CN107315036A - One kind is based on SnO2The alcohol gas sensor of composite nano fiber - Google Patents
One kind is based on SnO2The alcohol gas sensor of composite nano fiber Download PDFInfo
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- 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
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Abstract
SnO is based on the present invention relates to one kind2The alcohol gas sensor of composite nano fiber, the gas sensor is heater-type structure, wherein, sensitive material is SnO prepared by method of electrostatic spinning2Composite nano fiber, the SnO2Composite nano fiber includes SnO2Porous hollow sphere, ZnO nano-wire；Or, the SnO2Porous hollow sphere is doped with WO3。
Description
Technical field
SnO is based on the present invention relates to sensor technical field, more particularly to one kind2The alcohol gas of composite nano fiber are passed
Sensor.
Background technology
In recent years due to the development of science and technology, the continuous improvement of modern industrialization degree, the gas used in process of production
And species, the quantity of the gas generated in process of production are also increasing, wherein, many gases are inflammable and explosive, or
Many gases are toxic gases, for the sake of security, and just gas must be strengthened in terms of use, transport, storage to monitor, because
This, in sensor, gas sensor application field extensively, has a extensive future.
Sensor is typically to be made up of sensing element, conversion element and measuring circuit.Wherein, sensing element be can be direct
Impression is measured and is converted into the element of the electricity or the variable physical quantity into electricity that have determination relation with being measured.
Wherein, sensing element/material is the core of sensor production, while being also sensor design, optimization and business
Basis, sensitive material species is various, wherein, semi-conducting material is current most widely used sensitive material, with nano science
The rise of technology, nano material turns into study hotspot in the application of sensor field.
The content of the invention
The present invention is intended to provide a kind of be based on SnO2The alcohol gas sensor of composite nano fiber, it is set forth above to solve
Problem.
Provided in embodiments of the invention a kind of based on SnO2The alcohol gas sensor of composite nano fiber, the gas
Sensor is heater-type structure, including：The aluminium oxide ceramics of 2 parallel and discrete annular gold electrodes is come with by outer surface
Manage, be coated in and connect on the sensitive material of ceramic pipe surface, the nichrome heating coil composition through earthenware, each gold electrode
It is connected to two platinum filament pins；The sensitive material is SnO prepared by method of electrostatic spinning2Composite nano fiber, the SnO2Composite Nano
Fiber includes SnO2Porous hollow sphere, ZnO nano-wire.
Preferably, the SnO that the sensitive material includes2Porous hollow sphere is doped with WO3, WO3With SnO2Mass ratio is 1:
67。
The technical scheme that embodiments of the invention are provided can include the following benefits：
Sensor of the invention is heater-type structure, and its sensitive material is SnO prepared by method of electrostatic spinning2Composite Nano is fine
Dimension, the SnO2Composite nano fiber includes SnO2Porous hollow sphere, ZnO nano-wire；In technical solution of the present invention, by SnO2It is many
Hole hollow ball, ZnO nano-wire have been prepared by mixing into SnO2Composite nano fiber, thus has spirit as the sensor of sensitive material
Quick property is high, respond rapid advantage.
The additional aspect of the present invention and advantage will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.It should be appreciated that the general description of the above and detailed description hereinafter are only
It is exemplary and explanatory, the present invention can not be limited.
Brief description of the drawings
Using accompanying drawing, the invention will be further described, but the embodiment in accompanying drawing does not constitute any limit to the present invention
System, for one of ordinary skill in the art, on the premise of not paying creative work, can also be obtained according to the following drawings
Other accompanying drawings.
Fig. 1 is the structural representation of alcohol gas sensor of the present invention,
Wherein, the annular gold electrodes of 21-, 22- alumina ceramic tubes, 23- sensitive materials, 24- nichrome heating coils,
25- platinum filaments.
