CN112408463A - High-response-sensitivity SnO2Gas sensitive material, preparation process and application - Google Patents
High-response-sensitivity SnO2Gas sensitive material, preparation process and application Download PDFInfo
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Abstract
The invention discloses SnO with high response sensitivity in the technical field of nano materials2Gas sensitive material and preparation process and application, S1: preparation of carbon sphere template, S2: precursor liquid preparation for high voltage electrospinning, S3: preparing a high-response-sensitivity SnO2 gas-sensitive material; the high-response-sensitivity SnO synthesized by the technology2The gas sensitive material shows excellent response characteristics to low-concentration ethanol by preparing a sensor and performing static gas sensitive test: (1) the detection concentration is as low as 5 ppm; (2) the working temperature is 200 ℃; (3) the response value of 100ppm ethanol is up to 35.6, the response time and the recovery time are respectively 12s and 8s, and the problem of the reaction with methanol (CH) is solved3OH, Formaldehyde (HCHO), acetone (CH)3COCH3) Acetic acid (CH)3COOH) and ammonia (NH)3) And the cross-response problem of VOCs.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to high-response-sensitivity SnO2Gas sensitive material, preparation process and application.
Background
The research of nano semiconductor sensors is concerned by researchers at home and abroad in recent years. Innovative research on various gas sensors is focused on industrial emission control, household safety (indoor air quality monitoring), environmental monitoring, health care (disease diagnosis and microanalysis of components of exhaled gas of human bodies) and the like. A plurality of existing research reports of gas sensitive materials aim at ethanol (CH)3CH2OH), acetone (CH)3COCH3) And detecting Volatile Organic Compounds (VOCs). VOCs widely exist in various aspects such as dyes, medicines, building decoration materials and the like, have irritation and toxicity to human bodies, cause immune disorder to influence the functions of the central nervous system, and damage the liver and the hematopoietic system to cause lung diseases and even lung cancer. For example, ethanol is the most important breath analyte target monitored in the traffic field for determining drunk driving, besides being the most common flammable and explosive hazardous reagent in the industrial field and the laboratory. The ethanol sensitive monitoring has important practical significance.
At present, conventional tin dioxide (SnO)2) Low cost of semiconductor nano material preparation, SnO2The sensor has good response sensitivity characteristic to various VOCs, but has the outstanding defects of high working temperature (two hundred to three hundred degrees centigrade), high power consumption, and particularly strong cross selectivity to various VOCs, and the bottleneck problem seriously limits SnO2The marketable application of sensors for detection of VOCs.
Thus, a high response sensitivity SnO is provided2The gas sensitive material and the preparation process solve the problems.
Disclosure of Invention
The invention aims to provide SnO with high response sensitivity2Gas sensitive material, preparation process and application thereof, aiming at solving the problemsProblems are raised in the background art.
To achieve the above object, the present invention provides a high response sensitivity SnO2The preparation method of the gas sensitive material specifically comprises the following steps:
s1: preparing a carbon sphere template: at 35 ℃, 3.2g of glucose and 35ml of deionized water are put into a reactor to be fully dissolved, NaOH solution is added into the reactor, the PH value is adjusted to 10, mixed liquor is obtained, the mixed liquor is transferred into a 50ml of polytetrafluoroethylene-lined autoclave to react for 10 hours at 180 ℃, and then washing, collecting and drying precipitate are carried out, so as to obtain a carbon sphere template; (ii) a
S2: preparing a precursor liquid for high-voltage electrostatic spinning: dissolving 0.32g PVP in 2ml ethanol to obtain solution A, and collecting 0.73g SnCl2·2H2O and 0.036g Pr (NO)3)3·6H2Completely dissolving O in 2.6ml of DMF to obtain a solution B, putting the solution A and the solution B into a magnetic stirrer to stir for 3 hours, and then adding 0.08g of carbon balls prepared in the step S1 into the magnetic stirrer to slowly stir for 1 hour to obtain a precursor liquid of high-voltage electrostatic spinning;
s3: high response sensitivity SnO2Preparing a gas sensitive material: transferring the precursor liquid of the high-voltage electrostatic spinning in the step S2 into a glass injector, performing high-voltage electrostatic spinning, collecting to obtain a spinning primary product, and placing the spinning primary product into a tube furnace for high-temperature calcination to obtain SnO with high response sensitivity2A gas sensitive material.
