CN100580440C - Nano zinc oxide film gas sensor and method for preparing same - Google Patents
Nano zinc oxide film gas sensor and method for preparing same Download PDFInfo
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- CN100580440C CN100580440C CN200610026264A CN200610026264A CN100580440C CN 100580440 C CN100580440 C CN 100580440C CN 200610026264 A CN200610026264 A CN 200610026264A CN 200610026264 A CN200610026264 A CN 200610026264A CN 100580440 C CN100580440 C CN 100580440C
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Abstract
The disclosed nano ZnO film gas sensor comprises: a fork quartz wafer with two electrodes derivated from its rocker roots, and 50-500nm nano ZnO film with 10-100nm size on rocker. Compared to traditional frequency-form sensor by crystal oscillator, this invention has simple structure and high sensitivity, and outputs digital signal without conversion for successive application.
Description
Technical field
The present invention relates to a kind of nano zinc oxide film gas sensor and preparation method thereof, belong to the technical field of sensor and manufacturing thereof.
Background technology
Gas sensor is the senser element that is used to detect the concentration of certain specific gas, as detecting ethanol, acetone, gases such as ether.The granularity of the particulate of the sensitive material of gas sensor is more little, and specific surface area is big more, and the interaction that sensor takes place with contacting of ambient gas is big more.Nano zinc oxide film has very large specific surface area, helps the absorption of tested gas, is a kind of desirable gas sensitive material.
The tradition gas sensor all is that electric capacity waits the concentration value of expressing corresponding certain gas by the analog quantity electrical quantity such as the resistance of detection sensitive material to the gas response.The shortcoming of background technology is must carry out analog to digital conversion to the simulating signal of gas sensor sensing, and analog quantity is converted to digital quantity, just can carry out follow-up signal Processing.
Summary of the invention
An object of the present invention is to provide a kind of nano zinc oxide film gas sensor, this gas sensor has simple in structure, highly sensitive, easy to make and its output signal frequency is a digital quantity, need not to carry out analog to digital conversion, just can directly carry out the advantage of follow-up signal Processing by digital circuit.
For realizing above purpose, the present invention adopts following technical scheme.Existing accompanying drawings is as follows.
A kind of nano zinc oxide film gas sensor 5, comprise the tuning-fork-type quartz wafer, two electrode leading foots 6,7 of described tuning-fork-type quartz wafer are drawn from two root of 9 of raising one's arm respectively, it is characterized in that, raising one's arm at two, growth has Nano zinc oxide film 8 on 9, the particle grain size of described nano zine oxide is 10～100 nanometers, and the thickness of Nano zinc oxide film 8 is 50～500 nanometers.
Another object of the present invention provides the preparation method of the sensor.For realizing above purpose, the technical solution used in the present invention is that two at ready-made tuning-fork-type quartz wafer raise one's arm and are respectively the Nano zinc oxide film 8 of 10～100 nanometers and 50～500 nanometers on 9 by sol-gel process growth grain diameter and thickness.
Now describe the preparation method of gas sensor of the present invention in conjunction with the accompanying drawings in detail.
A kind of preparation method of nano zinc oxide film gas sensor 5 is characterized in that, prepares from the tuning-fork-type quartz wafer concrete operations step:
The pre-treatment of first step tuning-fork-type quartz wafer
The tuning-fork-type quartz wafer was soaked in acetone 30 minutes, used deionized water rinsing again 5 minutes, in 50 ℃ baking oven, dry at last, standby;
Second step preparation precursor liquid
In 100 milliliters of absolute ethyl alcohols with 60 ℃ of 3 gram acetate dihydrate zinc salts inputs, stirred 30 minutes, get precursor liquid;
The precursor of the 3rd one-step growth Nano zinc oxide film 8
In the precursor liquid that will make through two second steps of 9 immersions of raising one's arm of the tuning-fork-type quartz wafer that the first step is handled, mention then, in 50 ℃ baking oven, dry, the number of times of above-mentioned immersion-mention-drying course is 1～10 time, two of tuning-fork-type quartz wafer raise one's arm and have depended on one deck white film on 9, i.e. the precursor of Nano zinc oxide film 8;
The 4th step annealing, finished product
To be placed in 200～900 ℃ the baking oven annealing through the tuning-fork-type quartz wafer that the 3rd step handled 30 minutes, Nano zinc oxide film 8 is attached to two of tuning-fork-type quartz wafer and raises one's arm on 9, nano zinc oxide film gas sensor 5 finished products.
