CN109502632A - A kind of multistage SnO2The preparation method and applications of nanotube-shaped gas sensitive - Google Patents
A kind of multistage SnO2The preparation method and applications of nanotube-shaped gas sensitive Download PDFInfo
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- CN109502632A CN109502632A CN201811636425.6A CN201811636425A CN109502632A CN 109502632 A CN109502632 A CN 109502632A CN 201811636425 A CN201811636425 A CN 201811636425A CN 109502632 A CN109502632 A CN 109502632A
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- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses a kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, comprising the following steps: (1) PVP is added in ethylene glycol and is stirred, ultrasound obtains a solution;(2) molybdenum oxide nano rod is added in a solution, it is evenly dispersed to obtain b solution;(3) stannous chloride solution and thioacetyl amine aqueous solution are added in b solution, are transferred in reaction kettle after stirring, incubation water heating 10-14h;(4) it is collected by centrifugation with dehydrated alcohol, is then transferred to gained precipitating in beaker with dehydrated alcohol after cooling, ammonium hydroxide is added, stirred 1-2h, be collected by centrifugation, and gained is precipitated into drying, obtain SnS2;(5) by gained SnS2Be put into tube furnace calcine to get.Raw material of the present invention are cheap and easy to get, and operating method is simple, energy consumption is lower, repeatable strong and yield is high, multistage SnO suitable for mass production, and being prepared2Nanotube-shaped gas sensitive can be used for the materials such as sensor, catalyst, catalyst carrier, have good application prospect.
Description
Technical field
The present invention relates to gas sensitive technical field more particularly to a kind of multistage SnO2The preparation of nanotube-shaped gas sensitive
Method and its application.
Background technique
In recent years, the exploitation and application of the development greatly pushing function material of nanosecond science and technology.Size, the shape of nano material
Looks and component all can greatly influence the property of itself, to influence its application prospect.So far, two-dimensional slice, hollow
Tubulose or three-dimensional multistage nanometer semiconductor structure and multi-component modulation cause researcher's greatly interest, become and receive
The new hot spot of rice investigation of materials.Such material has large specific surface area, the advantage of structure opening, so have in gas sensitive field
There is extremely important application value.
Gas sensitive is related to the interaction between sensitive material surface and adsorption gas molecule, passes through charge between the two
Transfer causes the chemical property of sensitive material to change, and generates gas sensitive signal.More crucially change in above process
Function and effect between kind sensitive material and gas molecule.Therefore, the specific surface area of air-sensitive nano material is improved, sensitivity is also
Nowadays the crucial direction of gas sensitive research.
The method that tradition prepares gas-sensitive nano material requires greatly the reaction item of cumbersome step, expensive instrument and harshness
Part, and volatile toxic reagent is used, human health and ambient enviroment are all affected.Therefore, selection is simple, passes through
Ji, environmental-friendly synthetic method, obtain structure optimization, the multi-stage nano superstructure gas sensitive haveing excellent performance is also air-sensitive material
Expect the trend of development.
Summary of the invention
It is an object of the invention to: in view of the above problems, provide a kind of multistage SnO2Nanotube-shaped gas sensitive
Preparation method and applications, this method preparation cost is low, environmental-friendly, and repeatability is strong, multistage SnO2Nanotube superstructure
Nano material large specific surface area, be widely used in transparent conductive film, gas sensor, photocatalysis and solar energy conversion etc. neck
Domain.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, comprising the following steps:
(1) PVP is added in ethylene glycol and is stirred, then ultrasound to solution is clarified, and obtains a solution;
(2) molybdenum oxide nano rod is added in a solution, stirring is dispersed in a solution to molybdenum oxide, and it is molten to obtain b
Liquid;
(3) stannous chloride solution and thioacetyl amine aqueous solution are added in b solution, are transferred in reaction kettle after stirring,
Incubation water heating 10-14h;
(4) it is collected by centrifugation with dehydrated alcohol, 3-6 times repeatedly, then shifts gained precipitating with dehydrated alcohol after cooling
Into beaker, ammonium hydroxide is added, stirs 1-2h, then be collected by centrifugation with dehydrated alcohol, cleans 3-6 times repeatedly, and gained is precipitated and is done
It is dry, obtain SnS2;
(5) by gained SnS2Be put into tube furnace under air atmosphere calcine to get.
Preferably, the solid-to-liquid ratio of the PVP and ethylene glycol is 1:45-100.
Preferably, the additive amount of the molybdenum oxide is the 0.05-0.15% of a solution weight.
Preferably, the mass ratio of the stannous oxide solution and the thioacetyl amine aqueous solution is 1:1-1.2;The chlorination
The total weight of stannous solution and thioacetyl amine aqueous solution is the 10-18% of b solution weight.
