CN108414585A - Gas sensor device and method is prepared in situ in a kind of method of electrostatic spinning - Google Patents
Gas sensor device and method is prepared in situ in a kind of method of electrostatic spinning Download PDFInfo
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- CN108414585A CN108414585A CN201810216606.7A CN201810216606A CN108414585A CN 108414585 A CN108414585 A CN 108414585A CN 201810216606 A CN201810216606 A CN 201810216606A CN 108414585 A CN108414585 A CN 108414585A
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- gas sensor
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- electrostatic spinning
- collecting board
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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
-
- 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
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
Abstract
The invention discloses a kind of method of electrostatic spinning, and gas sensor device and method is prepared in situ, especially a kind of for manufacturing the device and method based on micron or nano-scale fiber gas sensor.Device includes liquid storage syringe, syringe needle, peristaltic pump, high voltage power supply, collecting board, electric rotating machine, ceramic tube etc., wherein liquid storage syringe is connected with peristaltic pump, liquid storage syringe syringe needle and collecting board are vertically opposite, high-voltage power supply anode is connected with syringe needle, high-voltage power supply cathode is connected with collecting board, iron needle is connected with electric rotating machine, and ceramic tube, which is tightly placed on iron needle, makes it vacantly be placed in and collecting board groove.Apparatus of the present invention and method prepare the device and method of gas sensor relative to tradition, reduce grinding, applied with two passes process, promote its production efficiency and controllability, more conducively realize scale industrial production.
Description
【Technical field】
The present invention relates to a kind of method of electrostatic spinning, and gas sensor device and method is prepared in situ, more particularly to one kind is used for
Manufacture the device and method based on micron or nano-scale fiber gas sensor.
【Background technology】
Gas sensor is widely used in examining the toxic and harmful gas in the presence of industrial production and public place
It surveys, ensures the movable safety of the production and living of people.Electrostatic spinning manufacturing device is simple, cost of spinning is cheap, by method of electrostatic spinning
The Application of micron of preparation has larger prospects for commercial application in gas sensor.Currently, the gas based on electrostatic spinning passes
Sensor need by the material that electrostatic spinning is prepared need through Overheating Treatment again underhand polish, be coated on ceramic tube, significantly
Reduce production efficiency and repeatability.
The purpose of the present invention is to provide a kind of method of electrostatic spinning, and gas sensor device and method is prepared in situ,
The ceramic tube controlled with electric rotating machine is increased on the collection device of conventional electrostatic spinning, realizes and gas sensing is prepared in situ
Device.Method of the present invention reduces grinding, applied with two passes process relative to conventional method, makes production efficiency and controllability
It greatly promotes, it is easy to accomplish scale industrialization production.
【Invention content】
1. gas sensor device and method is prepared in situ in a kind of method of electrostatic spinning, production efficiency can be effectively improved.
2. gas sensor device is prepared in situ in a kind of method of electrostatic spinning, it is characterised in that include mainly
(1) spinning supplying module, including the syringe needle of the liquid storage syringe of storage solution and connection liquid storage syringe, offer spinning
The peristaltic pump of silk power；
(2) high voltage power supply is electrically connected to spinning attack unit and collector unit, for spinning solution and collector unit it
Between form an electric field；
(3) collection module, including collecting board, electric rotating machine, ceramic tube etc..
3. gas sensor method is prepared in situ in a kind of method of electrostatic spinning, carry out as steps described below：
(1) by 10% polymer, including polyvinylpyrrolidone PVP or polyacrylonitrile (PAN), 10% salting liquid, including nitre
Hydrochlorate, acetate or 80% ethyl alcohol of chloride and the mixture of DMF are mixed evenly, place in liquid storage syringe；
(2) liquid storage syringe is connected with peristaltic pump, liquid storage syringe syringe needle and collecting board are vertically opposite, high-voltage power supply anode and needle
Head is connected, and high-voltage power supply cathode is connected with collecting board, and iron needle is connected with electric rotating machine, and ceramic tube is tightly placed on iron needle, and iron needle is hanging
It is placed in and collecting board groove；
(3) after checking line security, peristaltic pump, high-voltage power supply and electric rotating machine are opened；
(4) after lasting a period of time, power supply is closed, ceramic tube is taken out from needle, ceramic tube is heat-treated；
(5) gold paste is coated at ceramic tube both ends, around upper platinum filament；
(6) ceramic tube that the 5th step obtains is heat-treated.
