CN113624807B - Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor - Google Patents
Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor Download PDFInfo
- Publication number
- CN113624807B CN113624807B CN202110734274.3A CN202110734274A CN113624807B CN 113624807 B CN113624807 B CN 113624807B CN 202110734274 A CN202110734274 A CN 202110734274A CN 113624807 B CN113624807 B CN 113624807B
- Authority
- CN
- China
- Prior art keywords
- nanocellulose
- tin oxide
- gas sensor
- hydrothermal reaction
- temperature hydrothermal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 54
- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 38
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002086 nanomaterial Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 238000000643 oven drying Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000004044 response Effects 0.000 description 8
- 238000001514 detection method Methods 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 201000005202 lung cancer Diseases 0.000 description 1
- 208000020816 lung neoplasm Diseases 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Immunology (AREA)
- Biochemistry (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Electrochemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a method for preparing tin oxide and SO by utilizing nanocellulose to carry out low-temperature hydrothermal reaction 2 A method of a gas sensor belongs to the field of gas sensors. The SO 2 The gas sensor takes nano cellulose and tin tetrachloride pentahydrate as raw materials, and the tin oxide material is obtained through low-temperature hydrothermal synthesis. Then preparing the material into suspension, uniformly spraying the suspension on the interdigital electrode by a spraying method to form a layer of gas-sensitive film, thereby obtaining SO 2 A gas sensor. The preparation method is simple and environment-friendly, and the obtained sensor can detect SO with low concentration 2 。
Description
Technical Field
The invention relates to the field of gas sensors, in particular to a synthesis method for preparing tin oxide by utilizing nanocellulose to carry out low-temperature hydrothermal reaction and an application of the tin oxide in SO (SO) 2 Application in gas sensors. Detection of SO based on sensor resistance change under UV light from nanocellulose-prepared tin oxide 2 And (3) gas.
Background
SO 2 Is a typical polluted ambient gas. Since coal and petroleum generally contain elemental sulfur, SO is produced during combustion 2 。SO 2 Can be oxidized into SO 3 Reacts with rainwater to form acid rain, and has great health hazard to aquatic ecosystems and land ecosystems. In addition, it is a toxic gas, has a tolerance of about 5ppm in the human body, and has a long-term contact limit of 2ppm because it causes serious diseases such as respiratory and cardiovascular diseases and lung cancer in the human body. Thus to SO2 gasTime-continuous detection is important, especially in the detection of low SO concentrations 2 。
The metal oxide semiconductor is considered as the most promising gas-sensitive material, and plays a vital role in monitoring toxic and harmful gases due to the advantages of simple manufacture, low cost and the like. However, the semiconductor sensor has problems such as complicated operation equipment, high reaction temperature, long reaction time, high detection concentration, low response value, and the like. Therefore, a sensor that is simple to operate, requires low requirements for conditions of use, and has high sensitivity is required.
Disclosure of Invention
The present invention is directed to providing a method for preparing tin oxide and SO by low-temperature hydrothermal reaction of nanocellulose 2 Method for measuring gas sensor under ultraviolet light to effectively detect SO 2 And the gas can reduce the use temperature of the equipment and the operation complexity.
In order to solve the technical problems in the prior art, the scheme of the invention is as follows:
a method for preparing tin oxide by utilizing nanocellulose to carry out low-temperature hydrothermal reaction comprises the following preparation processes:
adding a certain mass of nano cellulose solution into the solution, wherein the solution is tin tetrachloride pentahydrate and is dissolved in deionized water; and uniformly stirring the mixed solution, performing low-temperature hydrothermal reaction, and performing centrifugation, washing, drying and calcination treatment after the reaction is finished to obtain the tin oxide material.
The invention also discloses a method for preparing the tin oxide by utilizing the nanocellulose to carry out low-temperature hydrothermal reaction and application of the tin oxide to SO 2 A gas sensor comprising the steps of:
step 1: the preparation method of the tin oxide gas-sensitive material comprises the following steps:
209.32mg of tin tetrachloride pentahydrate is added into the nanocellulose solution with different quality, deionized water is added to ensure that the solution is 10ml, the solution is stirred uniformly, the hydrothermal reaction is carried out at low temperature, and after the reaction is finished, the tin oxide precursor (Sn (OH) is obtained through centrifugation, washing, drying and the like 4 ) Finally, high-temperature calcination is carried out at 600 ℃/2h to obtain the tin oxide nano material.
