CN107367528A - A kind of alcohol gas sensor based on ZnO composite fibres - Google Patents
A kind of alcohol gas sensor based on ZnO composite fibres Download PDFInfo
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- CN107367528A CN107367528A CN201710634391.6A CN201710634391A CN107367528A CN 107367528 A CN107367528 A CN 107367528A CN 201710634391 A CN201710634391 A CN 201710634391A CN 107367528 A CN107367528 A CN 107367528A
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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Abstract
The present invention relates to a kind of alcohol gas sensor based on ZnO composite fibres, the alumina ceramic tube, the sensitive material coated in ceramic pipe surface, the nichrome heating coil through earthenware that the gas sensor is come with 2 parallel and discrete annular gold electrodes by outer surface are formed, and two platinum filament pins are connected with each gold electrode；The sensitive material is ZnO composite nano fibers prepared by method of electrostatic spinning, and the ZnO composite nano-fiber materials are specially ZnO microsphere doping metals nano wire and Al.
Description
Technical field
The present invention relates to gas sensor domain, more particularly to a kind of alcohol gas sensor based on ZnO composite fibres.
Background technology
Sensor has become core skill as the main path and means that obtain various information in nature and production field
Art and equipment.Definition of the standard GB/T 7665-87 to sensor be：It is measured and according to certain rule as defined in can experiencing
Rule is converted to the device or device of usable output signal.
In recent years, due to being controlled in industrial discharge, environment measuring, the extensive use in the field such as traffic safety and medical diagnosis on disease,
Concern of the people for alcohol gas sensor is more and more.In numerous gas sensors, partly led using metal oxide
Body as sensitive material resistor-type gas sensor due to being mesh with low cost, high sensitivity and simple operation and other advantages
One of preceding most widely used gas sensor.Metal-oxide gas transducer is exposed to test gas using sensitive material
It is measured different from concentration with test gaseous species when middle and produces prepared by the principle of change.Therefore, sensitive material, device
Structure and performance are the main researchs of metal-oxide gas transducer.
At present, people employ various methods to improve the air-sensitive of MOS type gas sensor
Characteristic, including construct the nanostructured of complex multi-dimensional, supported precious metal catalyst, form nano-complex, aliovalent doping etc..
The content of the invention
The present invention is intended to provide a kind of alcohol gas sensor based on ZnO composite fibres, to solve problem set forth above.
Technical scheme provides a kind of alcohol gas sensor based on ZnO composite fibres, the gas sensing
Device is come with the alumina ceramic tube of 2 parallel and discrete annular gold electrodes by outer surface, coated in the quick of ceramic pipe surface
Feel material, the nichrome heating coil composition through earthenware, two platinum filament pins are connected with each gold electrode；Its feature
It is, the sensitive material is ZnO composite nano fibers prepared by method of electrostatic spinning, and the ZnO composite nano-fiber materials are specific
For ZnO microsphere doping metals nano wire and Al.
Technical scheme provided by the invention can include the following benefits：
1. in the present invention, the composite nano fiber based on zinc oxide is prepared for using method of electrostatic spinning, the composite Nano is fine
Dimension has big specific surface area, and fiber has microcellular structure, improves the sensitivity decrease response time of sensor, effectively
Improve the performance of sensor.
2. in the ZnO composite nano fibers, doped with Al, first, the introducing of Al ions inhibits the growth of ZnO microsphere,
Its Microsphere Size is significantly reduced, on the other hand, the position of the Zn ions in Al ionic compartmentations ZnO crystal, as compensation,
A certain amount of free electron is generated, so as to reduce the hole of material, in addition, the doping of Al ions changes
The distribution of oxygen component in material so that the quantity of defect oxygen and chemical absorption of surface oxygen is significantly greatly increased in material, above-mentioned
Aspect collective effect, the sensitivity of sensor greatly improved.
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 and following detailed description of the above 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 form 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 gas sensor of the present invention；
Wherein, 21- annulars gold electrode, 22- alumina ceramic tubes, 23- sensitive materials, 24- evanohm heating coils, 25-
Platinum filament.
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 being described in detail in claims, of the invention.
