CN109682867A - A kind of micron order tin dioxide gas-sensitive material and its preparation method and application - Google Patents
A kind of micron order tin dioxide gas-sensitive material and its preparation method and application Download PDFInfo
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- CN109682867A CN109682867A CN201910065075.0A CN201910065075A CN109682867A CN 109682867 A CN109682867 A CN 109682867A CN 201910065075 A CN201910065075 A CN 201910065075A CN 109682867 A CN109682867 A CN 109682867A
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- 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
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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Abstract
The invention discloses a kind of micron order tin dioxide gas-sensitive materials and its preparation method and application, and stannous chloride and ethyl alcohol are configured to solution；It is then transferred into reaction kettle, by the reaction of certain time, obtains the mixed solution containing solid-like stannic oxide after reaction system is cooling, obtain faint yellow pure phase stannic oxide micron particles by being centrifuged, drying.The present invention is micron SnO2Environmentally protective industrialized production in terms of a kind of completely new resolving ideas and process flow are provided, method and process is simple and easy, reproducible.And entire reaction system, without any pollution, is a kind of environmentally protective micro-powder synthesis technology to environment.There is very strong practicability in gas sensor, while also with good application prospect and economic benefit.
Description
Technical field
The invention belongs to gas-sensitive nano material synthesis and sensor technical fields, and in particular to a kind of micron order stannic oxide
Gas sensitive and its preparation method and application.
Background technique
With the progress of science and technology, people's living standard is stepped up, but industrial or agricultural and people's daily routines discharge
Gas also increase.In these gases, some are inflammable and explosive, such as the gases such as hydrogen, alcohol, first institute；Some are
Have virose, such as gases such as formaldehyde, hydrogen sulfide, carbon monoxide；Detection for these gases is one that people to be solved
Hang-up, this is for producing and life is of great significance, and gas sensor plays this indispensable role.
Gas sensor is capable of detecting when the ingredient and concentration of gas, and converts usable output signal for relevant information,
To play the functions such as detection, alarm to gas.Up to the present, gas sensor can be divided into following a few classes: semiconductor-type,
Catalytic combustion type, electric chemical formula and thermal conductivity, wherein semiconductor gas sensor due to high sensitivity, at low cost, performance is steady
The advantages that determining is current most study, most popular gas sensitive device.And in these semiconductor gas sensors, SnO2Again
It is to study and apply most gas sensitives.
Stannic oxide is a kind of important broad-band gap (3.6-4.0eV) metal oxide semiconductor material, and crystal is gold
Red stone structure, structure cell are body-centered-orthorhomic parallelepipeds.Stannic oxide can be used as gas sensitive, mainly since it is in certain temperature
When contacting certain gas under degree, its resistance can change, in addition, since stannic oxide belongs to N-type semiconductor, when it is adsorbed
When reducibility gas, its resistance returns decline, and when its adsorption and oxidation gas, its resistance can be increased.Come from preparation process
It says, the method for preparing stannic oxide at present is generally divided into solwution method, solid precursor hot-cast socket method, electrochemical deposition method and hot oxygen
Change method etc..Stannic oxide (the SnO of the different-shape of different method preparations2) gas sensitive, air-sensitive performance has very big
Difference.Such as a series of stannic oxide (SnO with different-diameter are prepared by template of carbon ball2) tiny balloon, find crystal ruler
The very little tiny balloon for 12.7nm is to nitrogen dioxide (NO2) most sensitive.As Chiu et al. uses SnCl4Position is raw material, using hydro-thermal
The nano particle that the size of method preparation is 3.0nm, surface area have reached 130m2/ g, at 220 DEG C to 25mg/L (ppm) ethyl alcohol
Response reach 26, response and recovery time are respectively 30s and 18s.Although being prepared for by the above method with different-shape
And adulterate the SnO of the micro-nano structure of different metal and metal oxide2Gas sensor, the more traditional SnO of air-sensitive performance2
Gas sensor is greatly improved, but still there are some problems, such as poor selectivity, operating temperature is low, responds and extensive
The multiple time is slow, and preparation process is complicated, and selected raw material is more and to environmental and human health impacts nocuousness, therefore, how to improve
Titanium dioxide is to the research hotspot that the selectivity of gas and sensitivity, reduction operating temperature, optimization preparation process are still from now on
In conclusion the Study on Preparation of highly sensitive micron order tin dioxide gas-sensitive material not only has important
Art value, and with important practical value, for this purpose, preparing and studying highly sensitive micron order stannic oxide air-sensitive material
The synthesis technology of material seems extremely important.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of simple, green
Color, micron order tin dioxide gas-sensitive material of high-purity and its preparation method and application, entire simple process, pollution-free, operation
Process is simple, repeatability is high, can get the tin dioxide powder of high-purity, is had by its sensor made to alcohol gas
High sensitivity under low concentration, the advantages that response and recovery time are fast.