Preferably, in step S1, the NaOH solution is 5% by mass.
Preferably, in the step S1, the precipitate is dried in an oven at 80 ℃ for 12 hours.
Preferably, in step S2, the temperature in the magnetic stirrer is controlled to be 30 ℃.
Preferably, in the step S3, the temperature of the tube furnace is 600 ℃, and the calcination time is 4 h.
The invention also provides high response sensitivity SnO2Production of SnO by gas-sensitive material2Application in a base sensor.
The invention has the beneficial effects that:
the invention aims to greatly improve SnO by regulating and controlling the microstructure and the electron transmission performance of the nano material2The sensitivity of the sensor to ethanol detection is based on, the problem of cross selectivity of VOCs detection is mainly solved, and meanwhile, the working temperature of the sensor is reduced to a certain extent. In particular, praseodymium ions (Pr) with catalytic activity are combined by introducing functionalized sacrificial carbon sphere (C) templates3+，Pr4+) By optimizing the technological parameters of high-voltage electrostatic spinning, the unique beaded SnO with rich micropores and large specific surface is obtained2Based hollow fiber structures, SnO produced by the inventive technique having unique microstructural characteristics2The base hollow fiber semiconductor material has significant performance advantages in high-sensitivity detection of low-concentration ethanol;
the high-response-sensitivity SnO synthesized by the technology2The gas sensitive material shows excellent response characteristics to low-concentration ethanol by preparing a sensor and performing static gas sensitive test: (1) the detection concentration is as low as 5 ppm; (2) the working temperature is 200 ℃; (3) the response value of 100ppm ethanol is up to 35.6, the response time and the recovery time are respectively 12s and 8s, and the problem of the reaction with methanol (CH) is solved3OH, Formaldehyde (HCHO), acetone (CH)3COCH3) Acetic acid (CH)3COOH) and ammonia (NH)3) And the cross-response problem of VOCs.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a high-responsivity SnO in example 1 of the present invention2XRD and EDX spectrograms of the gas-sensitive material;
FIG. 2 is a high-responsivity SnO in example 1 of the present invention2SEM topography of the gas sensitive material;
FIG. 3 is a high-responsivity SnO in example 1 of the present invention2TEM shape of gas sensitive materialAppearance graph and element Mapping;
FIG. 4 is a high responsivity SnO in example 1 of the present invention2A base sensor digital photo;
FIG. 5 is SnO of the present invention2A gas sensitive test result graph of the base sensor;
FIG. 6 is SnO of the present invention2Response and recovery time profiles for the base sensors.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
High-response-sensitivity SnO2The gas sensitive material and the preparation process thereof comprise the following steps:
s1: preparing a carbon sphere template: at 35 ℃, 3.2g of glucose and 35ml of deionized water are placed into a reactor for full dissolution, a 5% NaOH solution by mass is added into the reactor, the PH is adjusted to 10 to obtain a mixed solution, the mixed solution is transferred into a 50ml polytetrafluoroethylene-lined autoclave for reaction for 10 hours at 180 ℃, and then washing, collecting and depositing are carried out, and the mixture is placed into a drying oven for drying for 12 hours at 80 ℃ to obtain a carbon sphere template;
s2: preparing a precursor liquid for high-voltage electrostatic spinning: dissolving 0.32g PVP in 2ml ethanol to obtain solution A, and collecting 0.73g SnCl2·2H2O and 0.036g Pr (NO)3)3·6H2Completely dissolving O in 2.6ml of DMF to obtain a solution B, putting the solution A and the solution B into a magnetic stirrer, stirring for 3 hours, keeping the temperature in the magnetic stirrer at 30 ℃, and then adding 0.08g of carbon balls prepared in the step S1 into the magnetic stirrer, and slowly stirring for 1 hour to obtain a precursor liquid of high-voltage electrostatic spinning;
s3: high response sensitivity SnO2Preparing a gas sensitive material: the high pressure in step S2 is settledTransferring the precursor liquid of the electrospinning into a glass injector, performing high-voltage electrostatic spinning, collecting to obtain a spinning primary product, and calcining the spinning primary product in a tubular furnace at 600 ℃ for 4h to obtain SnO with high response sensitivity2A gas sensitive material.