Technical scheme is related to a kind of alcohol gas sensor based on ZnO composite fibres, described with reference to Fig. 1
Sensor is heater-type structure, by outer surface come with 2 parallel and discrete annular gold electrodes 21 alumina ceramic tube 22,
Sensitive material 23 coated in the surface of earthenware 22, the nichrome heating coil 24 through earthenware 22 form, each gold electricity
Two pins of platinum filament 25 are connected with pole 21；The sensitive material 23 is ZnO composite nano fibers prepared by method of electrostatic spinning, thick
Spend for 0.2~0.5mm, and, the ZnO composite nano-fiber materials are specially ZnO microsphere doping metals nano wire and Al.
ZnO is the n-type semiconductor material with wide forbidden band for having wurtzite structure, and it is in optics, electricity, catalysis etc. performance
Uniqueness, practical application is suffered from fields such as sensor, solar cell, lithium battery, catalysis.Particularly in gas sensor side
Face.At present, the research to zno-based gas sensor mainly takes the mode such as nanostructured control, doping, compound raising property
Energy；Meanwhile electrostatic spinning is a kind of short-cut method for preparing nano material, and the technology on zinc oxide gas sensor at present
In scheme, it is few as the technical scheme of sensitive material that zinc oxide composite fibre is prepared using method of electrostatic spinning；In the present invention, adopt
The composite nano fiber based on zinc oxide is prepared for method of electrostatic spinning, the composite nano fiber has big specific surface area, and
Fiber has microcellular structure, improves the sensitivity decrease response time of sensor, effectively increases the performance of sensor.
In technical scheme, a diameter of 300nm of ZnO composite nano fibers.
A kind of preferred embodiment is that the mass content of metal nanometer line is 6~9% in the ZnO composite nano fibers,
The metal nanometer line is preferably Ag nano wires, and the Ag nanowire lengths are 200nm, a diameter of 50nm.
ZnO composite nano fibers in the technical program, ZnO is compound with metal nanometer line.In the prior art scheme,
As described above, on zno-based gas sensitive, the electric conductivity of gas sensitive, catalytic are improved typically by doping particle etc.,
And the technical scheme for adulterating metal nanometer line is few.In technical solution of the present invention, pass through the metal nanometer line of doping so that
The metal nanometer line is parallel between each other, and the metal nanometer line can provide conductive path for sensitive material, while improve quick
Feel the intensity and toughness of material.
A kind of preferred embodiment is that Al mass content is 5~7% in the ZnO composite nano fibers.
In the ZnO composite nano fibers, doped with Al, first, the introducing of Al ions inhibits the growth of ZnO microsphere, makes
Its Microsphere Size significantly reduces, on the other hand, the position of the Zn ions in Al ionic compartmentations ZnO crystal, as compensation, production
A certain amount of free electron is given birth to, so as to reduce the hole of material, in addition, the doping of Al ions changes material
The distribution of oxygen component in material so that the quantity of defect oxygen and chemical absorption of surface oxygen is significantly greatly increased in material, above-mentioned side
Face collective effect, the sensitivity of sensor greatly improved.
Technical solution of the present invention further relates to the preparation process of above-mentioned ZnO composite nano fibers：
Step 1, take 5mmol zinc acetates and 10mmol urea to be dissolved in 40ml deionized water, stir；
Step 2, state then up and Al (NO are added in solution3)2·9H2O, stir；
Step 3, Ag nano wires then into above-mentioned solution are added, after stirring, are transferred the solution into water heating kettle, in perseverance
Hydro-thermal reaction 20h at 130 DEG C of temperature, after reaction terminates, room temperature is naturally cooled to, centrifuged successively with alcohol and deionized water,
Washing, repeated washing three times after, gained is precipitated into drying；
Step 4, 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,
It is allowed to be completely dissolved, naturally cools to room temperature；Then above-mentioned precipitation is taken, continues to stir 6h, obtains mixed solution A；
Step 5, above-mentioned mixed solution A is fitted into spinneret pipe, inserts 10cm copper wire as positive pole, aluminium foil conduct
Receiver board, is negative pole, and electrostatic spinning when institute making alive is 15kV, and distance is 20cm between spinning head fish receiver board, carries out electrostatic
Spinning, obtain polyvinyl alcohol/ZnO/Ag/Al composite nano fibers；
Step 6, above-mentioned polyvinyl alcohol/ZnO/Ag/Al composite nano fibers are made annealing treatment into 5h at 550 DEG C, to remove
High-molecular polyivnyl alcohol, obtain ZnO composite nano fibers.
