CN109211985A - A kind of flexibility alkaline gas sensing chip and preparation method thereof - Google Patents
A kind of flexibility alkaline gas sensing chip and preparation method thereof Download PDFInfo
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- CN109211985A CN109211985A CN201811022316.5A CN201811022316A CN109211985A CN 109211985 A CN109211985 A CN 109211985A CN 201811022316 A CN201811022316 A CN 201811022316A CN 109211985 A CN109211985 A CN 109211985A
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- 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
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Abstract
The present invention is a kind of flexible alkaline gas sensing chip and preparation method thereof, belongs to gas sensor domain；The chip can adsorb the alkaline gas with amino to change the conductivity of itself, to achieve the purpose that for ammonia concentration to be transformed into electric signal, and then detection gas concentration；Specifically include flexible material, conductive silver glue, the Copper thin film of 2 one-side band glue；Flexible material entirely senses primitive and electrode as the substrate-loading of entire chip, chip surface is two-dimentional acidic surface class graphene Ti3C2Tx, two panels Copper thin film is affixed on above sensing primitive, will be sensed primitive by conductive silver glue and is connected with Copper thin film, pad of the exposed copper electrode as conducting wire.Compared with traditional alkaline gas sensing chip, the chip volume is small, it is at low cost, it can produce in enormous quantities, chip can change shape because of flexible substrates, structure is simple, it is easy to operate, there is sensitive response, fast response time to the alkaline gas containing amino or amido, detectable limit is low, is convenient for carrying.
Description
Technical field
The invention belongs to electronic gas sensor fields, and in particular to a kind of flexibility alkaline gas sensing chip and its preparation
Method.
Background technique
With the development of industrial technology, atmosphere pollution has become the environmental problem got worse that countries in the world face, system
The about fast development of various countries' political economy, while compromising the normal health life of the people.How its harm and shadow are mitigated
It rings, is current great and urgent project.Therefore, for some inflammable, explosive and toxic volatile organic compounds such as ammonia
The detection of gas, amide, nitrogenous compound or sulfur-containing compound seems ever more important.Gas sensor is mainly used for various gases
Detection, gas sensor is a kind of device that gaseous species and its concentration relevant information can be converted into electric signal.According to this
The power of a little electric signals is obtained under test gas relevant information, so as to be detected, monitored, alarmed；It can also lead to
Cross interface circuit and the automatic detection of computer composition, control, alarm system.Gas sensor can be divided into four major class from principle:
Electricity gas sensor, optics gas sensor, electrochemistry class gas sensor, other types sensor.
A current important development direction of gas sensor is exactly to develop new gas sensitive material, and new gas is sensitive
Material is the material base of sensor technology progress.The research of current novel gas sensitive primarily focuses on semiconductor material, pottery
Ceramic material and high-molecular organic material.To semiconductor material except one metal oxide materials of bill outside, also develop many multiple
Close metal oxide materials and mixed metallic oxide material.It mainly is improved by the way of doping to semiconductor gas sensor
Performance, such as by adding Pt in semiconductor material, Pd, Ir etc. are greatly improved gas sensitivity and response time,
The selectivity of gas sensor can be improved by adding different catalyst.The spirit of gas sensor is improved by improving manufacture craft
Sensitivity, selectivity, stability etc..By means of semiconductor technology, it can make sensor from unit piece, single function to polynary
It is part, multi-functional, i.e., it is multiple sensors and information processing and conversion circuit is integrated on one chip, with computer technology knot
It closes, intelligent gas sensor system-electronic nose is made, for automatic identification gaseous species, Automatic-searching gas source etc..
Currently, two-dimentional class graphene Ti3C2Tx starts than the new material of graphene advantageously by pass as a kind of
Note.Two-dimentional Ti3C2Tx removes carbide Ti3AlC2, the multilayer corroded using hydrofluoric acid by ternary alloy three-partalloy as a kind of
Grain, makes it have biggish specific surface area and porous adsorption capacity, compared with common graphene, two-dimentional Ti3C2Tx tool
There are very high elasticity modulus and bending strength.In terms of characteristic electron, two-dimentional class graphene Ti3C2Tx remains the gold of its alloy
While belonging to characteristic, due to that can only be prepared using the equal chemical liquid phase etching method of HF etching MAX with functional groups such as F, OH, O
MXene, the Ti3C2 with F and OH functional group show apparent characteristic of semiconductor, and have apparent thermoelectricity effect in low temperature
It answers.
Summary of the invention
For detection gas concentration, the invention proposes a kind of flexible alkaline gas sensing chips and preparation method thereof, should
Chip can adsorb the alkaline gas with amino to change the conductivity of itself, and ammonia concentration is transformed into electric signal to reach
Purpose.The flexible alkaline gas sensing chip, specifically includes flexible material, and the copper of conductive silver glue, 2 one-side band glue is thin
Film；Flexible material entirely senses primitive and electrode as the substrate-loading of entire chip, and chip surface is two-dimentional acidic surface class
Graphene Ti3C2Tx, two panels Copper thin film are affixed on above sensing primitive, will be sensed primitive by conductive silver glue and are connected with Copper thin film,
Pad of the exposed copper electrode as conducting wire.