The above-mentioned high response sensitivity SnO2Production of SnO by gas-sensitive material2Applications in base sensors: the high response sensitivity SnO2Grinding the gas-sensitive material, mixing the ground gas-sensitive material with deionized water to form slurry, coating the slurry on a ceramic substrate of the sensor to obtain the SnO with high response sensitivity2A base sensor.
All chemicals and reagents used in this example were of analytical grade and were not subjected to any further purification treatment.
Example 2
Nano-scale pure SnO was prepared under the same conditions as in example 12Sample (carbon-containing sphere template) and SnO obtained by the method in example 12Base sensors (carbon containing sphere templates).
Example 3
Nano-scale pure SnO was prepared under the same conditions as in example 12Sample (carbon-free sphere template) and SnO obtained by the method in example 12Base sensors (carbon-free sphere template).
FIG. 1 of the present invention gives: high response sensitivity SnO2The main component of the gas-sensitive material is Pr-doped SnO2。
FIG. 2 of the present invention can be seen: high response sensitivity SnO2The gas sensitive material is in a bead-shaped hollow fiber structure with a rough surface.
FIG. 3 of the present invention can be seen: high response sensitivity SnO2The fiber element composition and the microstructure detail characteristics of the gas sensitive material are well documented.
In fig. 5 of the present invention:
(a) high response sensitivity SnO2Base sensor, SnO2Base sensor (carbon-containing sphere template) and SnO2Response of the base sensor (carbon-free sphere template) to 100ppm ethanol at different operating temperatures;
(b) high response sensitivity SnO2Base sensor, SnO2Base sensor (carbon-containing sphere template) and SnO2Response of the base sensor (carbon-free sphere template) to various test gases at optimum operating temperature;
(c) high response sensitivity SnO2Base sensor, SnO2Base sensor (carbon-containing sphere template) and SnO2Single cycle response recovery characteristic curve for a base sensor (carbon-free sphere template) to 100ppm ethanol;
(d) high response sensitivity SnO2Response curves of the base sensor to 5-1000ppm ethanol;
(e) high response sensitivity SnO2Base sensor, SnO2Base sensor (carbon-containing sphere template) and SnO2Response of the base sensor (no carbon sphere template) to different concentrations of ethanol (5-1500 ppm);
(f) high response sensitivity SnO2Base sensor, SnO2Base sensor (carbon-containing sphere template) and SnO2Long-term stability of the base sensor (without carbon sphere template) to 100ppm ethanol.
In fig. 6 of the present invention:
(a)SnO2response and recovery time curves for the base sensor (carbonless sphere template);
(b)SnO2response and recovery time profiles for the base sensor (carbon sphere containing template);
(c) high response sensitivity SnO2The response and recovery time profiles of the base sensors.
