CN113135587A - Method for preparing flower-shaped nano SnO by hydrothermal synthesis2Method for producing gas-sensitive material - Google Patents

Method for preparing flower-shaped nano SnO by hydrothermal synthesis2Method for producing gas-sensitive material Download PDF

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CN113135587A
CN113135587A CN202010046709.0A CN202010046709A CN113135587A CN 113135587 A CN113135587 A CN 113135587A CN 202010046709 A CN202010046709 A CN 202010046709A CN 113135587 A CN113135587 A CN 113135587A
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sensing
gas
flower
sno
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王琼
亓成
庞宗宇
燕朝阳
卢若云
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Civil Aviation University of China
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

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Abstract

The invention discloses a method for preparing flower-shaped nano SnO by adopting a hydrothermal synthesis method2The method for preparing gas-sensitive material adopts hydrothermal synthesis method, uses trisodium citrate as additive and uses tin dichloride as tin salt to synthesize flower-like SnO with high dispersivity and uniform size by one-step process2The nanometer material solves the problems of high cost, complex synthesis steps, complex post-treatment process and the like in the prior synthesis technology, can be widely applied to the field of gas sensing, adopts cheap trisodium citrate as an inducer, and synthesizes the SnO with a flower-shaped structure with uniform size and good dispersibility in one step2The nano material can be widely applied to dangerous chemical gas detection in various environments.

Description

Method for preparing flower-shaped nano SnO by hydrothermal synthesis2Method for producing gas-sensitive material
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing flower-shaped nano SnO by adopting a hydrothermal synthesis method2A method of gas sensing materials.
Background
Along with the rapid speed of national economyThe development and the increasing environmental pollution problems and the increasing discharge of toxic and polluting gases have gradually affected the normal life of people, which makes it necessary to effectively detect and control these gases. At present, the main semiconductor metal oxide gas-sensitive materials used for gas sensors are: fe2O3、ZnO、WO3、In2O3And SnO2Etc. as a wide band n-type semiconductor (E)g＝3.6ev,300K)，SnO2The method has the advantages of good stability, high sensitivity, low cost and the like, and is most widely applied and researched in semiconductor metal oxide gas sensors.
SnO2The gas-sensitive performance of the gas-sensitive material depends on the size, uniformity, stability and surface structure of tin dioxide nanoparticles, so people have turned their attention to the preparation of micro-nano tin dioxide gas-sensitive materials with special structures (zero-dimensional, one-dimensional, two-dimensional and three-dimensional) and morphologies, which further improves the sensitivity and gas selectivity and shortens the response recovery time. Flower-like SnO2The surface area and the internal crystal defects of the nano-particles are increased rapidly, and the multi-layer structure can ensure that the gas molecules to be detected and SnO are mixed2Full contact is realized, which is beneficial to more tested gases to enter and adsorb SnO2The surface of the gas sensitive material, thereby improving the sensitivity and the response recovery time of the gas sensitive material. Thus, flower-like SnO2SnO of gas sensitive materials with respect to other dimensions2The gas-sensitive material has greatly improved gas-sensitive performance. At present, people prepare a series of micro-nano structure SnO with different structural morphologies through a chemical vapor deposition method, a sol-gel method, a hydrothermal precipitation method and a template method2The gas sensitive material has the defects of complicated steps, complex post-treatment process, high cost and the like. SnO prepared by hydrothermal synthesis method2The nanometer material is formed by one-time grain formation in the solvent, and does not need the later crystallization heat treatment, thereby effectively avoiding the defects of powder hard agglomeration, impurity mixing and the like caused by the later heat treatment. Therefore, how to synthesize SnO with three-dimensional flower-like structure by simple one-step cheap hydrothermal synthesis method2The nano gas-sensitive material is one of the challenges of a plurality of researchersHas important theoretical value and practical significance.
Disclosure of Invention
The invention aims to provide a method for synthesizing flower-shaped SnO with high dispersibility and uniform size in one step by adopting a hydrothermal synthesis method and taking trisodium citrate as an additive and tin dichloride as a tin salt2The nano material solves the problems of high cost, complex synthesis steps, complex post-treatment process and the like in the prior synthesis technology, and can be widely applied to the field of gas sensing.
In order to achieve the purpose, the invention provides the following technical scheme: method for preparing flower-shaped nano SnO by hydrothermal synthesis2A method of gas sensing materials, characterized by the steps of:
step 1: preparation of the precursor
Under the condition of room temperature, dissolving 1.0 mmol-4.0 mmol of tin dichloride dihydrate and 5.0 mmol-10 mmol of sodium citrate dihydrate in 20mL of deionized water, stirring for 10 minutes, adding 1.0 mmol-2.0 mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, placing into a stainless steel autoclave, keeping for 12 hours under the hydrothermal condition of 180 ℃, cooling to room temperature, centrifuging, and washing to obtain a precursor;
step 2: preparation of flower-like nano SnO2 material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material;
and step 3: carbon monoxide gas sensing performance test
Dispersing a certain amount of sample to be tested into 200 mu L of aqueous solution, uniformly dispersing by ultrasonic, taking 10 mu L of the sample to be tested, dripping the sample to the surface of the sensing device, naturally drying the sample, and then loading the sample into a sensing test system to test the sensing performance of various gases.
Further, the total flow rate of the gas in the step 3 is controlled to be constant at 200sscm through a gas flowmeter, and the sensing test temperature is 350 ℃.
Further, in the step 3, the gas sensitivity is defined as S ═ Rair/Rgas, and the response time T is1For sensing the gas entering, the sensing materialThe time required for the resistance change value of the material to fall to 90% of the maximum difference value, and the recovery time T2The time required for the resistance change value of the sensing material to rise to 90% of the maximum difference value after the sensing gas is turned off.
Further, Rair is the resistance value of the sensing material under the air condition, and Rgas is the resistance value of the sensing material under the air condition.
Compared with the prior art, the invention has the beneficial effects that: adopts a hydrothermal synthesis method, uses cheap trisodium citrate as an inducer to synthesize the SnO with a flower-shaped structure with uniform size and good dispersibility in one step2The nano material can be widely applied to dangerous chemical gas detection in various environments.
Drawings
FIG. 1 shows a flower-like SnO obtained by the present invention2Powder X-ray powder diffraction pattern of (1), and Rutile (Rutile) structure SnO2The standard spectra (JCPDS card number is 41-1445) are completely consistent, no impurity peak appears in the obtained XRD spectrum, and the obtained flower-shaped SnO is shown2Has high crystallinity;
FIG. 2 is a flower-like SnO prepared in accordance with example four of the present invention2The scanning electron microscope image clearly shows that the three-dimensional flower-like microspheres have uniform size distribution, the average particle diameter is 3-5 mu m, and the three-dimensional flower-like microspheres are formed by stacking a plurality of nano flaky structures;
FIG. 3 shows flower-like SnO prepared by the fourth embodiment of the invention at 350 ℃ working temperature2The change curve of the sensing sensitivity of the material to CO gas along with the increase of concentration (10-50 ppm). When the CO concentration was 10ppm, the response time and recovery time were 20s and 32s, respectively. The inner picture is flower-shaped SnO2A linear relationship between sensitivity and concentration for CO gas sensing.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
The first embodiment is as follows:
(1) preparation of the precursor