The invention adopts the following technical scheme:
A kind of preparation method of micron order tin dioxide gas-sensitive material, is configured to solution for stannous chloride and ethyl alcohol；Then
It is transferred in reaction kettle, by the reaction of certain time, is obtained after reaction system is cooling mixed containing solid-like stannic oxide
Solution is closed, obtains faint yellow pure phase stannic oxide micron particles by being centrifuged, drying.
Specifically, the stannous chloride of 1~2mmol is added in ethyl alcohol, ethyl alcohol accounts for the 70~80% of reaction kettle capacity.
Specifically, the solution of configuration is transferred in reaction kettle, 160~240 are warming up to the rate of 5~10 DEG C/min
DEG C, the mixed solution containing solid-like stannic oxide is obtained after warm processing.
Further, the time of isothermal holding is 4~8h.
Further, the set temperature of reaction kettle is 180~220 DEG C.
Specifically, the rate of centrifugal treating is 5000~10000r/min, the time is 3~6min.
Further, the number of centrifugal treating is 2~4 times.
Specifically, the temperature being dried is 60~80 DEG C, the time is 2~6h.
Another technical solution of the invention is a kind of micron order stannic oxide micron particles, stannic oxide micron particles
Partial size is 1~3 micron.
Another technical solution of the invention is a kind of gas sensor of micron order stannic oxide micron particles preparation.
Compared with prior art, the present invention at least has the advantages that
A kind of preparation method of micron order tin dioxide gas-sensitive material of the present invention, raw material and generation in entire technical process
Solution is easy to handle and pollution-free, and preparation cost is low, and operating process is simple, and repeatability is high, can prepare the micron of high-purity
The spherical tin dioxide powder of grade, entire reaction system, without any pollution, are a kind of environmentally protective micro-powder synthesis to environment
Technique.There is very strong practicability in gas sensor, while also with good application prospect and economic benefit.
The invention also discloses a kind of gas sensor, gas made of the tin dioxide powder using the method for the present invention preparation
Body sensor shows excellent air-sensitive performance, and the response to alcohol is that commercially available SnO_2 gas sensor responds alcohol
10 times or so, in addition, (1ppm) still has that high sensitivity, response recovery time is fast, work to alcohol gas at low concentrations
Make the advantages such as temperature is low, furthermore it has been found that its PARA FORMALDEHYDE PRILLS(91,95) gas also has higher response.
In conclusion the present invention is micron SnO2Environmentally protective industrialized production in terms of a kind of completely new solution be provided think
Road and process flow.This method is simple for process, reproducible.And entire reaction system, without any pollution, is to environment
A kind of environmentally protective micro-powder synthesis technology.There is very strong practicability in gas sensor, while also having preferable
Application prospect and economic benefit.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the XRD spectrum of embodiment 1；
Fig. 2 is the SEM photograph of embodiment 1；
Fig. 3 is the XRD spectrum of embodiment 2；
Fig. 4 is the SEM photograph of embodiment 2；
Fig. 5 is the XRD spectrum of embodiment 3；
Fig. 6 is the SEM photograph of embodiment 3；
Fig. 7 is gas sensor made by the tin dioxide powder that is prepared using the method for the present invention in 100ppm concentration second
Response in alcohol gas at a temperature of different operating；
Fig. 8 is gas sensor made by the tin dioxide powder that is prepared using the method for the present invention to different concentration ethanol
The response of gas；
Fig. 9 is gas sensor made by the tin dioxide powder that is prepared using the method for the present invention in 100ppm ethanol gas
Response time and recovery time in bulk concentration；
Figure 10 is gas sensor made by the tin dioxide powder that is prepared using the method for the present invention in 100ppm ethyl alcohol
Loop test in gas concentration；
Figure 11 is gas sensor made by the tin dioxide powder that is prepared using the method for the present invention to 100ppm concentration
Four kinds of gases (ammonia, dimethylbenzene, acetone, ethyl alcohol) response；
Figure 12 is gas sensor and commercially available titanium dioxide made by the tin dioxide powder that prepare using the method for the present invention
The response comparison diagram of tin sensor.
