, its antimony ion concentration is 20mmol/L; Get 1.476g zinc nitrate hexahydrate again and add 110mL deionized water, after dissolving, add 2mL antimony ion doping liquid, more dropwise add 5mL ammoniacal liquor;
(2) titanium sheet clean through ultrasonic cleaning is immersed in above-mentioned solution, again solution be heated to 70 DEG C and keep 36 hours, then titanium sheet is taken out, with deionized water and ethanol purge, last dry under 50 DEG C of environment, obtain the humidity inductive original paper of the stibium-doped zinc oxide nano-array grown in titanium sheet; The scanning electron microscope vertical view of 0.8% obtained stibium-doped zinc oxide nano-array is shown in Fig. 5 .b;
(3) by the stibium-doped zinc oxide nano-array of growth in titanium sheet, aluminium foil and Kapton film fit together.
Embodiment 2
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework; Described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 1.2% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton film.
Its preparation method is:
(1) first get 0.912g glycollic acid to be dissolved in 50mL deionized water, then add 0.48g NaOH and 0.30g antimony acetate and be mixed with antimony ion doping liquid, its antimony ion concentration is 20mmol/L; Get 1.470g zinc nitrate hexahydrate again and add 123.5mL deionized water, after dissolving, add 3mL antimony ion doping liquid, more dropwise add 6mL ammoniacal liquor;
(2) titanium sheet clean through ultrasonic cleaning is immersed in above-mentioned solution, again solution be heated to 75 DEG C and keep 30 hours, then titanium sheet is taken out, with deionized water and ethanol purge, last dry under 70 DEG C of environment, obtain the humidity inductive original paper of the stibium-doped zinc oxide nano-array grown in titanium sheet;
(3) by the stibium-doped zinc oxide nano-array of growth in titanium sheet, aluminium foil and Kapton film fit together.
Embodiment 3
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework; Described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 1.6% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton film.
Its preparation method is:
(1) first get 1.064g glycollic acid to be dissolved in 50mL deionized water, then add 0.56g NaOH and 0.30g antimony acetate and be mixed with antimony ion doping liquid, its antimony ion concentration is 20mmol/L; Get 1.464g zinc nitrate hexahydrate again and add 141mL deionized water, after dissolving, add 4mL antimony ion doping liquid, more dropwise add 7mL ammoniacal liquor;
(2) titanium sheet clean through ultrasonic cleaning is immersed in above-mentioned solution, again solution be heated to 80 DEG C and keep 24 hours, then titanium sheet is taken out, with deionized water and ethanol purge, last dry under 60 DEG C of environment, obtain the humidity inductive original paper of the stibium-doped zinc oxide nano-array grown in titanium sheet; The optical photograph figure of this sensor is shown in Fig. 4.
(3) by the stibium-doped zinc oxide nano-array of growth in titanium sheet, aluminium foil and Kapton film fit together.
The scanning electron microscope vertical view of the zinc oxide nano array of 1.6% Sb doped that the present embodiment obtains is shown in Fig. 5 .c, can see, nano-array grows very neat, Sb doped concentration be the mean diameter of the zinc oxide nano array of 1.6% be approximately 100nm and its mean diameter with doping content raise and reduce.The sectional drawing of Fig. 6 to be Sb doped concentration be zinc oxide nano array of 1.6%, can find out that its average length is about 3 μm.The transmission electron microscope picture of Fig. 7 to be Sb doped concentration be zinc paste single nano-wire of 1.6%, its high-resolution-ration transmission electric-lens figure is Fig. 8, grating constant is 002 of the corresponding zinc paste of 0.26nm, and electronics selected diffraction figure (in Fig. 8 illustration) further demonstrates nano wire well-crystallized.Fig. 9 to be Sb doped concentration be zinc oxide nano array of 1.6% can spectrogram, demonstrate and there are four kinds of elements (O, Zn, Ti and Sb) in this region.As shown in Figure 10, the diffraction peak in figure corresponds to hexagonal Wurzite structure and the Ti crystal of zinc paste to its X-ray diffractogram, does not find other assorted peak, illustrates that antimony atoms is introduced into instead type doping way and do not change mother crystal structure.The room temperature spectrum of pure zinc oxide and stibium-doped zinc oxide nano-array is as Figure 11, the spectrogram of pure zinc oxide mainly comprises a strong burst of ultraviolel peak and a weak excited by visible light peak, the optical excitation in Uv and visible light district respectively can owing to the compound of the intrinsic excitation of zinc paste and photohole and zinc oxide surface Lacking oxygen electronics, to stibium-doped zinc oxide nano-array, the obvious step-down of the intensity of burst of ultraviolel simultaneously excited by visible light significantly strengthens, and demonstrates because Sb doped result in a large amount of Lacking oxygen on the surface of nano-array.
By the systems axiol-ogy after tested of the humidity sensor in the present embodiment, Figure 12 represents that the voltage of 1.6% stibium-doped zinc oxide nano-array under uniform pressure different humidity exports, and the output voltage of device is respectively 1.35,1.08,0.88,0.75,0.54,0.38 and 0.22V for 10%, 20%, 30%, 40%, 50%, 60%, 70% time in humidity.Figure 13 a and b is respectively the enlarged drawing of humidity 10% and 70% time voltage output.The sensitivity of this humidity sensor can simply be defined as follows:
Wherein V
0and V
tvoltage under being respectively humidity 10% time voltage and measuring humidity, as Figure 14, its sensitivity is respectively 20.0,34.8,44.4,60.0,71.9 and 83.7 20%, 30%, 40%, 50%, 60%, 70% time in humidity, meanwhile, the sensitivity of pure zinc oxide is then only respectively 6.3,9.9,10.8,12.5,17.5 and 23.9, from data, stibium-doped zinc oxide nano-array highly sensitive in pure zinc oxide nano-array.