Embodiment
Here exemplary embodiment will be illustrated in detail, its example is illustrated in the accompanying drawings.Following description is related to
During accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represent same or analogous key element.Following exemplary embodiment
Described in embodiment do not represent and the consistent all embodiments of the present invention.On the contrary, they be only with it is such as appended
The example of the consistent apparatus and method of some aspects be described in detail in claims, the present invention.
Technical scheme is related to a kind of based on SnO2The alcohol gas sensor of composite nano fiber, with reference to Fig. 1,
The gas sensor is heater-type structure, including：The oxidation of 2 parallel and discrete annular gold electrodes 21 is come with by outer surface
Aluminium earthenware 22, the sensitive material 23 for being coated in the surface of earthenware 22,24 groups of the nichrome heating coil through earthenware 22
Into being connected with two pins of platinum filament 25 on each gold electrode 21.
Above-mentioned sensitive material 23 is SnO prepared by method of electrostatic spinning2Composite nano fiber, including SnO2Porous air
Bulbus cordis, ZnO nano-wire.
Electrostatic spinning is a kind of short-cut method for preparing nano material, and the monodimension nanometer material prepared by electrostatic spinning is being received
The fields such as electronic device, catalyst, sensor have practical application.Particularly, in sensor field, prepared by Electrospinning
Sensitive material, with big specific surface area and fiber possesses microcellular structure, these features beneficial to it all with being used as sensitive material
For the response of gas.
And specific to SnO2In base gas sensor, current technical scheme, SnO is prepared using method of electrostatic spinning2Composite Nano
Fiber is few as the technical scheme of sensitive material；In technical solution of the present invention, by SnO2Porous hollow sphere, ZnO nano-wire are mixed
Conjunction has been prepared into SnO2Composite nano fiber, thus has sensitivity height, response rapidly excellent as the sensor of sensitive material
Point.
Above-mentioned sensitive material includes SnO2Porous hollow sphere, the SnO2Porous hollow sphere be by template of carbon paste ball, water
Prepared by hot method, the SnO2The particle diameter of porous hollow sphere is 200nm, and it is the porous crust knot being made up of a large amount of nano particles
Structure.
SnO2It is a kind of n-type semiconductor material with wide forbidden band, with unique optics, catalysis, electric property, it is in sensing
The fields such as device, solar cell, lithium battery, catalyst and transparent conductive electrode have extensive use；It is that one kind is opened earliest
The metal oxide gas sensitive material of hair, SnO2Because having the advantages that cost is low, stability is good, sensitivity is high and is closed
Note, with the development of nanometer technology, to the SnO of various nanostructureds2Investigation of materials increases.In the present invention, hydro-thermal legal system is utilized
Standby carbon paste ball has hydrophily, and surface has-OH and C-O functional groups, and the presence of these functional groups is easy to metal ion
Closed with carbon paste chou, the hydroxide for forming metal is simultaneously distributed its surface, then, by high-temperature calcination, the carbon in carbon paste ball is former
Son is oxidized to be discharged in the form of carbon dioxide, so that form metallic oxide hollow sphere, i.e. SnO2Porous hollow sphere, its is porous
Shell structurre is conducive to the absorption to gas, adds the sensitivity of sensitive material.
Above-mentioned sensitive material includes ZnO nano-wire, and the ZnO nano-wire length is 500nm, a diameter of 20~50nm.
ZnO unique properties in terms of optics, electricity, catalysis, in the neck such as sensor, solar cell, lithium battery, catalysis
Domain is suffered from practical application, technical solution of the present invention, by above-mentioned SnO2Porous hollow sphere and ZnO nano-wire are combined, and are used
Method of electrostatic spinning prepares composite nano fiber, in the fiber, and the ZnO nano-wire is to discrete SnO2Porous hollow sphere plays company
Effect is connect, the conductive path of carrier can be formed, simultaneously because ZnO is equally n-type semiconductor material with wide forbidden band, both forbidden bands
Similar width, substantially increases the electrical conductivity of composite nano fiber so that the response time of sensor reduces.