Step 2: preparation of SO 2 The gas sensor is characterized in that the tin oxide material obtained in the step 1 is added with a proper amount of water for ultrasonic dispersion to obtain a uniformly dispersed tin oxide suspension, the suspension is transferred into a container of a spray pen through a liquid-transferring gun, and is uniformly sprayed on an interdigital electrode by a spraying method, and SO is prepared after drying 2 A gas sensor.
On the basis of the scheme, the nanocellulose is preferably CNF ((the raw material is filter paper, the cellulose is prepared by a chemical mechanical method, and the cellulose is macromolecular polysaccharide consisting of D-glucose and beta-1, 4 glycosidic bonds).
On the basis of the scheme, preferably, the tin tetrachloride pentahydrate in the step 1 is 209.32mg; the nanocellulose solution was 30mg (3 ml).
The tin tetrachloride pentahydrate is 209.32mg; the nanocellulose solution was 40mg (4 ml).
The tin tetrachloride pentahydrate is 209.32mg; the nanocellulose solution was 50mg (5 ml).
The tin tetrachloride pentahydrate is 209.32mg; the nanocellulose solution was 60mg (6 ml).
Based on the scheme, preferably, the magnetic stirring time is 60min.
Based on the scheme, the low-temperature hydrothermal condition is preferably that the reaction is carried out in a polytetrafluoroethylene reaction kettle at 60 ℃ for 2 hours.
On the basis of the above protocol, it is preferable that the centrifugation conditions are centrifugation at 8000rpm for 10 minutes.
On the basis of the scheme, preferably, the washing and drying conditions are deionized water and absolute ethyl alcohol which are alternately washed and centrifuged for 3 times, and finally the obtained precipitate is dried at 60 ℃ for 24 hours.
On the basis of the above scheme, the condition of the high-temperature calcination is preferably that the temperature is raised to 600 ℃ at 4 ℃/min and maintained for 2 hours.
Based on the scheme, preferably, the concentration of the tin oxide in the suspension in the step 2 is 10mg/ml, and the ultrasonic treatment is carried out for 30-50 min.
Based on the above scheme, the air pressure of the spray pen is preferably 0.01MPa to 0.03MPa.
On the basis of the above scheme, preferably, the inter-finger electrode finger distance in the step 2 is 50 μm.
On the basis of the scheme, the sensor in the step 2 is preferably dried at 60 ℃ for 5 hours.
Compared with the prior art, the technical scheme of the invention is as follows:
(1) According to the invention, the nano-cellulose is used for preparing the tin oxide, the hydrothermal reaction temperature is 60 ℃, the time is short and only 2 hours are needed, and the method is environment-friendly. In the scheme of preparing the tin oxide by traditional hydrothermal method, sodium citrate is generally required to be reduced or sodium hydroxide is required to form a precipitate, meanwhile, other medicines are required to be added, various medicines are required, the reaction temperature is 160-200 ℃, the addition is not required, and the prepared tin oxide has good effect.
(2) The invention prepares tin oxide by nano cellulose and is used as SO 2 The gas sensor is capable of detecting low concentration of SO 2 . The nano-size effect of the nano-cellulose can prepare the tin oxide nano-material. In addition, the tin oxide nano material prepared from the nano cellulose has higher surface activity and stronger adsorptivity, and is beneficial to monitoring the SO with low concentration 2 。
Drawings
FIG. 1 shows the low temperature hydrothermal reaction of nanocellulose to prepare tin oxide and application to SO 2 Method of gas sensor TG/DTG analysis of tin oxide prepared in the examples was performed.
FIG. 2 shows the low temperature hydrothermal reaction of nanocellulose to prepare tin oxide and application to SO in the present invention 2 Methods of gas sensors XRD analysis of the tin oxide prepared in the examples was performed.
FIG. 3 shows the low temperature hydrothermal reaction of nanocellulose to prepare tin oxide and application to SO in the present invention 2 Electron microscopy scans of tin oxide prepared in the method embodiments of the gas sensor.
FIG. 4 is a low temperature hydrothermal reaction using nanocellulose in accordance with the present inventionPreparation of tin oxide and application to SO 2 Method of gas sensor embodiment examples tin oxide materials prepared from nanocellulose of different masses are used for different SO concentrations (250, 500, 750, 1000, 1250 ppb) 2 Gas response recovery test chart.