In summary, it is evident from the gas-sensitive test result of fig. 5 that SnO with high response sensitivity2The working temperature of the base sensor is 200 ℃, the detection concentration is as low as 5ppm, the response value to 100ppm ethanol is as high as 35.6, and the base sensor obviously protrudes from the sensor to methanol (CH)3OH, Formaldehyde (HCHO), acetone (CH)3COCH3) Acetic acid (CH)3COOH) and ammonia (NH)3) The sensor still keeps good gas-sensitive response value characteristic after being placed in the air for two months, and shows good practical market application potential;
from fig. 6, it can be derived that: high response sensitivity SnO2Base sensors compared to SnO2Base sensor (carbon-containing sphere template), SnO2The performance of the base sensor (carbon-free sphere template) is more excellent, and the SnO with high response sensitivity2The response and recovery time of the base sensor are both greatly reduced, down to 12s and 8s, respectively.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not exhaustive and do not limit the method of making a high strength caliper seal to the specific embodiments described. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. High-response-sensitivity SnO2The gas sensitive material and the preparation process are characterized by comprising the following steps:
s1: preparing a carbon sphere template: at 35 ℃, 3.2g of glucose and 35ml of deionized water are put into a reactor to be fully dissolved, NaOH solution is added into the reactor, the PH value is adjusted to 10, mixed liquor is obtained, the mixed liquor is transferred into a 50ml of polytetrafluoroethylene-lined autoclave to react for 10 hours at 180 ℃, and then washing, collecting and drying precipitate are carried out, so as to obtain a carbon sphere template;
s2: preparing a precursor liquid for high-voltage electrostatic spinning: take 0.3Dissolving 2g PVP in 2ml ethanol to obtain solution A, and collecting 0.73g SnCl2·2H2O and 0.036g Pr (NO)3)3·6H2Completely dissolving O in 2.6ml of DMF to obtain a solution B, putting the solution A and the solution B into a magnetic stirrer to stir for 3 hours, and then adding 0.08g of carbon balls prepared in the step S1 into the magnetic stirrer to slowly stir for 1 hour to obtain a precursor liquid of high-voltage electrostatic spinning;
s3: high response sensitivity SnO2Preparing a gas sensitive material: transferring the precursor liquid of the high-voltage electrostatic spinning in the step S2 into a glass injector, performing high-voltage electrostatic spinning, collecting to obtain a spinning primary product, and placing the spinning primary product into a tube furnace for high-temperature calcination to obtain SnO with high response sensitivity2A gas sensitive material.
2. A high response sensitivity SnO according to claim 12The gas sensitive material and the preparation process are characterized in that in the step S1, the mass fraction of the NaOH solution is 5%.
3. A high response sensitivity SnO according to claim 12The gas sensitive material and the preparation process are characterized in that in the step S1, the precipitate is dried in an oven at 80 ℃ for 12 hours.
4. A high response sensitivity SnO according to claim 12The gas sensitive material and the preparation process are characterized in that in the step S2, the temperature in the magnetic stirrer is controlled to be 30 ℃.
5. A high response sensitivity SnO according to claim 12The gas sensitive material and the preparation process are characterized in that in the step S3, the temperature of the tube furnace is 600 ℃, and the calcination time is 4 h.
6. A high response sensitivity SnO according to any of claims 1-52Production of SnO by gas-sensitive material2Application in a base sensor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113135589A (en) * | 2021-04-26 | 2021-07-20 | 浙江大学 | Vermicular tin oxide gas-sensitive material, preparation method thereof and application of vermicular tin oxide gas-sensitive material in ethanol detection |
| CN113281383A (en) * | 2021-05-24 | 2021-08-20 | 安徽大学绿色产业创新研究院 | Ethanol gas sensor made of heterojunction composite material and preparation method thereof |
| CN115262034A (en) * | 2022-07-19 | 2022-11-01 | 安徽大学 | Chain bead type tin oxide based heterogeneous nanofiber gas sensitive material and preparation and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113281383B (en) * | 2021-05-24 | 2024-04-12 | 安徽大学绿色产业创新研究院 | Ethanol gas sensor of heterojunction composite material and preparation method thereof |
| CN115262034A (en) * | 2022-07-19 | 2022-11-01 | 安徽大学 | Chain bead type tin oxide based heterogeneous nanofiber gas sensitive material and preparation and application thereof |
| CN115262034B (en) * | 2022-07-19 | 2024-04-19 | 安徽大学 | Chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, and preparation and application thereof |
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