【Description of the drawings】
(1) Fig. 1 is that gas sensor schematic device is prepared in situ in a kind of method of electrostatic spinning of the present invention
(2) in figure：1-spinning supplying module, 2-liquid storage syringes, 3-syringe needles, 4-high voltage power supplies, 5-collection modules,
6-iron needles, 7-ceramic tubes, 8-collecting boards, 9-electric rotating machines.
【Specific implementation mode】
It is further details of with reference to the accompanying drawings and examples to illustrate the present invention, but it is not only limited to following embodiment.
In addition, for ease of description, attached drawing only illustrates part-structure rather than entire infrastructure related to the present invention.
Referring to Fig. 1, gas sensor device is prepared in situ in a kind of method of electrostatic spinning, including：Spinning supplying module 1, height
Voltage source 4, collection module 5.
The spinning supplying module 1 includes liquid storage syringe 2 and the syringe needle 3 being connected with the liquid storage syringe, the syringe needle 3
It is the discharge port of spinning solution.Spinning solution is polymer solution, can form pendant drop at discharge port, that is, syringe needle 3, overhang
Drop maintains the end of syringe needle 3 under the action of surface tension.The vertical range of the syringe needle 3 and collection module 5 can be
The vertical range of selection in wide range, the syringe needle 3 and collection module 5 is 5-25cm.Further, the liquid storage syringe 2 can
The accurate adjusting for going out liquid speed degree between 0.1ml/h-10ml/h is realized to be connect with peristaltic pump.It is furthermore preferred that the syringe needle 3
It can be adjusted according to actual demand with the vertical range of collection template 5 and the liquid speed degree that goes out of peristaltic pump.
4 anode of the high voltage power supply is electrically connected with syringe needle three, and 4 cathode of the high voltage power supply is electrically connected with collecting board.Into one
Step, the high voltage power supply 4 can provide the high-pressure electrostatic of 0.1-30kv.It is furthermore preferred that the high voltage power supply 4 provides 10-20kv
High-pressure electrostatic.
The collection module 5 includes collecting board 8, ceramic tube 7, the electric rotating machine 9 being connected with the ceramic tube and described
Connector iron needle 6 between ceramic tube and the electric rotating machine.Further, ceramic tube 7 passes through connector iron needle 6 and electric rotating machine
9 form mechanical connection, and are parallelly vacantly placed among the groove of collecting board 8.The rotating speed of the electric rotating machine 9 is that 1-30 turns every
Second.Gas sensor device is prepared in situ with a kind of method of electrostatic spinning of the present invention and obtains the Static Spinning needed for single gas sensor
The silk time is 1-20 minutes.It is furthermore preferred that described need electric rotating machine rotating speed can be according to actual demand tune with the electrostatic spinning time
It is whole.