Specific embodiment
The present invention provides a kind of preparation methods of micron order tin dioxide gas-sensitive material, are matched using conventional stannous chloride
It is set to solution；It is then transferred into reaction kettle, by the reaction of certain time, after reaction system is cooling, by being centrifuged, drying
Obtain pure phase stannic oxide SnO2Micron particles overcome and use sodium hydroxide highly basic for presoma to meeting in prior art route
Lead to the pollution of ecology and causes dangerous disadvantage to human body.
A kind of preparation method of micron order tin dioxide gas-sensitive material of the present invention, comprising the following steps:
S1, the stannous chloride of 1~2mmol is placed in a certain amount of alcohol solvent, the amount of alcohol solvent is reaction kettle
The 70~80% of capacity, are configured to solution；
S2, the step S1 solution configured is transferred in reaction kettle, is warming up to 160 with the heating rate of 5~10 DEG C/min
~240 DEG C, 4~8h is then kept the temperature, in the process, solution reacts, to after the reaction was completed, obtain containing solid-like dioxy
Change the mixed solution of tin；
Preferably, the set temperature of reaction kettle is 180~220 DEG C.
S3, the mixed solution containing solid-like stannic oxide is taken out from reaction kettle, transfer them in centrifuge tube and carry out
Centrifuge separation, centrifugation rate are 5000~10000r/min, and the time is 3~6min, and number is 2~4 times, obtain solid-like dioxy
Change tin；
S4, it the solid-like stannic oxide is transferred to drying device is dried, drying temperature is 60~80 DEG C, through 2
~6h obtains finished product tin dioxide powder after being dried.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being described and shown in usually here in attached drawing is real
The component for applying example can be arranged and be designed by a variety of different configurations.Therefore, below to the present invention provided in the accompanying drawings
The detailed description of embodiment be not intended to limit the range of claimed invention, but be merely representative of of the invention selected
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
It weighs 1mmol stannous chloride to be dissolved in 30mL dehydrated alcohol, stirring obtains clear transparent solutions to dissolving；
Then clear solution is transferred in reaction kettle again, and then reaction kettle is put into baking oven and is heated, by reaction kettle
220 DEG C are heated to, then 6 hours is kept the temperature, is being since room temperature, with the liter of 5 DEG C/min to the heating process that reaction kettle heats
Warm rate is heated to 160 DEG C；
In above-mentioned process, the stannous chloride in clear solution chemically reacts in dehydrated alcohol, generates containing solid
The mixed solution of state stannic oxide；
After reaching soaking time, reaction kettle cooled to room temperature takes out mixed solution from reaction kettle, places centrifugation
It is centrifuged in machine, wherein the centrifugation rate of centrifuge is set as 8000r/min, centrifugation time 3min, and centrifugation number is
3 times；
After the completion of the centrifuge separation of centrifuge, solid-state like stannic oxide is collected, is placed by solid-state like stannic oxide
It is dried into drying device, such as drying 6 hours at 60 DEG C obtain faint yellow tin dioxide powder after the completion of dry.