FIG. 5 shows the low temperature hydrothermal reaction of nanocellulose to prepare tin oxide and application to SO in the present invention 2 Method of gas sensor the gas sensitive properties of the tin oxide material prepared in the examples of implementation.
Wherein (a) SnO 2 50mg CNF sensor in SO 2 Repeatability test chart for gas concentration of 1000ppb, (b) SnO 2 50mg CNF sensor in SO 2 Stability test chart (c) SnO at gas concentration of 1000ppb 2 50mg CNF sensor in SO 2 Response plot with increasing concentration (rh=9.4% -73.9%) for gas concentrations of 1000 ppb.
Detailed Description
The invention will be better understood from the examples set forth below, with reference to the drawings and examples of implementation.
Examples
Synthesis method for preparing tin oxide by taking stannic chloride pentahydrate as tin source and utilizing nanocellulose to carry out low-temperature hydrothermal reaction and SO 2 The application in the gas sensor is as follows:
step 1: preparing a tin oxide nano material; the preparation process is as follows:
adding a proper amount of nanocellulose solution dropwise into 209.32mg of tin tetrachloride pentahydrate, adding deionized water dropwise to ensure that the total volume of the four components is 10ml, magnetically stirring for 30min, placing the solution into a polytetrafluoroethylene reaction kettle, carrying out low-temperature hydrothermal treatment at 60 ℃ for 2h, centrifugally drying the obtained precipitate to obtain a tin oxide precursor, and finally calcining at high temperature (600 ℃/2 h) to obtain tin oxide nanomaterial powder.
Step 2: preparation of SO 2 A gas sensor; the preparation process is as follows:
mixing 10mg of the tin oxide material obtained in the step 1 into 1ml of deionized water, performing ultrasonic dispersion for 30min to obtain uniformly dispersed tin oxide suspension, and mixing the suspensionTransferring the turbid liquid into a container of a spray pen through a liquid transferring gun, uniformly spraying on a clean interdigital electrode by using a spraying method, and drying to prepare SO 2 A gas sensor. The SO obtained 2 The gas sensor performs a gas-sensitive performance test under ultraviolet light.
In this example, as shown in fig. 1, TG/DTG of the tin oxide nanomaterial has a slight mass loss at 41.97 ℃, which is caused by the removal of adsorbed water from the precursor, and a large mass loss occurs in the range of 41.97-381.25 ℃, and at this time CNF and crystal water are removed from the sample. In the whole process, the weight loss state is kept all the time, and the weight loss state tends to be stable until the temperature reaches about 600 ℃.
In this example, the XRD pattern of the tin oxide nanomaterial is shown in fig. 2, and it can be seen that the diffraction peaks of the four components can correspond to PDF, which means that the prepared product is tin oxide.
In this example, the XRD patterns of the tin oxide nanomaterial are shown in FIG. 3, and it can be seen that the size of the tin oxide is less than 100nm.
In this embodiment, SO 2 The response recovery test of the gas sensor for different concentrations (250, 500, 750, 1000, 1250 ppb) of the body is shown in fig. 4, and it can be seen that the response of the four components increases with the increase of the gas concentration, and the response value of the tin oxide prepared by 50mg of CNF is highest, followed by 60mg of tin oxide prepared by 40mg of CNF, and finally by 30mg of tin oxide prepared by CNF.
In the present embodiment, snO 2 50mg CNF sensor in SO 2 The repeatability at a gas concentration of 1000ppb is shown in fig. 5 a, and it can be seen that the sensor has better repeatability.
In the present embodiment, snO 2 50mg CNF sensor in SO 2 Stability at a gas concentration of 1000ppb as shown in fig. 5 b, it can be seen that there is better stability of the sensor without a significant change in response value over a month.
In the present embodiment, snO 2 50mg CNF sensor in SO 2 The response of a gas concentration of 1000ppb at different humidities is shown in FIG. 5 c, which canTo see that the sensor responds slightly to an increase in humidity but has little effect on the detection of gas sensitivity.
The foregoing has outlined and described the main features and advantages of the present invention.
The above embodiments are illustrative and not restrictive, and several embodiments may be listed in the defined scope, and therefore variations and modifications without departing from the general inventive concept should be considered as falling within the scope of the present invention.