Preparation method of the present invention is further characterized in that the nominal value of the natural frequency of described tuning-fork-type quartz wafer is 32768Hz.
The principle of work of gas sensor of the present invention: two of tuning-fork-type quartz wafer Nano zinc oxide film 8 adsorbed gases on 9 of raising one's arm, cause the quality of raising one's arm of tuning-fork-type quartz wafer to produce micro-increase, the natural frequency of tuning-fork-type quartz wafer is descended, and both relations are shown below:
M is the quality of raising one's arm of tuning-fork type quartz wafer in the formula, f
0Be the natural frequency of tuning-fork-type quartz wafer, Δ m is that the raise one's arm trace of quality changes Δ f
0The trace that is the natural frequency of nano zinc oxide film gas sensor 5 changes.
The quality of the gas of nano zinc oxide film gas sensor 5 absorption is relevant with the natural frequency of nano zinc oxide film gas sensor 5.During use, nano zinc oxide film gas sensor 5 is connected in traditional crystal oscillator, replaces the crystal of control oscillation frequency.At this moment, the oscillation frequency of this oscillator is exactly the natural frequency of nano zinc oxide film gas sensor 5.After nano zinc oxide film gas sensor 5 adsorbed gases, the oscillation frequency of this oscillator will descend.The variable quantity of oscillation frequency can be used to express the quality of the tested gas of nano zinc oxide film gas sensor 5 absorption.Because the quality of gas and the concentration of gas have direct relation, so demarcate by gas concentration, can obtain the relation of the concentration value of the variable quantity of oscillation frequency and tested gas, in other words, nano zinc oxide film gas sensor 5 can be used to detect the concentration value of tested gas after gas concentration is demarcated.
Compare with background technology, the present invention has following advantage:
1, susceptibility height
The nano zine oxide that gas sensor employing particle diameter of the present invention is a Nano grade helps the absorption of gas, the susceptibility height as sensitive material.
2, follow-up signal Processing is simple and direct
Gas sensor of the present invention and traditional crystal oscillator component frequency type gas sensor.The output signal of this oscillator is exactly the transducing signal of this gas sensor, and the frequency of this transducing signal is a digital quantity, so this transducing signal only need pass through shaping, amplification, needn't pass through analog to digital conversion, just can directly carry out follow-up signal Processing for digital circuit.
Description of drawings
Fig. 1 is the structural representation of nano zinc oxide film gas sensor 5.Wherein, the 6, the 7th, the electrode leading foot of nano zinc oxide film gas sensor 5, the 8th, Nano zinc oxide film, the 9th, raise one's arm for two of the tuning-fork type quartz wafer of nano zinc oxide film gas sensor 5.
Fig. 2 is the AFM figure of the Nano zinc oxide film of gas sensor of the present invention.
Fig. 3 is the frequency type gas sensor that gas sensor of the present invention and traditional crystal oscillator are formed, and wherein, the crystal of control oscillation frequency is served as by gas sensor of the present invention.
Fig. 4 is the response curve of frequency type gas sensor sensing alcohol gas of the present invention, and wherein horizontal ordinate is the drop-out value Δ f of the frequency of the transducing signal of frequency type gas sensor output
0, unit is Hz, and ordinate is the aerial concentration value of alcohol gas, and unit is ppm.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is described in further detail.