Embodiment 4
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework; Described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 1.0% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton film.
Embodiment 5
A kind of stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, electrode and framework; Described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet, and the molar content of antimony atoms is 1.4% of antimony atoms and zinc atom molal quantity summation; Described electrode is aluminium foil; Described framework is Kapton film.
Claims (4)
1. a stibium-doped zinc oxide nano-array self energizing humidity sensor, comprises humidity inductive original paper, and electrode and framework, is characterized in that, described humidity inductive original paper is the stibium-doped zinc oxide nano-array of growth in titanium sheet; Described electrode is aluminium foil; Described framework is Kapton.
2. a kind of stibium-doped zinc oxide nano-array self energizing humidity sensor according to claim 1, is characterized in that, in described stibium-doped zinc oxide nano-array, the molar content of antimony atoms doping is 0.8% ~ 1.6%.
3. a preparation method for stibium-doped zinc oxide nano-array self energizing humidity sensor, is characterized in that, comprise the steps:
(1) get ethanol in proper amount acid, NaOH and antimony acetate, add deionized water, be mixed with antimony ion doping liquid; Get appropriate zinc nitrate hexahydrate again, add deionized water, after dissolving, in zinc nitrate solution, add antimony ion doping liquid, more dropwise add ammoniacal liquor;
(2) titanium sheet of cleaning is immersed in above-mentioned solution, again solution be heated to 70 ~ 80 DEG C and keep 24 ~ 36 hours, then taking out titanium sheet, with deionized water and ethanol purge, last dry under 50 ~ 70 DEG C of environment, obtain growing the stibium-doped zinc oxide nano-array in titanium sheet;
(3) by the stibium-doped zinc oxide nano-array of growth in titanium sheet, aluminium foil and Kapton fit together.
4. the preparation method of a kind of stibium-doped zinc oxide nano-array self energizing humidity sensor according to claim 3, it is characterized in that, the molal quantity of described antimony acetate accounts for 0.8 ~ 1.6% of antimony acetate and zinc nitrate hexahydrate total mole number; The mol ratio of described glycollic acid and NaOH is 1:1, and is 10 ~ 14 times of antimony acetate molal quantity; The mol ratio of described ammoniacal liquor and zinc nitrate hexahydrate is 15 ~ 20:1.
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Cited By (7)
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| CN106018498A (en) * | 2016-07-28 | 2016-10-12 | 电子科技大学 | Self-powdered sensor for detecting automobile tail gas and preparation method thereof |
| CN106153690A (en) * | 2016-07-28 | 2016-11-23 | 电子科技大学 | A kind of self energizing sensor for alcohol detection and preparation method thereof |
| CN107179337A (en) * | 2017-05-25 | 2017-09-19 | 郑州大学 | A kind of bimodulus humidity sensor and preparation method thereof |
| CN107817273A (en) * | 2016-09-14 | 2018-03-20 | 河北工业大学 | The preparation method of aluminium, Ti doped Zinc oxide-base acetone gas sensor |
| WO2021092681A1 (en) * | 2019-11-12 | 2021-05-20 | Aquasensing Incorporated | Moisture, gas and fluid-enabled sensors |
| CN112924492A (en) * | 2021-03-18 | 2021-06-08 | 电子科技大学 | Self-powered humidity sensor based on composite spinning film and preparation method thereof |
| CN113834862A (en) * | 2021-09-17 | 2021-12-24 | 电子科技大学 | Method for regulating and controlling interface stress/enhancing sensitivity of self-driven flexible gas sensor |
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| CN106018498A (en) * | 2016-07-28 | 2016-10-12 | 电子科技大学 | Self-powdered sensor for detecting automobile tail gas and preparation method thereof |
| CN106153690A (en) * | 2016-07-28 | 2016-11-23 | 电子科技大学 | A kind of self energizing sensor for alcohol detection and preparation method thereof |
| CN106018498B (en) * | 2016-07-28 | 2018-07-10 | 电子科技大学 | It is a kind of for self energizing sensor of automobile emission gas analyzer and preparation method thereof |
| CN106153690B (en) * | 2016-07-28 | 2018-08-14 | 电子科技大学 | A kind of self energizing sensor and preparation method thereof for alcohol detection |
| CN107817273A (en) * | 2016-09-14 | 2018-03-20 | 河北工业大学 | The preparation method of aluminium, Ti doped Zinc oxide-base acetone gas sensor |
| CN107179337A (en) * | 2017-05-25 | 2017-09-19 | 郑州大学 | A kind of bimodulus humidity sensor and preparation method thereof |
| WO2021092681A1 (en) * | 2019-11-12 | 2021-05-20 | Aquasensing Incorporated | Moisture, gas and fluid-enabled sensors |
| CN112924492A (en) * | 2021-03-18 | 2021-06-08 | 电子科技大学 | Self-powered humidity sensor based on composite spinning film and preparation method thereof |
| CN113834862A (en) * | 2021-09-17 | 2021-12-24 | 电子科技大学 | Method for regulating and controlling interface stress/enhancing sensitivity of self-driven flexible gas sensor |
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