Preferably, the stannous oxide solution is that 0.5-0.9g stannous chloride is dissolved in 10mL ethylene glycol;It is described thio
Acetamide solution is that 0.1-0.5g thioacetamide is dissolved in 10mL ethylene glycol.
Preferably, the reaction kettle is the stainless steel cauldron of 50mL polytetrafluoroethyllining lining, the perseverance in step (3)
The temperature of warm water heat is 150-170 DEG C.
Preferably, the temperature of the drying is 40-50 DEG C, time 8-14h in step (4).
Preferably, the temperature of the calcining is 380-420 DEG C, calcination time 20-26h, heating rate in step (5)
For 5 DEG C/min.
The present invention also provides the multistage SnO obtained produced above2Nanotube-shaped gas sensitive is in transparent conductive film, sensing
The application of device, catalyst and catalyst carrier material.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) multistage SnO of the invention2The preparation method of nanotube-shaped gas sensitive, directly by SnS2Hollow pipe is changed into more
Grade SnO2Nanotube-shaped gas sensitive, using simple hydro-thermal method and annealing technology, raw material it is cheap and easy to get and for
It is environmental-friendly;Using molybdenum oxide as template, by SnS2The gas sensitive that hollow pipe predecessor situ converting comes, a large amount of SnO2Nanometer
Piece is stacked into novel tubular structure, basic construction unit SnO2Nanometer sheet thickness is about 4nm, and piece and piece are in multistage three-dimensional structure
It stacks, specific surface area and diffusion admittance quantity significantly increase, and are expected to the improvement of auxiliary gas sensor performance.
(2) raw material of the invention are cheap and easy to get, and used preparation method is environmental-friendly, and hydrothermal temperature is low, and energy consumption is small.
(3) preparation-obtained multistage SnO2The gas sensitive of nanotube superstructure is by the SnS of easy slabbing structure2It is empty
Heart pipe situ converting forms, and pattern is special rare, contacts large specific surface area.
(4) the multistage SnO prepared by2The gas sensitive of nanotube superstructure can be used for sensor, catalyst, catalyst and carry
The materials such as body have good application prospect.
Detailed description of the invention
Fig. 1 is prepared by SnS in embodiment 12Hollow pipe is changed into multistage SnO2The gas sensitive of nanotube superstructure
SEM figure;
Fig. 2 is prepared by SnS in embodiment 22Hollow pipe is transformed into multistage SnO2The air-sensitive material of nanotube superstructure
The SEM of material schemes;
Fig. 3 is prepared by SnS in embodiment 12Hollow pipe is transformed into multistage SnO2The air-sensitive material of nanotube superstructure
The TEM of material schemes;
Fig. 4 is prepared by SnS in embodiment 22Hollow pipe is transformed into multistage SnO2The air-sensitive material of nanotube superstructure
The TEM of material schemes;
Fig. 5 is prepared SnS in embodiment 12And SnO2XRD diagram, figure (a) be presoma SnS2Diffraction peak figure, figure
(b) SnO for being2Diffraction maximum.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
The one or more aspects of invention have a thorough explanation, also may be implemented even without these specific details of the invention
These aspects.
The ethylene glycol that the present invention uses is that volume content is 29.6%, and (20 DEG C) of density are 1.041.
Embodiment 1
A kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, comprising the following steps:
(1) 0.45gPVP (MW.58000) is added in 25ml ethylene glycol and stirs 30min, and ultrasound 10min is clear to solution
Clearly, a solution is obtained;
(2) 15mg molybdenum oxide nano rod being added in a solution, stirring 1h to molybdenum oxide is evenly dispersed in a solution,
Obtain b solution;
(3) by 1.6ml stannous chloride solution (0.758g stannous chloride is dissolved in 10ml ethylene glycol) and 1.6ml thioacetamide
Solution (0.3g thioacetamide is dissolved in 10ml ethylene glycol) is added in b solution, is transferred to 50ml polytetrafluoroethylene (PTFE) after stirring 20min
In the stainless steel cauldron of liner, 160 DEG C of incubation water heating 12h;
(4) be collected, be collected by centrifugation with dehydrated alcohol after cooling, 5 times repeatedly, then by gained precipitating with 20ml without
Water-ethanol is transferred in beaker, and 3ml concentrated ammonia liquor is added, and its object is to remove molybdenum oxide template, is stirred 90min, is then used nothing
Water-ethanol is collected by centrifugation, and 5 times repeatedly, gained is deposited in 45 DEG C of dry 12h;
(5) by gained SnS2It is put into tube furnace, is calcined under 400 DEG C of air atmospheres for 24 hours, 5 DEG C/min of heating rate.