One of preparation of embodiment 1 nano zinc oxide film gas sensor 5
Preparation is the tuning-fork-type quartz wafer of 32768Hz from the nominal value of natural frequency, the concrete operations step:
The pre-treatment of first step tuning-fork-type quartz wafer
The tuning-fork-type quartz wafer was soaked in acetone 30 minutes, used deionized water rinsing again 5 minutes, in 50 ℃ baking oven, dry at last, standby;
Second step preparation precursor liquid
In 100 milliliters of absolute ethyl alcohols with 60 ℃ of 3 gram acetate dihydrate zinc salts inputs, stirred 30 minutes, get precursor liquid;
The precursor of the 3rd one-step growth Nano zinc oxide film
In the precursor liquid that will make through two second steps of 9 immersions of raising one's arm of the tuning-fork-type quartz wafer that the first step is handled, mention then, in 50 ℃ baking oven, dry, the number of times of above-mentioned immersion-mention-drying course is 5 times, raise one's arm for two and depended on one deck white film on 9, be i.e. the precursor of Nano zinc oxide film 8;
The 4th step annealing, finished product
To be placed in 350 ℃ the baking oven annealing through the tuning-fork-type quartz wafer that the 3rd step handled 30 minutes, Nano zinc oxide film 8 is attached to two and raises one's arm on 9, get nano zinc oxide film gas sensor 5 finished products, the particle grain size of described nano zine oxide is 25～35 nanometers, and the thickness of Nano zinc oxide film 8 is 250 nanometers.
Because Nano zinc oxide film 8 is attached to two of tuning-fork-type quartz wafer and raises one's arm on 9, increased the quality of tuning-fork-type quartz wafer, make the natural frequency of the nano zinc oxide film gas sensor 5 that makes be reduced to 32509Hz.Fig. 2 shows the AFM photo that is attached to two Nano zinc oxide films 8 on 9 of raising one's arm of gained in the 4th step, and wherein, the particle diameter of nano granular of zinc oxide is 25～35 nanometers.When nano zinc oxide film gas sensor 5 detects ethanol, acetone, during gases such as ether, its natural frequency will descend.
Two of the preparation of embodiment 2 nano zinc oxide film gas sensors 5
Preparation is the tuning-fork-type quartz wafer of 32768Hz from the nominal value of natural frequency.Operation steps except for the following differences, all the other are with embodiment 1:
In the 3rd step, immerse-mention-number of times of drying course is 2 times; In the 4th step, the tuning-fork-type quartz wafer of handling through the 3rd step was placed in 200 ℃ the baking oven annealing 30 minutes, Nano zinc oxide film 8 is attached to two of tuning-fork-type quartz wafer and raises one's arm on 9, get nano zinc oxide film gas sensor 5 finished products, the particle grain size of described nano zine oxide is 10～20 nanometers, and the thickness of Nano zinc oxide film 8 is 100 nanometers.The natural frequency of the nano zinc oxide film gas sensor 5 that makes is reduced to 32700Hz.
Three of the preparation of embodiment 3 nano zinc oxide film gas sensors 5
Preparation is the tuning-fork-type quartz wafer of 32768Hz from the nominal value of natural frequency.Operation steps except for the following differences, all the other are with embodiment 1:
In the 3rd step, immerse-mention-number of times of drying course is 9 times; In the 4th step, the tuning-fork-type quartz wafer of handling through the 3rd step was placed in 800 ℃ the baking oven annealing 30 minutes, Nano zinc oxide film 8 is attached to two of tuning-fork-type quartz wafer and raises one's arm on 9, get nano zinc oxide film gas sensor 5 finished products, the particle grain size of described nano zine oxide is 90～100 nanometers, and the thickness of Nano zinc oxide film is 450 nanometers.The natural frequency of the nano zinc oxide film gas sensor 5 that makes is reduced to 32405Hz.
The frequency type gas sensor that embodiment 4 is made up of gas sensor of the present invention and traditional crystal oscillator
The circuit of the frequency type gas sensor of present embodiment as shown in Figure 3.
