CN110018204B - Method for preparing high-performance gas sensor by polyaniline carbonization method - Google Patents
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Abstract
The invention relates to a method for preparing a gas sensor array based on carbonization of hydrochloric acid doped polyaniline nano powder. The device involved in the method consists of 4 sensors, a ceramic substrate and 8 electrodes, changes of a semiconductor P, N type are caused simply by using different time of carbonization, and therefore, the difference of detection performance among the sensors is caused, and the sensitivity of the gas sensor is greatly improved. By adopting a data processing method of the radar fingerprint, the rapid (27 seconds) identification and detection of ammonia water, formaldehyde, ethanol and water vapor can be realized at room temperature (25 ℃), and the defects of low sensitivity and long recovery time of the traditional polyaniline sensor are overcome. The sensor array has the advantages of simple preparation method, non-contact identification and detection at room temperature, and greatly enhanced practicability.
Description
Technical Field
The invention relates to the field of toxic gas detection, in particular to a method for identifiably detecting toxic atmosphere.
Background
In recent years, the social economy of China is continuously developed, the consumption of agricultural mineral resources is continuously increased, and meanwhile, a large amount of toxic and harmful gas is generated, but the environmental protection of China is started late, and the environmental protection consciousness level is not high, so that the environment of daily life and production work of people is more severe, and the air pollution is more serious. The clean atmospheric environment is one of the most important conditions for people to live and is a necessary condition for ensuring normal life and health of people. Toxic gases invade the human body through various ways, cause various diseases and harm the health of the human body. Such as by direct contact with the skin, etc., by the respiratory system, and contaminated food by the digestive system. The growing situation of air pollution has attracted public and national high attention, so that the country also issues a series of laws and regulations to prevent and treat air pollution. The detection of harmful gases such as formaldehyde and benzene series released by home decoration, furniture and automobile interior decoration in daily life, the detection of various harmful gas leakage in industrial production process, the real-time monitoring of toxic and harmful gas in explosion accident site, and the like become important research subjects. For example, the method can realize high-efficiency early warning and real-time monitoring of various on-site polluted gases such as ammonia water, formaldehyde, ethanol and the like, and is also the basic work of environmental protection. Therefore, we have sought to find a low-cost, high-response, and environmentally-friendly gas detection sensor for detecting various toxic and harmful gases. The ammonia water and formaldehyde have great harm to human health. Formaldehyde is a toxic gas, colorless, readily soluble in water, and has an irritating odor. Formaldehyde is ubiquitous in daily life and is often found in furniture, clothing and industrial production. Inhalation of formaldehyde gas can cause burning sensation in eyes and throat and even difficulty in breathing. When formaldehyde concentrations are too high and inhaled for a long time, it can lead to more serious lung disease and even cancer. As early as 2017, at 27.10 months, formaldehyde appears in the carcinogen list published by the world health organization international cancer research institute. Ammonia is of considerable importance to living beings on earth, and is an important component of many foods and fertilizers, as well as a direct or indirect component of all drugs. Ammonia has a wide range of applications, but also has many dangerous properties, ammonia is a toxic gas, the inhalation of ammonia also can harm the health, and when high-concentration ammonia is inhaled, the injury of trachea and bronchial mucosa and even emphysema can be caused. Ammonia is also an important raw material for manufacturing nitric acid, chemical fertilizers and explosives, and is very likely to be used for terrorist attacks due to the very high explosiveness of the ammonia. Therefore, the detection and real-time monitoring of ammonia gas, a highly toxic gas, are very important in the fields of industry, agriculture, medical treatment, and even social safety hazard investigation, so that a gas sensor which better meets the actual situation and is more economical and effective is urgently needed to detect the gases.
In recent years, measurement and detection technology based on a resistance type gas sensor is rapidly developed, and a new thought and method are provided for gas detection. Doped polyaniline is commonly used for detecting strong acid and strong alkali gases, the conductivity of polyaniline before carbonization is poor, high selectivity and low power consumption are two important indexes for measuring the performance of a resistance type gas sensor, and carbonized polyaniline has higher selectivity and sensitivity, so that the identification detection of the gases except the strong acid and the strong alkali gases at room temperature is realized.
Disclosure of Invention
The invention aims to provide a preparation method of a gas sensor array based on hydrochloric acid doped polyaniline carbonized nano powder. The device involved in the method consists of 4 sensors, a ceramic substrate and 8 electrodes, changes of surface states and electron depletion layers are simply caused by different carbonization time, and detection performance differences among the sensors are caused, and the identification and detection of ammonia water, formaldehyde, ethanol and water vapor can be realized at room temperature (25 ℃) by adopting a data processing method of a radar fingerprint.
The invention relates to a method for preparing a gas sensor array based on carbonized hydrochloric acid doped polyaniline nanopowder, which comprises the following steps:
preparation of the gas sensitive material:
a. dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to a molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b for about 24 hours at the temperature of 25 ℃ to obtain polyaniline nano powder doped with hydrochloric acid;
d. and c, dividing the hydrochloric acid doped polyaniline nano powder obtained in the step c into four parts, taking out three parts, respectively putting into a chemical vapor deposition furnace, and carbonizing for 1h, 3h and 5h under the protection of introduced nitrogen.