Embodiment 2
(1) 0.5gPVP (MW.58000) is added in 25ml ethylene glycol and stirs 30min, and ultrasound 10min is clear to solution
Clearly;
(2) 20mg molybdenum oxide nano rod is added in a solution, stirring 1h to molybdenum oxide is evenly dispersed in a solution;
(3) by 1.6ml stannous chloride solution (0.758g stannous chloride is dissolved in 10ml ethylene glycol) and 1.6ml thioacetamide
Solution (0.3g thioacetamide is dissolved in 10ml ethylene glycol) is added in b solution, is transferred to 50ml polytetrafluoroethylene (PTFE) after stirring 20min
In the stainless steel cauldron of liner, incubation water heating 12h;
(4) be collected, be collected by centrifugation with dehydrated alcohol after cooling, 5 times repeatedly, then by gained precipitating with 20ml without
Water-ethanol is transferred in beaker, and 3ml concentrated ammonia liquor is added, and is stirred 90min its object is to remove molybdenum oxide template and is then used nothing
Water-ethanol is collected by centrifugation, and cleans 5 times repeatedly, gained is deposited in 45 DEG C of dry 10h;
(5) by gained SnS2It is put into tube furnace, is calcined under 400 DEG C of air atmospheres for 24 hours, 5 DEG C/min of heating rate.
Embodiment 3
A kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, comprising the following steps:
(1) 0.45gPVP (MW.58000) is added in 45ml ethylene glycol and stirs 30min, and ultrasound 10min is clear to solution
Clearly, a solution is obtained;
(2) 24mg molybdenum oxide nano rod being added in a solution, stirring 1h to molybdenum oxide is evenly dispersed in a solution,
Obtain b solution;
(3) by 2.18ml stannous chloride solution (0.5g stannous chloride is dissolved in 10ml ethylene glycol) and 2.62ml thioacetamide
Solution (0.5g thioacetamide is dissolved in 10ml ethylene glycol) is added in b solution, is transferred to 50ml polytetrafluoroethylene (PTFE) after stirring 20min
In the stainless steel cauldron of liner, 150 DEG C of incubation water heating 14h;
(4) be collected, be collected by centrifugation with dehydrated alcohol after cooling, 3 times repeatedly, then by gained precipitating with 20ml without
Water-ethanol is transferred in beaker, and 3ml concentrated ammonia liquor is added, and its object is to remove molybdenum oxide template, is stirred 90min, is then used nothing
Water-ethanol is collected by centrifugation, and cleans 6 times repeatedly, gained is deposited in 40 DEG C of dry 14h;
(5) by gained SnS2It is put into tube furnace, 26h, 5 DEG C/min of heating rate is calcined under 380 DEG C of air atmospheres.
Embodiment 4
A kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, comprising the following steps:
(1) 0.45gPVP (MW.58000) is added in 20ml ethylene glycol and stirs 30min, and ultrasound 10min is clear to solution
Clearly, a solution is obtained;
(2) 31.5mg molybdenum oxide nano rod is added in a solution, stirring 1h to molybdenum oxide is evenly dispersed in a solution
In, obtain b solution;
(3) by 1.89ml stannous chloride solution (0.9g stannous chloride is dissolved in 10ml ethylene glycol) and 1.89ml thioacetamide
Solution (0.1g thioacetamide is dissolved in 10ml ethylene glycol) is added in b solution, is transferred to 50ml polytetrafluoroethylene (PTFE) after stirring 20min
In the stainless steel cauldron of liner, 170 DEG C of incubation water heating 8h;
(4) be collected, be collected by centrifugation with dehydrated alcohol after cooling, 3 times repeatedly, then by gained precipitating with 20ml without
Water-ethanol is transferred in beaker, and 3ml concentrated ammonia liquor is added, and its object is to remove molybdenum oxide template, is stirred 90min, is then used nothing
Water-ethanol is collected by centrifugation, and cleans 6 times repeatedly, gained is deposited in 50 DEG C of dry 8h;
(5) by gained SnS2It is put into tube furnace, 20h, 5 DEG C/min of heating rate is calcined under 420 DEG C of air atmospheres.