Then by above-mentioned SnO2After porous hollow sphere, ZnO nano-wire are mixed in proportion, poly-vinyl alcohol solution is added to
In, spinning solution is obtained, electrostatic spinning is carried out, obtains composite cellulosic membrane, is calcined after removal polyvinyl alcohol, compound receive is obtained
Rice fiber.
Preferably, in above-mentioned spinning solution, polyvinyl alcohol mass percent is 9wt.%.
Preferably, in above-mentioned composite nano fiber, SnO2Porous hollow sphere, the mass ratio of ZnO nano-wire are 4:1.
In another preferred embodiment, the SnO that above-mentioned sensitive material includes2Porous hollow sphere is doped with WO3, its
In, WO3With SnO2Mass ratio is 1:67.
As described above, the current SnO to various nanostructureds2Investigation of materials increases, and the research of the material is mainly logical
Cross various means and improve sensor performance aspect, the metal or metal oxide of doping mainly have Zn, Pt, CuO, ZnO etc., and mix
Miscellaneous WO3Technical scheme it is few；In the present invention, by doping, WO is prepared for3The SnO of doping2Porous hollow sphere, the doping
WO3Acted synergistically with ZnO nano-wire, positive role is played in sensitivity and response time to sensor.
In order to obtain above-mentioned sensitive material, the invention further relates to the SnO2The preparation process of composite nano fiber：
Step 1, hydro-thermal method prepare carbon paste ball
9g glucose is added in 50ml deionized waters and stirred, is then moved into solution in water heating kettle, in drying
8h is heated under 180 DEG C of constant temperature of case, after reaction terminates, room temperature is naturally cooled to, is centrifuged, washed with alcohol and deionized water successively
Wash, after repeated washing three times, obtain dark brown product carbon paste ball, it is standby in 60 DEG C of dry 12h；
Step 2, preparation WO3Adulterate SnO2Porous hollow sphere
3.82mmol wolframic acid and stannic chloride are added to 60ml ethanol and stirred in the mixed liquor of 8ml water, is formed
Solution A, 35mmol urea is then added into solution A, stirs to form solution B, by the 32mmol carbon paste balls of above-mentioned preparation
Solution B is added, resulting solution is stood 30h by ultrasonic disperse 2h, centrifuged, washing, in 80 DEG C of dry 12h, finally by drying
Product afterwards dries 2h at 580 DEG C, obtains WO3Adulterate SnO2Porous hollow sphere；
Step 3, prepare spinning solution
Take 0.8g polyvinyl alcohol to be put into the conical flask equipped with 10g distilled water, be stirred continuously, be allowed in the case where being incubated 90 DEG C
Fully dissolved, naturally cools to room temperature；Then ZnO nano-wire and WO obtained above are added3Adulterate SnO2Porous hollow sphere, continues
6h is stirred, spinning solution is obtained；
Step 4, electrostatic spinning
Above-mentioned spinning solution is fitted into spinneret pipe, insert a 10cm copper wire as positive pole, aluminium foil as receiver board,
For negative pole, institute's making alive is 17kV during electrostatic spinning, and distance is 18cm between spinning head and receiver board, carries out electrostatic spinning, obtains
To WO3Adulterate SnO2Porous hollow sphere/ZnO nano-wire/polyvinyl alcohol composite fiber film；
Step 5, calcining
Above-mentioned composite cellulosic membrane is made annealing treatment into 5h at 700 DEG C, to remove high-molecular polyivnyl alcohol, SnO is obtained2It is compound
Nanofiber.
Then, by above-mentioned SnO2Composite nano fiber is configured to after slurry, is coated in ceramic pipe surface, is prepared after electrode,
Produce of the present invention a kind of based on SnO2The alcohol gas sensor of composite nano fiber.
Embodiment 1
In the present embodiment, the sensitive material is SnO prepared by method of electrostatic spinning2Composite nano fiber, including SnO2It is many
Hole hollow ball, ZnO nano-wire.