Further, after above-mentioned ZnO composite nano fibers being configured into slurry, coated in ceramic pipe surface, electrode is prepared
Afterwards, a kind of alcohol gas sensor based on ZnO composite fibres of the present invention is produced.
Embodiment 1
In the present embodiment, a kind of alcohol gas sensor based on ZnO composite fibres, the sensor is heater-type knot
Structure, the alumina ceramic tube of 2 parallel and discrete annular gold electrodes is come with, coated in the quick of ceramic pipe surface by outer surface
Feel material, the nichrome heating coil composition through earthenware, two platinum filament pins are connected with each gold electrode；It is described quick
It is ZnO composite nano fibers prepared by method of electrostatic spinning to feel material, and thickness is 0.2~0.5mm, and, the ZnO composite nano fibers
Material is specially ZnO microsphere doping metals nano wire and Al.
The preparation process of above-mentioned ZnO composite nano fibers is as follows：
Step 1, take 5mmol zinc acetates and 10mmol urea to be dissolved in 40ml deionized water, stir；
Step 2, state then up and Al (NO are added in solution3)2·9H2O, stir；
Step 3, Ag nano wires then into above-mentioned solution are added, after stirring, are transferred the solution into water heating kettle, in perseverance
Hydro-thermal reaction 20h at 130 DEG C of temperature, after reaction terminates, room temperature is naturally cooled to, centrifuged successively with alcohol and deionized water,
Washing, repeated washing three times after, gained is precipitated into drying；
Step 4, 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,
It is allowed to be completely dissolved, naturally cools to room temperature；Then above-mentioned precipitation is taken, continues to stir 6h, obtains mixed solution A；
Step 5, above-mentioned mixed solution A is fitted into spinneret pipe, inserts 10cm copper wire as positive pole, aluminium foil conduct
Receiver board, is negative pole, and electrostatic spinning when institute making alive is 15kV, and distance is 20cm between spinning head fish receiver board, carries out electrostatic
Spinning, obtain polyvinyl alcohol/ZnO/Ag/Al composite nano fibers；
Step 6, above-mentioned polyvinyl alcohol/ZnO/Ag/Al composite nano fibers are made annealing treatment into 5h at 550 DEG C, to remove
High-molecular polyivnyl alcohol, obtain ZnO composite nano fibers.
In the present embodiment, the mass content of metal nanometer line is 6% in the ZnO composite nano fibers, and the ZnO is compound
Al mass content is 5% in nanofiber.
The electric current of heating coil is flowed through to regulate and control the operating temperature of sensor by changing, and is 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 is 7.9 in the present embodiment.
Embodiment 2
In the present embodiment, a kind of alcohol gas sensor based on ZnO composite fibres, the sensor is heater-type knot
Structure, the alumina ceramic tube of 2 parallel and discrete annular gold electrodes is come with, coated in the quick of ceramic pipe surface by outer surface
Feel material, the nichrome heating coil composition through earthenware, two platinum filament pins are connected with each gold electrode；It is described quick
It is ZnO composite nano fibers prepared by method of electrostatic spinning to feel material, and thickness is 0.2~0.5mm, and, the ZnO composite nano fibers
Material is specially ZnO microsphere doping metals nano wire and Al.