By multistage SnO prepared by embodiment 1 and embodiment 22The gas sensitive of nanotube superstructure executes Flied emission electricity
Sub- flying-spot microscope (FE-SEM) experiment, can be obtained electromicroscopic photograph as shown in Figure 1 and Figure 2, the SnO of hollow tubular2Surface is grown
Countless nanometer sheets, these nanometer sheets are for example flower-shaped to be evenly distributed on SnO2Surface greatly increases the specific surface area of nanotube, mentions
The high sensitivity for changing material.Fig. 3, Fig. 4 are respectively the multistage SnO of embodiment 1, the preparation of embodiment 22The gas of nanotube superstructure
Quick material, it is observed that SnO in figure2The thickness of nanometer sheet is about 4nm, is largely stacked towards different directions into hollow tubular
Structure.By XRD diagram (a) diffraction maximum of Fig. 5 it is found that SnS2Most of diffraction maximum of hollow pipe presoma all with SnS2Phase (JCPDS
No.23-0677) corresponding, but have an apparent Sn in 12.605 degree of corresponding (020) faces of 2 θ2S3Phase (JCPDS
No.14-0619 diffraction maximum) illustrates that there are micro Sn in presoma2S3;And scheming (b) then is the SnO of pure tetragonal phase2
(JCPDS No.41-1445), compared with the diffraction maximum shown in the figure (a), diffracted intensity is bigger, after this illustrates annealing
SnO2Crystallinity is higher, and crystallite dimension is larger, and presoma has been completely reformed into SnO2, and free from admixture generates.
SnO2As a kind of semiconductor (Eg=3.62eV) of N-shaped broad-band gap, small, large specific surface area the spy with partial size
Point, small-size effect, surface and interface effect, macro quanta tunnel effect etc. are more significant, therefore can be widely applied to gas
The scientific researches such as dependent sensor, resistor, transparent heating element, catalyst and solar battery and industrial application.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of multistage SnO2The preparation method of nanotube-shaped gas sensitive, it is characterised in that: the following steps are included:
(1) PVP is added in ethylene glycol and is stirred, then ultrasound to solution is clarified, and obtains a solution;
(2) molybdenum oxide nano rod is added in a solution, stirring is dispersed in a solution to molybdenum oxide, obtains b solution;
(3) stannous chloride solution and thioacetyl amine aqueous solution are added in b solution, are transferred in reaction kettle after stirring, constant temperature
Hydro-thermal 10-14h;
(4) it is collected by centrifugation after cooling with dehydrated alcohol, 3-6 times repeatedly, gained precipitating is then transferred to burning with dehydrated alcohol
In cup, ammonium hydroxide is added, stirs 1-2h, then be collected by centrifugation with dehydrated alcohol, cleans 3-6 times, and gained is precipitated into drying, obtains repeatedly
To SnS2;
(5) by gained SnS2Be put into tube furnace under air atmosphere calcine to get.
2. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: the PVP
Solid-to-liquid ratio with ethylene glycol is 1:45-100.
3. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: the oxygen
The additive amount for changing molybdenum is the 0.05-0.15% of a solution weight.
4. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: the oxygen
The mass ratio for changing stannous solution and the thioacetyl amine aqueous solution is 1:1-1.2;The stannous chloride solution and thioacetamide
The total weight of solution is the 10-18% of b solution weight.
5. multistage SnO according to claim 42The preparation method of nanotube-shaped gas sensitive, it is characterised in that: the oxygen
Changing stannous solution is that 0.5-0.9g stannous chloride is dissolved in 10mL ethylene glycol;The thioacetyl amine aqueous solution is by 0.1-0.5g
Thioacetamide is dissolved in 10mL ethylene glycol.
6. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: in step
(3), the reaction kettle is the stainless steel cauldron of 50mL polytetrafluoroethyllining lining, and the temperature of the incubation water heating is 150-170
℃。
7. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: in step
(4), the temperature of the drying is 40-50 DEG C, time 8-14h.
8. multistage SnO according to claim 12The preparation method of nanotube-shaped gas sensitive, it is characterised in that: in step
(5), the temperature of the calcining is 380-420 DEG C, calcination time 20-26h, and heating rate is 5 DEG C/min.
9. a kind of multistage SnO being prepared such as any one of claim 1-82Nanotube-shaped gas sensitive is in transparent conductive film, biography
The application of sensor, catalyst and catalyst carrier material.
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CN110165228A (en) * | 2019-05-23 | 2019-08-23 | 北京科技大学 | From hydrophobic integrated ordered catalyst layer-diffusion layer electrode structure and preparation method |
CN110396700A (en) * | 2019-07-26 | 2019-11-01 | 中国科学院青岛生物能源与过程研究所 | A kind of tin oxide catalysts are in electrochemical reduction CO2Application in formic acid processed |
CN110396701A (en) * | 2019-08-19 | 2019-11-01 | 青岛科技大学 | A kind of efficient electro-catalysis reduction carbon dioxide prepares catalyst of formic acid and preparation method thereof |
CN111446374A (en) * | 2020-03-09 | 2020-07-24 | 浙江师范大学 | Perovskite solar cell and preparation method thereof |
CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
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CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
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