Embodiment 1：It is small that polyacrylonitrile 10%, stannous chloride 10%, N,N-dimethylformamide 80% stir 6 at normal temperatures
When, it is then transferred in liquid storage syringe, it is 12cm to adjust syringe needle end with collecting board distance, and adjustment wriggling pumps out liquid speed degree and is
0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjusts electric rotating machine
Speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, setting voltage is
10kv.After ten minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, at ceramic tube both ends
Coat gold paste, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 2：Polyacrylonitrile 10%, stannous chloride 9.5%, copper oxide 0.5%, N,N-dimethylformamide 80% exist
It stirs 6 hours, is then transferred in liquid storage syringe under room temperature, adjustment syringe needle end is 12cm with collecting board distance, adjusts peristaltic pump
It is 0.6ml/h to go out liquid speed degree.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, is adjusted
Whole electric rotating machine speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, if
It is 10kv to set voltage.After ten minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, in ceramics
Pipe coats gold paste at both ends, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 3：Polyacrylonitrile 10%, stannous chloride 9%, copper oxide 1%, N,N-dimethylformamide 80% are in room temperature
Lower stirring 6 hours, is then transferred in liquid storage syringe, and adjustment syringe needle end is 12cm with collecting board distance, and adjustment, which is wriggled, pumps out liquid
Speed is 0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjustment rotation
Rotating motor speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, setting electricity
Pressure is 10kv.After ten minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, in ceramic tube two
Gold paste is coated at end, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 4：Polyacrylonitrile 10%, stannous chloride 8.5%, copper oxide 1.5%, N,N-dimethylformamide 80% exist
It stirs 6 hours, is then transferred in liquid storage syringe under room temperature, adjustment syringe needle end is 12cm with collecting board distance, adjusts peristaltic pump
It is 0.6ml/h to go out liquid speed degree.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, is adjusted
Whole electric rotating machine speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, if
It is 10kv to set voltage.After ten minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, in ceramics
Pipe coats gold paste at both ends, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
As a child by gas sensor aging 24 made from above-described embodiment 1 to embodiment 4, air-sensitive performance survey is carried out to it
Examination, test result is as follows shown in table：
As seen from table, when copper oxide accounting amount is relatively low, fail to form a large amount of PN junction on material microstructure, therefore to sulphur
The sensitivity for changing hydrogen is relatively low.When copper oxide accounting is appropriate, the PN junction quantity of mass efficient is constituted, to the high sensitivity of hydrogen sulfide
Up to 30.When copper oxide accounting is excessively high, though forming a large amount of PN junction, due to the excess of copper oxide, the ratio that PN junction accounts for declines,
Therefore hydrogen sulfide sensitivity is declined.
Embodiment 5：Polyvinylpyrrolidone 10%, stannous chloride 10%, N,N-dimethylformamide 80% are at normal temperatures
Stirring 6 hours, is then transferred in liquid storage syringe, and adjustment syringe needle end is 12cm with collecting board distance, and adjustment, which is wriggled, pumps out liquid speed
Degree is 0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjustment rotation
Motor speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, voltage is set
For 10kv.After electrostatic spinning 1 minute, ceramic tube is taken out, is annealed 2 hours for 300 DEG C in Muffle furnace, at ceramic tube both ends
Coat gold paste, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 6：Polyvinylpyrrolidone 10%, stannous chloride 10%, N,N-dimethylformamide 80% are at normal temperatures
Stirring 6 hours, is then transferred in liquid storage syringe, and adjustment syringe needle end is 12cm with collecting board distance, and adjustment, which is wriggled, pumps out liquid speed
Degree is 0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjustment rotation
Motor speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, voltage is set
For 10kv.After five minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, at ceramic tube both ends
Coat gold paste, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 7：Polyvinylpyrrolidone 10%, stannous chloride 10%, N,N-dimethylformamide 80% are at normal temperatures
Stirring 6 hours, is then transferred in liquid storage syringe, and adjustment syringe needle end is 12cm with collecting board distance, and adjustment, which is wriggled, pumps out liquid speed
Degree is 0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjustment rotation
Motor speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, voltage is set
For 10kv.After ten minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, at ceramic tube both ends
Place coats gold paste, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Embodiment 8：Polyvinylpyrrolidone 10%, stannous chloride 10%, N,N-dimethylformamide 80% are at normal temperatures
Stirring 6 hours, is then transferred in liquid storage syringe, and adjustment syringe needle end is 12cm with collecting board distance, and adjustment, which is wriggled, pumps out liquid speed
Degree is 0.6ml/h.One ceramic tube is connected to electric rotating machine by iron needle and is placed in the groove of collecting board, adjustment rotation
Motor speed is 15 revolution per seconds.Syringe needle and collecting board are electrically connected with high voltage power supply, open high voltage power supply, voltage is set
For 10kv.After twenty minutes, ceramic tube is taken out for electrostatic spinning, is annealed 2 hours for 300 DEG C in Muffle furnace, at ceramic tube both ends
Place coats gold paste, around upper platinum filament again in Muffle furnace 300 DEG C annealing half an hour, obtain gas sensor.