Preparing a resistance type gas sensor array:
e. and d, dispersing the hydrochloric acid doped polyaniline nano powder obtained in the steps c and d in deionized water, grinding for 10 minutes to obtain 4 parts of hydrochloric acid doped polyaniline nano paste, uniformly coating the hydrochloric acid doped polyaniline nano paste on the first sensor, the second sensor, the third sensor and the fourth sensor respectively, and drying for 24 hours at room temperature to form the gas sensor array.
The gas sensor array with the nano structure obtained by carbonizing the polyaniline doped with hydrochloric acid by the method has the function of detecting toxic atmosphere containing ammonia water, formaldehyde, ethanol and water vapor, and can change a polyaniline P-type semiconductor into an N-type semiconductor after carbonization.
The invention aims to provide a preparation method of a gas sensor array based on carbonized hydrochloric acid doped polyaniline nanopowder. The device involved in the method consists of a first sensor, a second sensor, a third sensor and a fourth sensor, a ceramic substrate and 8 electrodes, changes of surface states and electron depletion layers are caused simply by different carbonization time, and therefore, the difference of detection performance among the sensors is caused, and the sensitivity of the gas sensor is enhanced. By adopting a data processing method of the radar fingerprint, the identification and detection of ammonia water, formaldehyde, ethanol and water vapor can be realized at room temperature (25 ℃).
Drawings
FIG. 1 is a scanning electron microscope image (a) to (d) of the present invention, respectively after the hydrochloric acid-doped polyaniline is not carbonized and carbonized for 1, 3, 5 hours;
FIG. 2 is a graph showing the response of the sensor array of the present invention to ammonia and air at room temperature, wherein the response curves from (a) to (d) correspond to the first sensor, the second sensor, the third sensor and the fourth sensor, respectively;
FIG. 3 is a graph showing the response of the sensor array of the present invention to formaldehyde and air at room temperature, wherein the response curves from (a) to (d) correspond to the first sensor, the second sensor, the third sensor and the fourth sensor, respectively;
FIG. 4 is a graph showing the response of the sensor array of the present invention to ethanol and air at room temperature, wherein the response curves from (a) to (d) correspond to the first sensor, the second sensor, the third sensor and the fourth sensor, respectively;
FIG. 5 is a graph showing the response of the sensor array of the present invention to saturated steam at room temperature, wherein the response curves from (a) to (d) correspond to the first sensor, the second sensor, the third sensor and the fourth sensor, respectively;
FIG. 6 shows the radar fingerprint spectrum of ammonia (a), formaldehyde (b), water vapor (c) and ethanol (d) in the present invention;
Detailed Description
The invention is described in detail below with reference to the following figures and examples:
The preparation method of the polyaniline carbonization method gas-sensitive material comprises four stages of preparation of the gas-sensitive material, preparation of a gas sensor array, detection of the gas sensor array on target atmosphere and identification and distinction of toxic gas.
a. Dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to a molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b for about 24 hours at the temperature of 25 ℃ to obtain polyaniline nano powder doped with hydrochloric acid;
a. dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to a molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b at the temperature of 25 ℃ for about 24 hours to obtain polyaniline nano powder doped with hydrochloric acid, taking out one part of the polyaniline nano powder, putting the other part of the polyaniline nano powder into a chemical vapor deposition furnace, and carbonizing the polyaniline nano powder for 1 hour under the protection of nitrogen gas, wherein the carbonization temperature is set to 600 ℃;
a. dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to a molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b at the temperature of 25 ℃ for about 24 hours to obtain polyaniline nano powder doped with hydrochloric acid, taking out one part of the polyaniline nano powder, putting the other part of the polyaniline nano powder into a chemical vapor deposition furnace, and carbonizing the polyaniline nano powder for 3 hours under the protection of nitrogen gas, wherein the carbonization temperature is set to 600 ℃;
a. dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to the molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b at the temperature of 25 ℃ for about 24 hours to obtain polyaniline nano powder doped with hydrochloric acid, taking out one part of the polyaniline nano powder, putting the other part of the polyaniline nano powder into a chemical vapor deposition furnace, and carbonizing the polyaniline nano powder for 5 hours under the protection of introduced nitrogen at the carbonization temperature of 600 ℃;
preparation of gas sensor array:
dispersing the hydrochloric acid doped polyaniline nanopowder obtained in step c of examples 1-4 in deionized water and grinding for 10 minutes respectively to obtain 4 parts of hydrochloric acid doped polyaniline nanopowder paste, uniformly coating the hydrochloric acid doped polyaniline nanopowder paste on the first sensor, the second sensor, the third sensor and the fourth sensor respectively, and drying at room temperature to form a gas sensor array.