Claims (7)
1. SO is prepared by utilizing nanocellulose to carry out low-temperature hydrothermal reaction 2 A method of a gas sensor comprising the steps of:
step 1: the preparation process of the tin oxide material is as follows:
adding a certain mass of nano cellulose solution into the solution, wherein the solution is tin tetrachloride pentahydrate and is dissolved in deionized water; uniformly stirring the mixed solution, performing low-temperature hydrothermal reaction, and performing centrifugation, washing, drying and calcination treatment after the reaction is finished to obtain a tin oxide material;
step 2: preparation of SO 2 The preparation process of the gas sensor is as follows:
adding deionized water into the tin oxide material obtained in the step 1, performing ultrasonic treatment to obtain a uniformly dispersed suspension, transferring the suspension into a spray pen container through a liquid transferring gun, uniformly spraying the suspension on the surfaces of interdigital electrodes, and drying to obtain SO 2 A gas sensor;
in the step 1, the added nanocellulose solution is CNF;
in the step 1, the low-temperature hydrothermal reaction condition is 60 ℃/2h; centrifuging at 8000rpm for 10min; oven-drying at 60deg.C for 24 hr.
2. SO prepared by low temperature hydrothermal reaction using nanocellulose as claimed in claim 1 2 The method of the gas sensor is characterized in that the mixture ratio of the mixed solution in the step 1 is any one of the following:
tin tetrachloride pentahydrate is 209.32mg and 30mg of nanocellulose solution;
alternatively, the tin tetrachloride pentahydrate is 209.32mg and 40mg of nanocellulose solution;
alternatively, the tin tetrachloride pentahydrate is 209.32mg and 50mg of nanocellulose solution;
alternatively, the tin tetrachloride pentahydrate is a solution of 209.32mg and 60mg nanocellulose.
3. The preparation of SO by low temperature hydrothermal reaction of nanocellulose as claimed in claim 1 2 A method for preparing a gas sensor is characterized in that in the step 1, the mixed solution is subjected to low-temperature hydrothermal reaction, and after the reaction is finished, a tin oxide precursor (Sn (OH) is obtained through centrifugation, washing and drying treatment 4 ) Finally, calcining for 2 hours at the high temperature of 600 ℃ to obtain the tin oxide nano material.
4. The preparation of SO by low temperature hydrothermal reaction of nanocellulose as claimed in claim 1 2 The method of the gas sensor is characterized in that in the step 2, the mass of tin oxide in the suspension is 10mg/ml.
5. The preparation of SO by low temperature hydrothermal reaction of nanocellulose as claimed in claim 1 2 The method of the gas sensor is characterized in that in the step 2, the interdigital electrode is firstly cleaned, and the cleaning step is as follows:
(1) Ultrasonic treating with acetone for 3-5 min;
(2) Ultrasonically cleaning the substrate for 3 to 5 minutes by using absolute ethyl alcohol;
(3) Ultrasonically cleaning with deionized water for 3-5 minutes;
(4) And drying the surface of the interdigital electrode by nitrogen.
6. The preparation of SO by low temperature hydrothermal reaction of nanocellulose as claimed in claim 1 2 A method of gas sensor, characterized in that in step 2 the inter-finger width of the interdigitated electrodes is 50 μm.