A kind of frequency type gas sensor of forming by nano zinc oxide film gas sensor 5 and crystal oscillator, described crystal oscillator comprises resistance R, first capacitor C 1, second capacitor C 2, the 3rd capacitor C 3 and integrated circuit (IC), the resistance of resistance R is 20 megaohms, first capacitor C 1, the electric capacity of second capacitor C 2 and the 3rd capacitor C 3 is respectively 33P, 100P and 10000P, the model of integrated circuit (IC) is 74HC04, the 1st pin of integrated circuit (IC), the 2nd pin and the 3rd pin are respectively by first capacitor C 1, second capacitor C 2 and the 3rd capacitor C 3 ground connection, the 2nd pin of integrated circuit (IC) is connected with the 3rd pin, resistance R is connected across between the 1st pin and the 2nd pin of integrated circuit (IC), it is characterized in that, the nominal value of the natural frequency of described nano zinc oxide film gas sensor 5 is 32509Hz, the electrode leading foot 6 of nano zinc oxide film gas sensor 5,7 are connected across between the 1st pin and the 2nd pin of integrated circuit (IC), and the 4th pin of integrated circuit (IC) is the output terminal of the transducing signal of described frequency type gas sensor.
When the nano zinc oxide film gas sensor 5 of frequency type gas sensor detected tested gas, the frequency of the transducing signal of the output terminal of transducing signal output descended, and its drop-out value is relevant with the concentration of tested gas.The frequency type gas sensor can be used to detect the aerial concentration of alcohol gas.For this reason, at first to carry out degree of deciding to nano zinc oxide film gas sensor 5: the response curve of the nano zinc oxide film gas sensor 5 that under various alcohol gas concentration, records, as shown in Figure 4.Simulate the relational expression of drop-out value of frequency of the transducing signal of the aerial concentration of alcohol gas and frequency type gas sensor output then according to response curve: C=83.3 Δ f
0 2-1416.6 Δ f
0, in the formula, C is the aerial concentration of alcohol gas, unit is ppm, Δ f
0Be the drop-out value of the frequency of the transducing signal of frequency type gas sensor output, unit is Hz.
The application of the frequency type gas sensor of embodiment 5 embodiment 4: measure the aerial concentration of alcohol gas
The frequency type gas sensor of embodiment 4 is used to measure the aerial concentration of alcohol gas, it is characterized in that operation steps:
The nominal value of the natural frequency of the frequency type gas sensor of first step embodiment 4 is 32509Hz, and this frequency type gas sensor is placed the air that contains tested alcohol gas;
The frequency f of the transducing signal of the frequency type gas sensor output of the second pacing amount embodiment 4, unit is Hz;
The 3rd goes on foot the drop-out value Δ f of the frequency of the transducing signal of obtaining the output of frequency type gas sensor
0, Δ f
0=f-32509, unit are Hz;
The 4th step was obtained the aerial concentration C of alcohol gas, C=83.3 Δ f
0 2-1416.6 Δ f
0, unit is ppm.
Claims (5)
1, a kind of nano zinc oxide film gas sensor (5), comprise the tuning-fork-type quartz wafer, two electrode leading foots (6,7) of described tuning-fork-type quartz wafer are drawn from the root of two raise one's arm (9) respectively, it is characterized in that, go up growth two raise one's arm (9) Nano zinc oxide film (8) is arranged, the particle grain size of described nano zine oxide is 10～100 nanometers, and the thickness of Nano zinc oxide film (8) is 50～500 nanometers.