Detection of target atmosphere by gas sensor array:
detection of target atmosphere by gas sensor array:
and (3) switching on a power supply of a Catherine electric meter, testing the resistance of the sensor array obtained in the step d in an ammonia water atmosphere and air at room temperature (the temperature is 25 ℃ and the relative humidity is 25%) under the bias voltage of 4V, and respectively carbonizing the sensor array from (a) to (d) for 0h, 1h, 3h and 5 h. As can be seen from the response curve, at room temperature, the response of the hydrochloric acid doped polyaniline resistance type sensor array to 1000ppm ammonia water atmosphere respectively reaches-69.7%, 34831.5%, 81918.9% and 60609.4%; response times were 1.4, 24.0, 25.9, and 22.9, respectively; recovery times were 7.2, 1.6, 0.9 and 1.8 respectively (see fig. 3).
And (3) switching on a power supply of a Catherine electric meter, testing the resistance of the sensor array obtained in the step d in the formaldehyde atmosphere and air at room temperature (the temperature is 25 ℃ and the relative humidity is 25%) under the bias voltage of 4V, and respectively carbonizing the sensor array from (a) to (d) for 0h, 1h, 3h and 5 h. As can be seen from the response curve, at room temperature, the response of the hydrochloric acid doped polyaniline resistance-type sensor array to 1000ppm formaldehyde atmosphere reaches-16%, 260.9%, 761.0% and 8191.9% respectively; response times were 11.0, 22.7, 24.8, and 14.8, respectively; the recovery times were 10.3, 2.1, 2.7 and 1.2 respectively (see fig. 4).
And (3) switching on a power supply of a Catherine electric meter, testing the resistance of the sensor array obtained in the step d in water vapor and air at room temperature (the temperature is 25 ℃ and the relative humidity is 25%) under the bias voltage of 4V, and respectively carbonizing the sensor array from (a) to (d) for 0h, 1h, 3h and 5 h. As can be seen from the response curve, the response of the hydrochloric acid doped polyaniline resistance-type sensor array to 1000ppm ethanol reaches-27.9%, 9887.5%, 6813.6% and 18876.4% respectively at room temperature; response times were 9.5, 20.5, 24.9 and 23.5, respectively; the recovery times were 10.3, 1.0, 1.4 and 1.7 respectively (see fig. 6).
And (3) switching on a power supply of a Catherine electric meter, testing the resistance of the sensor array obtained in the step d in an ethanol atmosphere and air at room temperature (the temperature is 25 ℃ and the relative humidity is 25%) under the bias voltage of 4V, and respectively carrying out carbonization on the sensor array from (a) to (d) for 0h, 1h, 3h and 5 h. As can be seen from the response curve, at room temperature, the response of the hydrochloric acid doped polyaniline resistance-type sensor array to the 1000ppm ethanol atmosphere reaches-42.6%, 949.0%, 7409.6% and 3132.2% respectively; response times were 9.5, 22.9, 16.5 and 17.7, respectively; recovery times were 8.8, 0.8, 1.1 and 1.0, respectively (see fig. 5).
Identification and differentiation of toxic atmospheres:
processing response sizes and response times of a first sensor, a second sensor, a third sensor and a fourth sensor in a sensor array to 4 atmospheres by using a radar fingerprint analysis method to obtain radar fingerprints of the 4 atmospheres, and distinguishing the 4 atmospheres according to the fingerprints, as shown in FIG. 6;
the present invention will be more readily understood from the specific examples given above. The above embodiments are merely illustrative and should not be construed as limiting the scope of the present invention.
Claims (3)
1. A method for preparing a gas sensor array based on improvement of sensor sensitivity by changing the P, N type of a sensor after carbonization of polyaniline doped with hydrochloric acid and by carbonizing at different time comprises the following specific operations:
preparation of the gas sensitive material:
a. dissolving ammonium persulfate and hydrochloric acid in 25mL of deionized water according to a molar ratio of 5: 16;
b. dissolving 5mL of aniline in 400mL of deionized water, slowly dropping the solution obtained in the step a into the solution, and stirring the solution for 19 hours at 25 ℃ in a dark condition; performing ultrasonic treatment on the obtained solution by using deionized water, and performing centrifugal separation for 6 times;
c. drying the precipitate obtained in the step b at the temperature of 25 ℃ for 24 hours to obtain polyaniline nano powder doped with hydrochloric acid;
d. dividing the hydrochloric acid doped polyaniline nano powder obtained in the step c into four parts respectively, taking out three parts, putting the three parts into a chemical vapor deposition furnace respectively, and carbonizing for 1 hour, 3 hours and 5 hours at 600 ℃ under the protection of introduced nitrogen;
preparing a resistance type gas sensor array:
e. and d, dispersing the hydrochloric acid doped polyaniline nano powder obtained in the step d in deionized water and grinding for 10 minutes to obtain 4 parts of hydrochloric acid doped polyaniline nano paste, uniformly coating the hydrochloric acid doped polyaniline nano paste on the first sensor, the second sensor, the third sensor and the fourth sensor respectively, and drying for 24 hours at room temperature to form the gas sensor array.
2. The method according to claim 1, wherein the temperature in step c is 24 ℃ and the reaction time is 24 hours.
3. The use of the nanostructured gas sensor array obtained by carbonizing a hydrochloric acid doped polyaniline according to the method of claim 1 for detecting an atmosphere containing ammonia, formaldehyde, ethanol and water vapor.
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