Gas sensor aging 24 made from above-described embodiment 5 to embodiment 8 as a child, is tested for the property it,
The results are shown in table below：
As seen from table, when the electrostatic spinning time is too low, tin oxide nano fiber is only deposited on ceramic tube on a small quantity, is only capable of shape
At a small amount of effective electron transmission path, thus it is relatively low to the sensitivity of hydrogen sulfide.When the electrostatic spinning time is appropriate, can be formed with
The electron-transport path of effect, to the sensitivity of hydrogen sulfide up to 2.And when electrostatic spinning overlong time, though form complete electricity
Sub- transmission network, but it increases in the film thickness of ceramic tube, causes effective sensitive layer accounting relatively low, therefore under hydrogen sulfide sensitivity
Drop.
Claims (10)
1. gas sensor device is prepared in situ in a kind of method of electrostatic spinning, it is characterised in that include mainly
Spinning supplying module, including the syringe needle of the liquid storage syringe of storage solution and connection liquid storage syringe, offer spinning power
Peristaltic pump；
High voltage power supply is electrically connected to spinning attack unit and collector unit, for being formed between spinning solution and collector unit
One electric field；
Collection module, including collecting board, electric rotating machine, ceramic tube.
2. a kind of method that gas sensor is prepared in situ in method of electrostatic spinning, which is characterized in that including step once
(1) spinning solution is configured：8-12% polymer, including polyvinylpyrrolidone PVP or polyacrylonitrile (PAN), 8-12% salt
Solution, including nitrate, acetate and chloride, 75-80% ethyl alcohol and n,N-Dimethylformamide DMF mixtures, stirring
Uniformly；
(2) it builds electrostatic spinning and gas sensor device is prepared in situ, liquid storage syringe is connected with peristaltic pump, high-voltage power supply anode and needle
Head is connected, and high-voltage power supply cathode is connected with collecting board, and syringe needle is vertically opposite with collecting board, and iron needle is vacantly placed in recessed with aluminum collecting board
At slot, ceramic tube is tightly placed on iron needle, and iron needle is connected with electric rotating machine；
(3) after checking line security, peristaltic pump, high-voltage power supply and electric rotating machine are opened；
(4) after lasting a period of time, power supply is closed, ceramic tube is taken out from needle, ceramic tube is heat-treated；
(5) ceramic tube two is brought out into gold coated slurry, around upper platinum filament, is heat-treated；
(6) ceramic tube and tube chamber welds with base prepared (5) step；
(7) sensor made from (6) step is subjected to aging.
3. gas sensor device is prepared in situ in a kind of method of electrostatic spinning according to claim 1, it is characterised in that collect
Unit is by with reeded collecting board, electric rotating machine, the iron needle being connected on electric rotating machine, ceramic tube composition.
4. gas sensor device is prepared in situ in a kind of method of electrostatic spinning according to claim 1, it is characterised in that syringe needle
It is vertically opposite with collecting board, spacing 5-25cm.
5. gas sensor device is prepared in situ in a kind of method of electrostatic spinning according to claim 1, it is characterised in that collect
Plate is metal or alloy.
6. gas sensor device is prepared in situ in a kind of method of electrostatic spinning according to claim 1, it is characterised in that ceramics
Pipe is parallel to collecting board and the groove in collecting board.
7. gas sensor device is prepared in situ in a kind of method of electrostatic spinning according to claim 1, it is characterised in that described
Electric rotating machine rotating speed be：1-30 revolution per seconds.
8. the method that gas sensor is prepared in situ in a kind of method of electrostatic spinning according to claim 2, it is characterised in that quiet
The time of Electrospun is 1-20 minutes.
9. the method that gas sensor is prepared in situ in a kind of method of electrostatic spinning according to claim 2, it is characterised in that the
(5) heat treatment temperature of step is 300 DEG C -500 DEG C.
10. the method that gas sensor is prepared in situ in a kind of method of electrostatic spinning according to claim 2, it is characterised in that the
(7) ageing time of step be 12 hours and its more than.
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Application publication date: 20180817 |