7. The method according to claim 1, wherein the nanocellulose is usedSO is prepared by low-temperature hydrothermal reaction 2 The method of the gas sensor is characterized in that in the step 2, when a spraying method is used, the air pressure of a spraying pen is 0.01MPa to 0.03MPa; the sprayed sensor was dried at 60 ℃ for 5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110734274.3A CN113624807B (en) | 2021-06-30 | 2021-06-30 | Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110734274.3A CN113624807B (en) | 2021-06-30 | 2021-06-30 | Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113624807A CN113624807A (en) | 2021-11-09 |
| CN113624807B true CN113624807B (en) | 2024-03-29 |
Family
ID=78378611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110734274.3A Active CN113624807B (en) | 2021-06-30 | 2021-06-30 | Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113624807B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107337802A (en) * | 2017-05-18 | 2017-11-10 | 武汉纺织大学 | Air-sensitive film sensitive to ethanol and acetone and preparation method thereof |
| WO2018103145A1 (en) * | 2016-12-08 | 2018-06-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Micro-porous hollow nickel oxide gas-sensitive material for selectively adsorbing formaldehyde as well as preparation and application thereof |
| KR20180090762A (en) * | 2017-02-03 | 2018-08-13 | 세종대학교산학협력단 | Nano cellulose-based composite having metal oxide layer and preparation method of thereof |
-
2021
- 2021-06-30 CN CN202110734274.3A patent/CN113624807B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103145A1 (en) * | 2016-12-08 | 2018-06-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Micro-porous hollow nickel oxide gas-sensitive material for selectively adsorbing formaldehyde as well as preparation and application thereof |
| KR20180090762A (en) * | 2017-02-03 | 2018-08-13 | 세종대학교산학협력단 | Nano cellulose-based composite having metal oxide layer and preparation method of thereof |
| CN107337802A (en) * | 2017-05-18 | 2017-11-10 | 武汉纺织大学 | Air-sensitive film sensitive to ethanol and acetone and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 二氧化锡基气敏材料研究进展;刘增伟;材料导报;23-29 * |
| 纳米微晶纤维素诱导制备方形纳米二氧化钛及其光催化性能;周艳;丁恩勇;;现代化工(第04期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113624807A (en) | 2021-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109799267B (en) | Planar humidity and ammonia gas sensor based on alkalized organ-shaped MXene sensitive material and preparation method thereof | |
| CN106732818B (en) | Double layer hollow material based on titanium dioxide and preparation method thereof and the application in hydrogen sulfide photocatalysis treatment | |
| Sun et al. | Formaldehyde gas sensors based on SnO2/ZSM-5 zeolite composite nanofibers | |
| CN108680610B (en) | Based on MoS2Room temperature NO of PbS composite2Gas sensor and preparation method thereof | |
| CN105928983B (en) | A kind of acetylene gas sensor and preparation method thereof | |
| CN108918633B (en) | Preparation of Pd-SnO2 nano composite material and application thereof in hydrogen sensor | |
| CN110412087A (en) | One kind being based on NiCoxFe2-xO4Isopropanol gas sensor of nanocube material and preparation method thereof | |
| CN110606503A (en) | Gold-modified porous tin dioxide micro-nanosheet composite material and preparation method and application thereof | |
| CN110068599A (en) | One kind being based on CoFe2O4/Co3O4The formaldehyde gas sensor and preparation method thereof of duplex shell structure cubic materials | |
| CN109342534A (en) | Lacking oxygen it is leading based on CuO/ZnFe2O4Dimethylbenzene gas sensor of core-shell structure microballoon and preparation method thereof | |
| CN105021672B (en) | PhotoelectrochemicalMethod Method detection dopamine based on in-situ oxidation reduction reaction | |
| Salagare et al. | Facile synthesis of silver nanoparticle-decorated zinc oxide nanocomposite-based pencil graphite electrode for selective electrochemical determination of nitrite | |
| Mylarappa et al. | Development of Coriander Honey loaded CeO2 for cyclic voltammetry, chemical sensor, dye purification, and antioxidant properties | |
| Li et al. | Xanthate sensing properties of Pt-functionalized WO3 microspheres synthesized by one-pot hydrothermal method | |
| CN113624807B (en) | Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor | |
| CN114348999A (en) | Pd-modified SnO2/rGO nano composite material, preparation method thereof, sensor and preparation method thereof | |
| CN109133183B (en) | α-Fe2O3Production of nano microsphere hydrogen sulfide gas-sensitive material and element | |
| CN108439460B (en) | SnO (stannic oxide)2-SnS2Chemical preparation method of core-shell structure nano particles | |
| CN114604903B (en) | Cobalt sulfide/reduced graphene oxide compound and application thereof in gas sensor | |
| CN107573513B (en) | Silver-copper dissimilar metal cluster compound and preparation method and application thereof | |
| CN115196694B (en) | NiS/rGO composite material, preparation method thereof and application thereof in gas sensitive material | |
| CN110026227B (en) | Chromium-doped titanium dioxide nanotube-amino modified graphene oxide composite material and preparation method and application thereof | |
| CN116500095B (en) | VOCs exhalation sensor array with high gas sensitivity and preparation method and application thereof | |
| Chen et al. | An electrochemical sensor for selective detection of Cu2+ by using a self-assembled Cu coordinated β-cyclodextrin-nitrogen-doped carbon quantum dots composite | |
| CN111474211A (en) | Biomass charcoal-double crystal phase metal oxide (WO)3) Composite material, preparation and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |