CN108217717A - Preparation method of Mn doping stannic oxide gas sensitives and products thereof and application - Google Patents
Preparation method of Mn doping stannic oxide gas sensitives and products thereof and application Download PDFInfo
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- CN108217717A CN108217717A CN201711376114.6A CN201711376114A CN108217717A CN 108217717 A CN108217717 A CN 108217717A CN 201711376114 A CN201711376114 A CN 201711376114A CN 108217717 A CN108217717 A CN 108217717A
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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
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- 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
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
The present invention provides a kind of preparation method of Mn doping stannic oxides gas sensitive and products thereof and application, by the use of butter of tin, potassium permanganate and oxalic acid as presoma, it is synthesized by hydro-thermal method, again through dioxygen water process and making annealing treatment, the features of the present invention utilizes the good catalytic activity of Mn PARA FORMALDEHYDE PRILLS(91,95)s, in combination with the adjusting of surface Lacking oxygen, pass through the control to preparation process, the Mn dopen Nanos SnO of acquisition2PARA FORMALDEHYDE PRILLS(91,95) has the Mn dopen Nanos SnO prepared by the good air-sensitive performance present invention at a lower temperature2, have abundant Mn active sites, and with very high oxygen vacancy concentration, at a temperature of 180 DEG C, PARA FORMALDEHYDE PRILLS(91,95) has good sensitivity and selectivity.
Description
Technical field
The invention belongs to material chemistry technical field, be related to a kind of Mn doping stannic oxides gas sensitive preparation method and
Its product and application, the material formaldehyde gas detection sensitivity are high.
Background technology
In Semiconductor gas sensors investigation of materials field, tin oxide（SnO2）Because it is easy to regulate and control, selectivity is strong, stability is good,
The advantages that high sensitivity, for a long time as research hotspot.SnO2The gas sensing mechanism of gas-sensitive nano material can with exhaust layer model into
Row is explained.SnO2The oxygen vacancies on surface can become the electron donor of conduction band, so as to which the material be made to become n-type semiconductor.Therefore,
In practical applications, Adsorption by doped chemical can be provided, adjust the modes such as surface Lacking oxygen, promote its gas sensing property
Energy.
Invention content
In order to overcome the deficiencies of the prior art, it is an object of the invention to propose a kind of Mn doping stannic oxides gas sensitive
Preparation method.
Another object of the present invention is：Product prepared by a kind of above method is provided.
Another object of the present invention is to：A kind of application of the said goods is provided.
The object of the invention is realized by following proposal：A kind of preparation method of Mn doping stannic oxides gas sensitive, it is special
Sign is, by the use of butter of tin, potassium permanganate and oxalic acid as presoma, is synthesized by hydro-thermal method, then through dioxygen water process
With make annealing treatment, comprise the steps of：
（1）4mmol butters of tin and 10mmol oxalic acid are dissolved in 100ml ice water, are sufficiently stirred, adds 0.1-0.4mmol
Potassium permanganate is sufficiently stirred 1 hour；
（2）By step（1）Middle solution is transferred in hydrothermal reaction kettle, then reaction kettle is placed at 180 DEG C, hydro-thermal reaction by sealing
For a period of time, it is subsequently cooled to room temperature；
（3）By step（2）Prepared powder, centrifugation, washing；
（4）By step（3）Prepared sample adds in time of infusion in 30% hydrogen peroxide；
（5）By step（4）Prepared sample, centrifugation, washing, anneals a period of time under the conditions of 400 DEG C, obtains Mn doping two
Tin oxide gas sensitive.
On the basis of said program, step（2）The hydro-thermal reaction, time are 12-24 hours.
Step（4）Described to be impregnated in hydrogen peroxide, the time is 10-30 minutes.
Step（5）Described to anneal under the conditions of 400 DEG C, the time is 1-2 hours.
The present invention provides a kind of Mn doping stannic oxides gas sensitive, is prepared according to any of the above-described the method.
The present invention provides a kind of application of Mn doping stannic oxides gas sensitive in formaldehyde gas detection.
The present invention is advantageous in that：Using the good catalytic activity of Mn PARA FORMALDEHYDE PRILLS(91,95)s, in combination with the adjusting of surface Lacking oxygen,
Pass through the control to preparation process, the Mn dopen Nanos SnO of acquisition2PARA FORMALDEHYDE PRILLS(91,95) has good gas sensing property at a lower temperature
Energy.Mn dopen Nanos SnO prepared by the present invention2, there are abundant Mn active sites, and there is very high oxygen vacancy concentration,
At a temperature of 180 DEG C, PARA FORMALDEHYDE PRILLS(91,95) has good sensitivity and selectivity.
Description of the drawings
Fig. 1 is Mn dopen Nanos SnO prepared by embodiment 12The TEM pictures of particle；
Fig. 2 is Mn dopen Nanos SnO prepared by embodiment 12The air-sensitive performance figure of particle.
Specific embodiment
Embodiment 1
（1）4mmol butters of tin and 10mmol oxalic acid are dissolved in 100ml ice water, are sufficiently stirred, adds 0.1mmol Gao Meng
Sour potassium is sufficiently stirred 1 hour；
（2）By step（1）Middle solution is transferred in hydrothermal reaction kettle, then reaction kettle is placed at 180 DEG C, hydro-thermal reaction by sealing
12 hours, it is subsequently cooled to room temperature；
（3）By step（2）Prepared powder, centrifugation, washing.
（4）By step（3）Prepared sample is added in 30% hydrogen peroxide and is impregnated 10 minutes；
（5）By step（4）Prepared sample, centrifugation, washing, anneals 1 hour under the conditions of 400 DEG C, obtains Mn doping dioxies
Change tin gas sensitive.
It is Mn dopen Nanos SnO shown in material Fig. 1 of gained2The TEM pictures of particle, the Mn doping prepared by the present invention
Nano SnO2, have abundant Mn active sites, and with very high oxygen vacancy concentration.
Powder dispersion is applied on six foot ceramic tube air-sensitive testing elements made from the present embodiment, tests various concentration PARA FORMALDEHYDE PRILLS(91,95)
Response, operating temperature be 180 DEG C.Fig. 2 is prepared Mn dopen Nanos SnO2The air-sensitive performance figure of particle.The present invention utilizes Mn
The good catalytic activity of PARA FORMALDEHYDE PRILLS(91,95), in combination with the adjusting of surface Lacking oxygen, by the control to preparation process, the Mn of acquisition mixes
Miscellaneous nano SnO2PARA FORMALDEHYDE PRILLS(91,95) has good sensitivity and selectivity at a lower temperature.
Embodiment 2
（1）4mmol butters of tin and 10mmol oxalic acid are dissolved in 100ml ice water, are sufficiently stirred, adds 0.2mmol Gao Meng
Sour potassium is sufficiently stirred 1 hour；
（2）By step（1）Middle solution is transferred in hydrothermal reaction kettle, then reaction kettle is placed at 180 DEG C, hydro-thermal reaction by sealing
18 hours, it is subsequently cooled to room temperature；
（3）By step（2）Prepared powder, centrifugation, washing.
（4）By step（3）Prepared sample is added in 30% hydrogen peroxide and is impregnated 30 minutes；
（5）By step（4）Prepared sample, centrifugation, washing, anneals 1.5 hours under the conditions of 400 DEG C, obtains Mn doping two
Tin oxide gas sensitive.
Embodiment 3
（1）4mmol butters of tin and 10mmol oxalic acid are dissolved in 100ml ice water, are sufficiently stirred, adds 0.4mmol Gao Meng
Sour potassium is sufficiently stirred 1 hour；
（2）By step（1）Middle solution is transferred in hydrothermal reaction kettle, then reaction kettle is placed at 180 DEG C, hydro-thermal reaction by sealing
24 hours, it is subsequently cooled to room temperature；
（3）By step（2）Prepared powder, centrifugation, washing.
（4）By step（3）Prepared sample is added in 30% hydrogen peroxide and is impregnated 20 minutes；
（5）By step（4）Prepared sample, centrifugation, washing, anneals 2 hours under the conditions of 400 DEG C, obtains Mn doping dioxies
Change tin gas sensitive.
Powder dispersion is applied on six foot ceramic tube air-sensitive testing elements made from this above-described embodiment 1-3, and test is different dense
The response of PARA FORMALDEHYDE PRILLS(91,95) is spent, operating temperature is 180 DEG C.
The description of the above embodiments is understood that for ease of those skilled in the art and using the present invention.