The SnO2The preparation process of composite nano fiber：
Step 1, hydro-thermal method prepare carbon paste ball
9g glucose is added in 50ml deionized waters and stirred, is then moved into solution in water heating kettle, in drying
8h is heated under 180 DEG C of constant temperature of case, after reaction terminates, room temperature is naturally cooled to, is centrifuged, washed with alcohol and deionized water successively
Wash, after repeated washing three times, obtain dark brown product carbon paste ball, it is standby in 60 DEG C of dry 12h；
Step 2, preparation SnO2Porous hollow sphere
3.82mmol stannic chlorides are added to 60ml ethanol and stirred in the mixed liquor of 8ml water, solution A are formed, so
35mmol urea is added in backward solution A, stirs to form solution B, the 32mmol carbon pastes ball of above-mentioned preparation is added into solution
B, ultrasonic disperse 2h, 30h is stood by resulting solution, is centrifuged, washing, in 80 DEG C of dry 12h, finally by dried product
2h is dried at 580 DEG C, SnO is obtained2Porous hollow sphere；
Step 3, prepare spinning solution
Take 0.8g polyvinyl alcohol to be put into the conical flask equipped with 10g distilled water, be stirred continuously, be allowed in the case where being incubated 90 DEG C
Fully dissolved, naturally cools to room temperature；Then ZnO nano-wire and SnO obtained above are added2Porous hollow sphere, continues to stir 6h,
Obtain spinning solution；
Step 4, electrostatic spinning
Above-mentioned spinning solution is fitted into spinneret pipe, insert a 10cm copper wire as positive pole, aluminium foil as receiver board,
For negative pole, institute's making alive is 17kV during electrostatic spinning, and distance is 18cm between spinning head and receiver board, carries out electrostatic spinning, obtains
To SnO2Porous hollow sphere/ZnO nano-wire/polyvinyl alcohol composite fiber film；
Step 5, calcining
Above-mentioned composite cellulosic membrane is made annealing treatment into 5h at 700 DEG C, to remove high-molecular polyivnyl alcohol, SnO is obtained2It is compound
Nanofiber.
Flow through the electric current of heating coil to regulate and control the operating temperature of sensor by change, be in not by measurement sensor
Resistance value during with gas between two gold electrodes can obtain the sensitivity of sensor.Spirit of the sensor for alcohol gas
Sensitivity S is defined as：S=Rg/Ra, wherein Rg and Ra be respectively sensor in alcohol gas and air when two gold electrodes between electricity
Resistance, it is found that the sensitivity of the sensor of this in the present embodiment is 6.3.
Embodiment 2
In the present embodiment, the sensitive material is SnO prepared by method of electrostatic spinning2Composite nano fiber, including WO3Mix
Miscellaneous SnO2Porous hollow sphere, ZnO nano-wire.
The SnO2The preparation process of composite nano fiber：
Step 1, hydro-thermal method prepare carbon paste ball
9g glucose is added in 50ml deionized waters and stirred, is then moved into solution in water heating kettle, in drying
8h is heated under 180 DEG C of constant temperature of case, after reaction terminates, room temperature is naturally cooled to, is centrifuged, washed with alcohol and deionized water successively
Wash, after repeated washing three times, obtain dark brown product carbon paste ball, it is standby in 60 DEG C of dry 12h；
Step 2, preparation WO3Adulterate SnO2Porous hollow sphere
3.82mmol wolframic acid and stannic chloride are added to 60ml ethanol and stirred in the mixed liquor of 8ml water, is formed
Solution A, 35mmol urea is then added into solution A, stirs to form solution B, by the 32mmol carbon paste balls of above-mentioned preparation
Solution B is added, resulting solution is stood 30h by ultrasonic disperse 2h, centrifuged, washing, in 80 DEG C of dry 12h, finally by drying
Product afterwards dries 2h at 580 DEG C, obtains WO3Adulterate SnO2Porous hollow sphere；
Step 3, prepare spinning solution
Take 0.8g polyvinyl alcohol to be put into the conical flask equipped with 10g distilled water, be stirred continuously, be allowed in the case where being incubated 90 DEG C
Fully dissolved, naturally cools to room temperature；Then ZnO nano-wire and WO obtained above are added3Adulterate SnO2Porous hollow sphere, continues
6h is stirred, spinning solution is obtained；
Step 4, electrostatic spinning
Above-mentioned spinning solution is fitted into spinneret pipe, insert a 10cm copper wire as positive pole, aluminium foil as receiver board,
For negative pole, institute's making alive is 17kV during electrostatic spinning, and distance is 18cm between spinning head and receiver board, carries out electrostatic spinning, obtains
To WO3Adulterate SnO2Porous hollow sphere/ZnO nano-wire/polyvinyl alcohol composite fiber film；
Step 5, calcining
Above-mentioned composite cellulosic membrane is made annealing treatment into 5h at 700 DEG C, to remove high-molecular polyivnyl alcohol, SnO is obtained2It is compound
Nanofiber.