2, the preparation method of the described nano zinc oxide film gas sensor of claim 1 (5) is characterized in that, prepares from the tuning-fork-type quartz wafer concrete operations step:
The pre-treatment of first step tuning-fork-type quartz wafer
The tuning-fork-type quartz wafer was soaked in acetone 30 minutes, used deionized water rinsing again 5 minutes, in 50 ℃ baking oven, dry at last, standby;
Second step preparation precursor liquid
In 100 milliliters of absolute ethyl alcohols with 60 ℃ of 3 gram acetate dihydrate zinc salts inputs, stirred 30 minutes, get precursor liquid;
The precursor of the 3rd one-step growth Nano zinc oxide film (8)
To immerse second through two raise one's arm (9) of the tuning-fork-type quartz wafer that the first step is handled goes on foot in the precursor liquid that makes, mention then, in 50 ℃ baking oven, dry, the number of times of above-mentioned immersion-mention-drying course is 1～10 time, depended on one deck white film on two raise one's arm (9) of tuning-fork-type quartz wafer, i.e. the precursor of Nano zinc oxide film (8);
The 4th step annealing, finished product
To be placed in 200～900 ℃ the baking oven annealing through the tuning-fork-type quartz wafer that the 3rd step handled 30 minutes, Nano zinc oxide film (8) is attached on two raise one's arm (9) of tuning-fork-type quartz wafer, nano zinc oxide film gas sensor (5) finished product.
3, the preparation method of nano zinc oxide film gas sensor according to claim 2 (5) is characterized in that, the nominal value of the natural frequency of described tuning-fork-type quartz wafer is 32768Hz.
4, a kind of frequency type gas sensor of forming by described nano zinc oxide film gas sensor of claim 1 (5) and crystal oscillator, described crystal oscillator comprises resistance (R), first electric capacity (C1), second electric capacity (C2), the 3rd electric capacity (C3) and integrated circuit (IC), the resistance of resistance (R) is 20 megaohms, first electric capacity (C1), the electric capacity of second electric capacity (C2) and the 3rd electric capacity (C3) is respectively 33P, 100P and 10000P, the model of integrated circuit (IC) is 74HC04, the 1st pin of integrated circuit (IC), the 2nd pin and the 3rd pin are respectively by first electric capacity (C1), second electric capacity (C2) and the 3rd electric capacity (C3) ground connection, the 2nd pin of integrated circuit (IC) is connected with the 3rd pin, resistance (R) is connected across between the 1st pin and the 2nd pin of integrated circuit (IC), it is characterized in that, the nominal value of the natural frequency of described nano zinc oxide film gas sensor (5) is 32509Hz, the electrode leading foot (6 of nano zinc oxide film gas sensor (5), 7) be connected across between the 1st pin and the 2nd pin of integrated circuit (IC), the 4th pin of integrated circuit (IC) is the output terminal of the transducing signal of described frequency type gas sensor.
5, the described frequency type gas sensor of claim 4 is used to measure the aerial concentration of alcohol gas, it is characterized in that operation steps:
The nominal value of the natural frequency of the described frequency type gas sensor of the first step is 32509Hz, and this frequency type gas sensor is placed the air that contains tested alcohol gas;
The frequency f of the transducing signal of this frequency type gas sensor output of the second pacing amount, unit is Hz;
The 3rd goes on foot the drop-out value Δ f of the frequency of the transducing signal of obtaining this frequency type gas sensor output
0, Δ f
0=f-32509, unit are Hz;
The 4th step was obtained the aerial concentration C of alcohol gas, C=83.3 Δ f
0 2-1416.6 Δ f
0, unit is ppm.
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| CN103245764B (en) * | 2013-05-27 | 2015-02-18 | 北京联合大学生物化学工程学院 | Nanocomposite for monitoring diethyl ether |
| CN108226233B (en) * | 2018-01-08 | 2020-01-31 | 中国工程物理研究院化工材料研究所 | Hierarchical ZnO @ ZnO nanocomposite gas-sensitive material and preparation method thereof |
| CN112345405B (en) * | 2020-09-25 | 2022-02-18 | 西安电子科技大学 | Sulfur hexafluoride gas density monitoring device and method |
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| 一种新型高性能石英音叉温度传感器. 李欣等.仪表技术与传感器，第4期. 2003 |
| 一种新型高性能石英音叉温度传感器. 李欣等.仪表技术与传感器，第4期. 2003 * |
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