Embodiment 2
It weighs 1mmol stannous chloride to be dissolved in 35mL dehydrated alcohol, stirring obtains clear transparent solutions to dissolving；
Then clear solution is transferred in reaction kettle again, and then reaction kettle is put into baking oven and is heated, by reaction kettle
200 DEG C are heated to, then 6 hours is kept the temperature, is being since room temperature, with the liter of 10 DEG C/min to the heating process that reaction kettle heats
Warm rate is heated to 240 DEG C；
In above-mentioned process, the stannous chloride in clear solution chemically reacts in dehydrated alcohol, generates containing solid
The mixed solution of state stannic oxide；
After reaching soaking time, reaction kettle cooled to room temperature takes out mixed solution from reaction kettle, places centrifugation
It is centrifuged in machine, wherein the centrifugation rate of centrifuge is set as 5000r/min, centrifugation time 6min, and centrifugation number is
4 times；
After the completion of the centrifuge separation of centrifuge, solid-state like stannic oxide is collected, is placed by solid-state like stannic oxide
It is dried into drying device, such as drying 2 hours at 80 DEG C obtain faint yellow tin dioxide powder after the completion of dry.
Embodiment 3:
It weighs 1mmol stannous chloride to be dissolved in 40mL dehydrated alcohol, stirring obtains clear transparent solutions to dissolving；
Then clear solution is transferred in reaction kettle again, and then reaction kettle is put into baking oven and is heated, by reaction kettle
180 DEG C are heated to, then 4 hours is kept the temperature, is being since room temperature, with the liter of 8 DEG C/min to the heating process that reaction kettle heats
Warm rate is heated to 180 DEG C；
In above-mentioned process, the stannous chloride in clear solution chemically reacts in dehydrated alcohol, generates containing solid
The mixed solution of state stannic oxide；
After reaching soaking time, reaction kettle cooled to room temperature takes out mixed solution from reaction kettle, places centrifugation
It is centrifuged in machine, wherein the centrifugation rate of centrifuge is set as 10000r/min, centrifugation time 5min, and centrifugation number is
2 times；
After the completion of the centrifuge separation of centrifuge, solid-state like stannic oxide is collected, is placed by solid-state like stannic oxide
It is dried into drying device, such as drying 4 hours at 70 DEG C obtain faint yellow tin dioxide powder after the completion of dry.
Embodiment 4
It weighs 2mmol stannous chloride to be dissolved in 40mL dehydrated alcohol, stirring obtains clear transparent solutions to dissolving；
Then clear solution is transferred in reaction kettle again, and then reaction kettle is put into baking oven and is heated, by reaction kettle
200 DEG C are heated to, then 8 hours is kept the temperature, is being since room temperature, with the liter of 5 DEG C/min to the heating process that reaction kettle heats
Warm rate is heated to 200 DEG C；
In above-mentioned process, the stannous chloride in clear solution chemically reacts in dehydrated alcohol, generates containing solid
The mixed solution of state stannic oxide；
After reaching soaking time, reaction kettle cooled to room temperature takes out mixed solution from reaction kettle, places centrifugation
It is centrifuged in machine, wherein the centrifugation rate of centrifuge is set as 7000r/min, centrifugation time 5min, and centrifugation number is 4
It is secondary；
After the completion of the centrifuge separation of centrifuge, solid-state like stannic oxide is collected, is placed by solid-state like stannic oxide
It is dried into drying device, such as drying 5 hours at 70 DEG C obtain faint yellow tin dioxide powder after the completion of dry.
In addition, in the method for the invention, the reaction kettle of inner lining material can also be selected, if the liner of reaction kettle not with
Stannous chloride chemically reacts, the heating to reaction kettle, can also be controlled using other heating rates.
Fig. 1,3 and 5 are please referred to, using X-ray diffractometer to obtained using the method for the present invention between 20~80 degree
Stannic oxide is scanned, all diffraction maximums and SnO2Standard card (PDF#04-009-8478) fits like a glove, not any
Miscellaneous peak occurs, and thus proves, the stannic oxide prepared using the above method has very high purity.
Fig. 2,4 and 6 are please referred to, from SEM pattern photo it is known that the micron order titanium dioxide prepared using the method for the present invention
Tin, stannic oxide are evenly distributed, micron bulb diameter is in 1~3 microns in spherical.
Referring to Fig. 7, using the method for the present invention preparation tin dioxide powder made by gas sensor, in fixation
In the alcohol gas of 100ppm concentration, sensor can show higher response at lower operating temperature (230 DEG C)
24.9 and most fast response time 3s.Compared to the SnO_2 gas sensor of other reports, the sensing of the method for the present invention preparation
Device has lower operating temperature.