Flow through the electric current of heating coil to regulate and control the operating temperature of sensor by change, be in not by measurement sensor
Resistance value during with gas between two gold electrodes can obtain the sensitivity of sensor.Spirit of the sensor for alcohol gas
Sensitivity S is defined as：S=Rg/Ra, wherein Rg and Ra be respectively sensor in alcohol gas and air when two gold electrodes between electricity
Resistance, it is found that the sensitivity of the sensor of this in the present embodiment is 9.7.
The preferred mode of the present invention is the foregoing is only, is not intended to limit the invention, all spiritual and originals in the present invention
Within then, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (8)
1. one kind is based on SnO2The alcohol gas sensor of composite nano fiber, the gas sensor is heater-type structure, including：
The alumina ceramic tube of 2 parallel and discrete annular gold electrodes is come with by outer surface, the sensitivity of ceramic pipe surface is coated in
Material, the nichrome heating coil through earthenware are constituted, and two platinum filament pins are connected with each gold electrode；Its feature exists
In the sensitive material is SnO prepared by method of electrostatic spinning2Composite nano fiber, the SnO2Composite nano fiber includes SnO2
Porous hollow sphere, ZnO nano-wire.
2. it is according to claim 1 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO2The preparation process of composite nano fiber is：By SnO2After porous hollow sphere, ZnO nano-wire are mixed in proportion, it is added to
In poly-vinyl alcohol solution, spinning solution is obtained, electrostatic spinning is carried out, obtains composite cellulosic membrane, removal polyvinyl alcohol is calcined
Afterwards, the SnO is obtained2Composite nano fiber.
3. it is according to claim 2 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
In above-mentioned spinning solution, polyvinyl alcohol mass percent is 9wt.%.
4. it is according to claim 3 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO2In composite nano fiber, SnO2Porous hollow sphere, the mass ratio of ZnO nano-wire are 4:1.
5. it is according to claim 2 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO2Porous hollow sphere be by template of carbon paste ball, hydro-thermal method prepare, the SnO2The particle diameter of porous hollow sphere is 200nm, its
It is the porous crust structure being made up of a large amount of nano particles；The ZnO nano-wire length is 500nm, a diameter of 20~50nm.