Person skilled in the art obviously can easily make these embodiments various modifications, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to embodiment here, sheets
Field technology personnel announcement according to the present invention, the improvement made for the present invention and modification all should be in the protection models of the present invention
Within enclosing.
Claims (6)
1. a kind of preparation method of Mn doping stannic oxides gas sensitive, which is characterized in that with butter of tin, potassium permanganate and grass
Acid is synthesized, then through dioxygen water process and make annealing treatment by hydro-thermal method, is comprised the steps of as presoma：
（1）4mmol butters of tin and 10mmol oxalic acid are dissolved in 100ml ice water, are sufficiently stirred, adds 0.1-0.4mmol
Potassium permanganate is sufficiently stirred 1 hour；
（2）By step（1）Middle solution is transferred in hydrothermal reaction kettle, then reaction kettle is placed at 180 DEG C, hydro-thermal reaction by sealing
For a period of time, it is subsequently cooled to room temperature；
（3）By step（2）Prepared powder, centrifugation, washing；
（4）By step（3）Prepared sample adds in time of infusion in 30% hydrogen peroxide；
（5）By step（4）Prepared sample, centrifugation, washing, anneals a period of time under the conditions of 400 DEG C, obtains Mn doping two
Tin oxide gas sensitive.
2. the preparation method of Mn doping stannic oxides gas sensitive according to claim 1, which is characterized in that step（2）Institute
Hydro-thermal reaction is stated, the time is 12-24 hours.
3. the preparation method of Mn doping stannic oxides gas sensitive according to claim 1, which is characterized in that step（4）Institute
It states and is impregnated in hydrogen peroxide, the time is 10-30 minutes.
4. the preparation method of Mn doping stannic oxides gas sensitive according to claim 1, which is characterized in that step（5）Institute
It states and anneals under the conditions of 400 DEG C, the time is 1-2 hours.
5. a kind of Mn doping stannic oxides gas sensitive, it is characterised in that be prepared into according to any the methods of claim 1-4
It arrives.
6. a kind of application of the doping stannic oxides of Mn according to claim 6 gas sensitive in formaldehyde gas detection.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711376114.6A CN108217717B (en) | 2017-12-19 | 2017-12-19 | Preparation method of Mn-doped tin dioxide gas-sensitive material, product and application thereof |
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| CN201711376114.6A CN108217717B (en) | 2017-12-19 | 2017-12-19 | Preparation method of Mn-doped tin dioxide gas-sensitive material, product and application thereof |
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| CN108217717A true CN108217717A (en) | 2018-06-29 |
| CN108217717B CN108217717B (en) | 2020-02-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1737558A (en) * | 2005-06-16 | 2006-02-22 | 广州大学 | Stannic oxide based nanometer rod air-sensitive material and process for preparing the same |
| CN105152202A (en) * | 2015-07-17 | 2015-12-16 | 济南大学 | Preparation method for antimony-doped flower-ball-shaped tin dioxide gas-sensing material |
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2017
- 2017-12-19 CN CN201711376114.6A patent/CN108217717B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1737558A (en) * | 2005-06-16 | 2006-02-22 | 广州大学 | Stannic oxide based nanometer rod air-sensitive material and process for preparing the same |
| CN105152202A (en) * | 2015-07-17 | 2015-12-16 | 济南大学 | Preparation method for antimony-doped flower-ball-shaped tin dioxide gas-sensing material |
Non-Patent Citations (4)
| Title |
|---|
| A.-M. UNGUREANU ET AL.: "STRUCTURAL CHARACTERISATION AND LUMINESCENCE PROPERTIES OF PARAMAGNETIC Mn DOPED SnO2 NANOPOWDERS OBTAINED VIA SIMPLE BUTHANOL ASSISTED SOL-GEL SYNTHESIS", 《DIGEST JOURNAL OF NANOMATERIALS AND BIOSTRUCTURES》 * |
| HUIQIN ZHANG ET AL.: "Photoelectrochemical performance of birnessite films and photoelectrocatalytic activity toward oxidation of phenol", 《JOURNAL OF ENVIRONMENTAL SCIENCES》 * |
| MOHAMED M. RASHAD ET AL.: "Decomposition of Methylene Blue on Transition Metals Doped SnO2 Nanoparticles", 《CLEAN – SOIL, AIR, WATER》 * |
| 王利军等: "锰掺杂诱导正交相SnO2的生长行为", 《上海大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
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