The preparation process of above-mentioned ZnO composite nano fibers is as follows：
Step 1, take 5mmol zinc acetates and 10mmol urea to be dissolved in 40ml deionized water, stir；
Step 2, state then up and Al (NO are added in solution3)2·9H2O, stir；
Step 3, Ag nano wires then into above-mentioned solution are added, after stirring, are transferred the solution into water heating kettle, in perseverance
Hydro-thermal reaction 20h at 130 DEG C of temperature, after reaction terminates, room temperature is naturally cooled to, centrifuged successively with alcohol and deionized water,
Washing, repeated washing three times after, gained is precipitated into drying；
Step 4, 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,
It is allowed to be completely dissolved, naturally cools to room temperature；Then above-mentioned precipitation is taken, continues to stir 6h, obtains mixed solution A；
Step 5, above-mentioned mixed solution A is fitted into spinneret pipe, inserts 10cm copper wire as positive pole, aluminium foil conduct
Receiver board, is negative pole, and electrostatic spinning when institute making alive is 15kV, and distance is 20cm between spinning head fish receiver board, carries out electrostatic
Spinning, obtain polyvinyl alcohol/ZnO/Ag/Al composite nano fibers；
Step 6, above-mentioned polyvinyl alcohol/ZnO/Ag/Al composite nano fibers are made annealing treatment into 5h at 550 DEG C, to remove
High-molecular polyivnyl alcohol, obtain ZnO composite nano fibers.
In the present embodiment, the mass content of metal nanometer line is 8% in the ZnO composite nano fibers, and the ZnO is compound
Al mass content is 6% in nanofiber.
The electric current of heating coil is flowed through to regulate and control the operating temperature of sensor by changing, and is 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 is 15.2 in the present embodiment.
Embodiment 3
In the present embodiment, a kind of alcohol gas sensor based on ZnO composite fibres, the sensor is heater-type knot
Structure, the alumina ceramic tube of 2 parallel and discrete annular gold electrodes is come with, coated in the quick of ceramic pipe surface by outer surface
Feel material, the nichrome heating coil composition through earthenware, two platinum filament pins are connected with each gold electrode；It is described quick
It is ZnO composite nano fibers prepared by method of electrostatic spinning to feel material, and thickness is 0.2~0.5mm, and, the ZnO composite nano fibers
Material is specially ZnO microsphere doping metals nano wire and Al.
The preparation process of above-mentioned ZnO composite nano fibers is as follows：
Step 1, take 5mmol zinc acetates and 10mmol urea to be dissolved in 40ml deionized water, stir；
Step 2, state then up and Al (NO are added in solution3)2·9H2O, stir；
Step 3, Ag nano wires then into above-mentioned solution are added, after stirring, are transferred the solution into water heating kettle, in perseverance
Hydro-thermal reaction 20h at 130 DEG C of temperature, after reaction terminates, room temperature is naturally cooled to, centrifuged successively with alcohol and deionized water,
Washing, repeated washing three times after, gained is precipitated into drying；
Step 4, 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,
It is allowed to be completely dissolved, naturally cools to room temperature；Then above-mentioned precipitation is taken, continues to stir 6h, obtains mixed solution A；
Step 5, above-mentioned mixed solution A is fitted into spinneret pipe, inserts 10cm copper wire as positive pole, aluminium foil conduct
Receiver board, is negative pole, and electrostatic spinning when institute making alive is 15kV, and distance is 20cm between spinning head fish receiver board, carries out electrostatic
Spinning, obtain polyvinyl alcohol/ZnO/Ag/Al composite nano fibers；
Step 6, above-mentioned polyvinyl alcohol/ZnO/Ag/Al composite nano fibers are made annealing treatment into 5h at 550 DEG C, to remove
High-molecular polyivnyl alcohol, obtain ZnO composite nano fibers.
In the present embodiment, the mass content of metal nanometer line is 9% in the ZnO composite nano fibers, and the ZnO is compound
Al mass content is 7% in nanofiber.
The electric current of heating coil is flowed through to regulate and control the operating temperature of sensor by changing, and is 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 is 13.1 in the present embodiment.