Dissolving 1.0mmol of tin dichloride dihydrate and 5.0mmol of sodium citrate dihydrate in 20mL of deionized water at room temperature, stirring for 10 minutes, adding 1.0mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, filling into a stainless steel autoclave, and keeping for 12 hours at 180 ℃ under hydrothermal conditions. Cooling to room temperature, centrifuging and washing to obtain the precursor.
(2) Flower-like nano SnO2Preparation of the Material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material.
Example two:
(1) preparation of the precursor
Dissolving 2.0mmol of tin dichloride dihydrate and 5.0mmol of sodium citrate dihydrate in 20mL of deionized water at room temperature, stirring for 10 minutes, adding 1.0mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, filling into a stainless steel autoclave, and keeping for 12 hours at 180 ℃ under hydrothermal conditions. Cooling to room temperature, centrifuging and washing to obtain the precursor.
(2) Flower-like nano SnO2Preparation of the Material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material.
Example three:
(1) preparation of the precursor
Dissolving 3.0mmol of tin dichloride dihydrate and 10mmol of sodium citrate dihydrate in 20mL of deionized water at room temperature, stirring for 10 minutes, adding 2.0mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, loading into a stainless steel autoclave, and keeping for 12 hours at 180 ℃ under hydrothermal conditions. Cooling to room temperature, centrifuging and washing to obtain the precursor.
(2) Flower-like nano SnO2Preparation of the Material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material.
Example four:
(1) preparation of the precursor
Dissolving 4.0mmol of tin dichloride dihydrate and 10mmol of sodium citrate dihydrate in 20mL of deionized water at room temperature, stirring for 10 minutes, adding 2.0mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, loading into a stainless steel autoclave, and keeping for 12 hours at 180 ℃ under hydrothermal conditions. Cooling to room temperature, centrifuging and washing to obtain the precursor.
(2) Flower-like nano SnO2Preparation of the Material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material.
(3) Carbon monoxide gas sensing performance test
Dispersing 10mg of a sample to be tested into 200 mu L of water solution, uniformly dispersing by ultrasonic, dripping 10 mu L of the sample to be tested on the surface of a sensing device, naturally drying, and then loading the sample to a sensing test system for testing the sensing performance of various gases. The total gas flow rate was controlled by a gas flow meter to be constant at 200sscm (standard cubic meter per minute) and the sensory test temperature was 350 ℃. Defining gas sensitivity as S ═ Rair/Rgas(wherein R isairIs the resistance value of the sensing material under air condition, RgasResistance value of the sensing material under air condition), response time T1The time required for the resistance change value of the sensing material to fall to 90% of the maximum difference value after the sensing gas enters, and the recovery time T2The time required for the resistance change value of the sensing material to rise to 90% of the maximum difference value after the sensing gas is turned off.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. Method for preparing flower-shaped nano SnO by hydrothermal synthesis2A method of gas sensing materials, characterized by the steps of:
step 1: preparation of the precursor
Under the condition of room temperature, dissolving 1.0 mmol-4.0 mmol of tin dichloride dihydrate and 5.0 mmol-10 mmol of sodium citrate dihydrate in 20mL of deionized water, stirring for 10 minutes, adding 1.0 mmol-2.0 mmol of sodium hydroxide, stirring for 30 minutes at room temperature, transferring to a 25mL polytetrafluoroethylene lining, placing into a stainless steel autoclave, keeping for 12 hours under the hydrothermal condition of 180 ℃, cooling to room temperature, centrifuging, and washing to obtain a precursor;
step 2: preparation of flower-like nano SnO2 material
Calcining the precursor for 2 hours at 500 ℃ under the condition of introducing air to obtain flower-shaped nano SnO2A material;
and step 3: carbon monoxide gas sensing performance test
Dispersing a certain amount of sample to be tested into 200 mu L of aqueous solution, uniformly dispersing by ultrasonic, taking 10 mu L of the sample to be tested, dripping the sample to the surface of the sensing device, naturally drying the sample, and then loading the sample into a sensing test system to test the sensing performance of various gases.
2. The method for preparing flower-shaped nano SnO by hydrothermal synthesis method according to claim 12A method of gas sensing materials, characterized by: the total flow of the gas in the step 3 is controlled by a gas flowmeter to be constant at 200sscm, and the sensing test temperature is 350 ℃.
3. The method for preparing flower-shaped nano SnO by hydrothermal synthesis method according to claim 12A method of gas sensing materials, characterized by: the gas sensitivity is defined as S ═ Rair/Rgas in the step 3, and the response time T1The time required for the resistance change value of the sensing material to fall to 90% of the maximum difference value after the sensing gas enters, and the recovery time T2The time required for the resistance change value of the sensing material to rise to 90% of the maximum difference value after the sensing gas is turned off.
4. The method for preparing the flower-like nano SnO2 gas-sensitive material by hydrothermal synthesis method according to claim 3, wherein: where Rair is the resistance value of the sensing material under air conditions, and Rgas is the resistance value of the sensing material under air conditions.
CN202010046709.0A 2020-01-16 2020-01-16 Method for preparing flower-shaped nano SnO by hydrothermal synthesis2Method for producing gas-sensitive material Pending CN113135587A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106542569A (en) * 2015-09-17 2017-03-29 天津工业大学 A kind of preparation method of flower ball-shaped tin ash
CN109682865A (en) * 2019-01-07 2019-04-26 北京工业大学 A kind of autoreduction preparation method of the stannic oxide nanometer flower gas sensitive of load gold nano grain
CN110194483A (en) * 2019-05-08 2019-09-03 武汉工程大学 A kind of SnO of multilevel structure2Nano material
US20190369040A1 (en) * 2018-06-05 2019-12-05 King Fahd University Of Petroleum And Minerals Room temperature nitrogen dioxide gas sensor
CN110606503A (en) * 2019-09-16 2019-12-24 安徽师范大学 Gold-modified porous tin dioxide micro-nanosheet composite material and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106542569A (en) * 2015-09-17 2017-03-29 天津工业大学 A kind of preparation method of flower ball-shaped tin ash
US20190369040A1 (en) * 2018-06-05 2019-12-05 King Fahd University Of Petroleum And Minerals Room temperature nitrogen dioxide gas sensor
CN109682865A (en) * 2019-01-07 2019-04-26 北京工业大学 A kind of autoreduction preparation method of the stannic oxide nanometer flower gas sensitive of load gold nano grain
CN110194483A (en) * 2019-05-08 2019-09-03 武汉工程大学 A kind of SnO of multilevel structure2Nano material
CN110606503A (en) * 2019-09-16 2019-12-24 安徽师范大学 Gold-modified porous tin dioxide micro-nanosheet composite material and preparation method and application thereof

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Application publication date: 20210720