Referring to Fig. 8, using the method for the present invention preparation tin dioxide powder made by gas sensor, sensor pair
Different concentration ethanol gas all has accordingly, especially under low-concentration ethanol environment (1ppm), still has high response
(7.24) and response and recovery time are fast.
Referring to Fig. 9, being gas sensor made by the tin dioxide powder using the method for the present invention preparation, in 100ppm
Response time and recovery time in ethanol gas concentration have reached 3s and 24s.
Referring to Fig. 10, existing for gas sensor made by the tin dioxide powder that is prepared using the method for the present invention
Loop test in 100ppm ethanol gas concentration, the response of sensor is held essentially constant in six loop tests, is said
Bright sensor has stability.
Figure 11 is please referred to, to use gas sensor made by the tin dioxide powder of the method for the present invention preparation, most
Under good operating temperature (230 DEG C), response to four kinds of gases (ammonia, dimethylbenzene, acetone, ethyl alcohol) of 100ppm concentration, discovery pair
The response highest of ethyl alcohol, so sensor have to alcohol gas it is highly selective.
Figure 12 is please referred to, is gas sensor and commercially available made by the tin dioxide powder using the method for the present invention preparation
SnO_2 gas sensor such as believes emerging microelectronics MQ-3 gas sensor, at different temperatures to pair of alcohol gas response
Than, as shown in figure 4, using the method for the present invention preparation tin dioxide powder made by gas sensor, in optimum working temperature
Under, such as 230 DEG C, the response to alcohol gas is that commercially available SnO_2 gas sensor such as believes emerging microelectronics MQ-3 gas sensing
Device 10 times or so that alcohol gas is responded.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of preparation method of micron order tin dioxide gas-sensitive material, which is characterized in that stannous chloride and ethyl alcohol to be configured to
Solution；It is then transferred into reaction kettle, by the reaction of certain time, obtains after reaction system is cooling containing solid-like dioxy
The mixed solution for changing tin obtains faint yellow pure phase stannic oxide micron particles by being centrifuged, drying.
2. the preparation method of micron order tin dioxide gas-sensitive material according to claim 1, which is characterized in that by 1~
The stannous chloride of 2mmol is added in ethyl alcohol, and ethyl alcohol accounts for the 70~80% of reaction kettle capacity.
3. the preparation method of micron order tin dioxide gas-sensitive material according to claim 1, which is characterized in that by configuration
Solution is transferred in reaction kettle, is warming up to 160~240 DEG C with the rate of 5~10 DEG C/min, is obtained after warm processing containing solid
The mixed solution of body shape stannic oxide.
4. the preparation method of micron order tin dioxide gas-sensitive material according to claim 3, which is characterized in that isothermal holding
Time be 4~8h.
5. the preparation method of micron order tin dioxide gas-sensitive material according to claim 3, which is characterized in that reaction kettle
Set temperature is 180~220 DEG C.
6. the preparation method of micron order tin dioxide gas-sensitive material according to claim 1, which is characterized in that centrifugal treating
Rate be 5000~10000r/min, the time be 3~6min.
7. the preparation method of micron order tin dioxide gas-sensitive material according to claim 6, which is characterized in that centrifugal treating
Number be 2~4 times.
8. the preparation method of micron order tin dioxide gas-sensitive material according to claim 1, which is characterized in that be dried
Temperature be 60~80 DEG C, the time be 2~6h.
9. using the micron order stannic oxide micron particles of claim 1 the method preparation, the grain of stannic oxide micron particles
Diameter is 1~3 micron.
10. the gas sensor of the micron order stannic oxide micron particles preparation using the preparation of claim 1 the method.
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| CN111229198A (en) * | 2020-03-02 | 2020-06-05 | 陕西科技大学 | Amorphous/crystalline structure SnO2Preparation method of @ GO heterojunction composite material and photocatalytic application thereof |
| CN111484071A (en) * | 2020-03-02 | 2020-08-04 | 陕西科技大学 | SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111229198A (en) * | 2020-03-02 | 2020-06-05 | 陕西科技大学 | Amorphous/crystalline structure SnO2Preparation method of @ GO heterojunction composite material and photocatalytic application thereof |
| CN111484071A (en) * | 2020-03-02 | 2020-08-04 | 陕西科技大学 | SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof |
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