6. it is according to claim 2 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO2The preparation process of composite nano fiber：
Step 1, hydro-thermal method prepare carbon paste ball
9g glucose is added in 50ml deionized waters and stirred, is then moved into solution in water heating kettle, in drying box 180
8h is heated under DEG C constant temperature, after reaction terminates, room temperature is naturally cooled to, is centrifuged successively with alcohol and deionized water, washing, weight
After backwashing is washed after three times, obtains dark brown product carbon paste ball, and it is standby in 60 DEG C of dry 12h；
Step 2, preparation SnO2Porous hollow sphere
3.82mmol stannic chlorides are added to 60ml ethanol and stirred in the mixed liquor of 8ml water, solution A, Ran Houxiang is formed
35mmol urea is added in solution A, stirs to form solution B, the 32mmol carbon pastes ball of above-mentioned preparation is added into solution B, is surpassed
Sound disperses 2h, and resulting solution is stood into 30h, centrifuges, and washing, in 80 DEG C of dry 12h, finally exists dried product
2h is dried at 580 DEG C, SnO is obtained2Porous hollow sphere；
Step 3, prepare spinning solution
Take 0.8g polyvinyl alcohol to be put into the conical flask equipped with 10g distilled water, be stirred continuously in the case where being incubated 90 DEG C, be allowed to completely molten
Solution, naturally cools to room temperature；Then ZnO nano-wire and SnO obtained above are added2Porous hollow sphere, continues to stir 6h, obtains
Spinning solution；
Step 4, electrostatic spinning
Above-mentioned spinning solution is fitted into spinneret pipe, 10cm copper wire is inserted as positive pole, aluminium foil, as receiver board, is negative
Pole, institute's making alive is 17kV during electrostatic spinning, and distance is 18cm between spinning head and receiver board, carries out electrostatic spinning, obtains
SnO2Porous hollow sphere/ZnO nano-wire/polyvinyl alcohol composite fiber film；
Step 5, calcining
Above-mentioned composite cellulosic membrane is made annealing treatment into 5h at 700 DEG C, to remove high-molecular polyivnyl alcohol, SnO is obtained2Composite Nano
Fiber.
7. it is according to claim 2 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO that the sensitive material includes2Porous hollow sphere is doped with WO3, WO3With SnO2Mass ratio is 1:67.
8. it is according to claim 7 a kind of based on SnO2The alcohol gas sensor of composite nano fiber, it is characterised in that
The SnO2The preparation process of composite nano fiber：
Step 1, hydro-thermal method prepare carbon paste ball
9g glucose is added in 50ml deionized waters and stirred, is then moved into solution in water heating kettle, in drying box 180
8h is heated under DEG C constant temperature, after reaction terminates, room temperature is naturally cooled to, is centrifuged successively with alcohol and deionized water, washing, weight
After backwashing is washed after three times, obtains dark brown product carbon paste ball, and it is standby in 60 DEG C of dry 12h；
Step 2, preparation WO3Adulterate SnO2Porous hollow sphere
3.82mmol wolframic acid and stannic chloride are added to 60ml ethanol and stirred in the mixed liquor of 8ml water, solution is formed
A, 35mmol urea is then added into solution A, stirs to form solution B, and the 32mmol carbon pastes ball of above-mentioned preparation is added
Resulting solution is stood 30h by solution B, ultrasonic disperse 2h, is centrifuged, and washing, finally will be dried in 80 DEG C of dry 12h
Product dries 2h at 580 DEG C, obtains WO3Adulterate SnO2Porous hollow sphere；
Step 3, prepare spinning solution
Take 0.8g polyvinyl alcohol to be put into the conical flask equipped with 10g distilled water, be stirred continuously in the case where being incubated 90 DEG C, be allowed to completely molten
Solution, naturally cools to room temperature；Then ZnO nano-wire and WO obtained above are added3Adulterate SnO2Porous hollow sphere, continues to stir
6h, obtains spinning solution；
Step 4, electrostatic spinning
Above-mentioned spinning solution is fitted into spinneret pipe, 10cm copper wire is inserted as positive pole, aluminium foil, as receiver board, is negative
Pole, institute's making alive is 17kV during electrostatic spinning, and distance is 18cm between spinning head and receiver board, carries out electrostatic spinning, obtains WO3
Adulterate SnO2Porous hollow sphere/ZnO nano-wire/polyvinyl alcohol composite fiber film；
Step 5, calcining
Above-mentioned composite cellulosic membrane is made annealing treatment into 5h at 700 DEG C, to remove high-molecular polyivnyl alcohol, SnO is obtained2Composite Nano
Fiber.
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