The preferred mode of the present invention is the foregoing is only, is not intended to limit the invention, it is all in the spiritual and former of the present invention
Within then, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (7)
1. a kind of alcohol gas sensor based on ZnO composite fibres, the gas sensor by outer surface come with 2 it is parallel and
Alumina ceramic tube, the sensitive material coated in ceramic pipe surface, the nickel chromium triangle through earthenware of discrete annular gold electrode close
Golden heating coil is formed, and two platinum filament pins are connected with each gold electrode；Characterized in that, the sensitive material is Static Spinning
Silk method prepare ZnO composite nano fibers, the ZnO composite nano-fiber materials be specially ZnO microsphere doping metals nano wire and
Al。
2. a kind of alcohol gas sensor based on ZnO composite fibres according to claim 1, it is characterised in that described
ZnO composite nano fibers thickness is 0.2~0.5mm.
3. a kind of alcohol gas sensor based on ZnO composite fibres according to claim 1, it is characterised in that described
The a diameter of 300nm of ZnO composite nano fibers.
4. a kind of alcohol gas sensor based on ZnO composite fibres according to claim 3, it is characterised in that described
The mass content of metal nanometer line is 6~9% in ZnO composite nano fibers.
A kind of 5. alcohol gas sensor based on ZnO composite fibres according to claim 4, it is characterised in that the gold
Category nano wire is Ag nano wires, and the Ag nanowire lengths are 200nm, a diameter of 50nm.
6. a kind of alcohol gas sensor based on ZnO composite fibres according to claim 3, it is characterised in that described
Al mass content is 5~7% in ZnO composite nano fibers.
7. a kind of alcohol gas sensor based on ZnO composite fibres according to claim 3, it is characterised in that above-mentioned
The preparation process of ZnO composite nano fibers：
Step 1, take 5mmol zinc acetates and 10mmol urea to be dissolved in 40ml deionized water, stir；
Step 2, state then up and Al (NO are added in solution3)2·9H2O, stir；
Step 3, Ag nano wires then into above-mentioned solution are added, after stirring, are transferred the solution into water heating kettle, in constant temperature
Hydro-thermal reaction 20h at 130 DEG C, after reaction terminates, room temperature is naturally cooled to, centrifuged, washed with alcohol and deionized water successively
Wash, repeated washing three times after, gained is precipitated into drying；
Step 4, 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
It is completely dissolved, naturally cools to room temperature；Then above-mentioned precipitation is taken, continues to stir 6h, obtains mixed solution A；
Step 5, above-mentioned mixed solution A is fitted into spinneret pipe, inserts 10cm copper wire as positive pole, aluminium foil is as reception
Plate, is negative pole, and electrostatic spinning when institute making alive is 15kV, and distance is 20cm between spinning head fish receiver board, carries out electrostatic spinning,
Obtain polyvinyl alcohol/ZnO/Ag/Al composite nano fibers；
Step 6, above-mentioned polyvinyl alcohol/ZnO/Ag/Al composite nano fibers are made annealing treatment into 5h at 550 DEG C, to remove high score
Sub- polyvinyl alcohol, obtain ZnO composite nano fibers.
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|---|---|---|---|---|
| CN108387612A (en) * | 2018-02-26 | 2018-08-10 | 吉林大学 | With Al2O3/α-Fe2O3Composite nano fiber is sensitive material triethylamine sensor and preparation method thereof |
| CN108956713A (en) * | 2018-06-29 | 2018-12-07 | 五邑大学 | ZnO/ carbon nanocoils sensitive material of propagation path horizontal distribution and preparation method thereof and high sensitivity sensor |
| CN110865034A (en) * | 2019-10-22 | 2020-03-06 | 东北大学 | Ethanol gas sensor based on tunable polymer micro-bottle |
| CN113092539A (en) * | 2021-03-16 | 2021-07-09 | 宁波大学 | High-stable-state PUF (physical unclonable function) utilizing semiconductor gas sensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108956713B (en) * | 2018-06-29 | 2020-12-01 | 五邑大学 | ZnO/carbon nanowire sensitive material with horizontally distributed propagation paths, preparation method thereof and high-sensitivity sensor |
| CN110865034A (en) * | 2019-10-22 | 2020-03-06 | 东北大学 | Ethanol gas sensor based on tunable polymer micro-bottle |
| CN113092539A (en) * | 2021-03-16 | 2021-07-09 | 宁波大学 | High-stable-state PUF (physical unclonable function) utilizing semiconductor gas sensor |
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