The two-dimentional acidic surface class graphene Ti3C2Tx is specifically included: the two-dimentional acidic surface class graphene
Ti3C2Tx reacts open loop with the hydroxyl on the surface class graphene Ti3C2Tx under anhydrous liquid environment using succinic anhydride, by carboxylic acid
Functional group modification forms acidic surface class graphene Ti3C2Tx in class grapheme material surface.
The flexible material is the similar materials materials such as filter paper or cloth；Template is the flexible material when preparation,
Surface corresponds to ink when making galley with hydrophobic material be water-based material, and surface corresponds to ink when making galley with water wetted material
Water is oily material.
A kind of preparation method of flexibility alkaline gas sensing chip, specifically comprises the following steps:
(1) two-dimentional acidic surface class graphene Ti3C2Tx is prepared；
(2) flexible alkaline gas sensing chip is prepared.
The step (1) specifically includes:
The succinic anhydride of the two-dimentional class graphene Ti3C2Tx powder of 0.5mg and 1.9g is successively poured into dehydrated alcohol, is put
Enter magneton, bottleneck is sealed with sealed membrane；It is stirred at room temperature with the speed of 500r, post-processing in a length of 24 hours is to remove when stirring
Remove unreacted succinic anhydride, above-mentioned solution be transferred in centrifuge tube, in supercentrifuge under the revolving speed of 5000rpm from
Heart 20min, removes supernatant later, adds suitable dehydrated alcohol concussion, and centrifugation repeats this process 6 times；It finally will centrifugation
Under powder in N2 protective atmosphere 60 DEG C drying, obtaining surface modification has carboxylic acid functional, with multilayer porous structure, particularly two
Tie up acidic surface class graphene Ti3C2Tx.
The step (2) specifically includes:
Filter paper is fixed on A4 paper, is placed in laser printer, with computer editing's pattern, is all compiled as outside pattern
Print area, it is entirely hydrophobic graphite outside pattern that by laser printer types, obtaining area of the pattern, which is still filter paper,；It will beat
Printed template is placed on pressurizing device, low pressure is formed below template, low pressure size is according to the row between hydrophobic material and ink
Depending on repulsion, generally can smoothly it be flowed down with ink best without being adsorbed as by low pressure；Template slant setting, for hydrophily
Ink topples over ink above template, and hydrophobic region ink flows directly to lower section, and filter paper area of the pattern absorbs ink,
Under low pressure, moisture is drained in ink, and pattern is colored.
The beneficial effects of the present invention are: compared with traditional alkaline gas sensing chip, the chip volume is small, cost
It is low, it can produce in enormous quantities, for chip because flexible substrates can change shape, structure is simple, easy to operate, to containing amino or amine
The alkaline gas of base has sensitive response, and fast response time, usual response time 10-20 seconds, detectable limit was low, can be detected
The low concentration of 0.5ppm, is convenient for carrying.
Detailed description of the invention
Fig. 1 is the substrate filter paper of template；
Fig. 2 is common laser printer；
Fig. 3 is printed die plate pattern；
Fig. 4 is that ink rinses printing；
Fig. 5 is printed pattern；
Fig. 6 is the pictorial diagram of induction chip；
Fig. 7 is that gas sensing tests the schematic device used；
Fig. 8 is response of the flexible alkaline gas sensing chip to NH3 various concentration；
Fig. 9 is induction situation of the flexible alkaline gas sensing chip to gas with various；
Figure 10 is that flexible alkaline gas sensing chip responds the organic amine gas that hairtail corruption distributes.
Specific embodiment
A specific embodiment of the invention is further described below with reference to legend.It is as used in the following examples
Experimental method is conventional method unless otherwise specified.
The present invention specifically includes flexible material, conductive silver glue, the Copper thin film of 2 one-side band glue；Flexible material is as entire
The substrate-loading of chip entirely senses primitive and electrode, and chip surface is two-dimentional acidic surface class graphene Ti3C2Tx, two panels copper
Film is affixed on above sensing primitive, will be sensed primitive by conductive silver glue and is connected with Copper thin film, exposed copper electrode is as conducting wire
Pad.Prepare the method for chip in the present invention and method filtered using a kind of template of regioselectivity, the template with paper or
Based on cloth, surface corresponds to ink when making galley with hydrophobic material be water-based material, and surface makes galley with water wetted material
When to correspond to ink be oily material.Template bottom is reduced into air pressure, template is rinsed with ink, area of the pattern absorbs ink because of low pressure
Moisture pump forms pattern, and non-area of the pattern is because repelling ink without being colored.
Material as used in the following examples, reagent etc., are commercially available unless otherwise specified.
The preparation side of the two-dimentional acidic surface class graphene Ti3C2Tx of -400 mesh of 200 mesh as used in the following examples
Method: the succinic anhydride of the two-dimentional class graphene Ti3C2Tx powder of 0.5mg and 1.9g is successively poured into, in dehydrated alcohol, is put into
Magneton seals bottleneck with sealed membrane.It is stirred at room temperature with the speed of 500r, when stirring is 24 hours a length of.Post-processing is to remove
Go unreacted succinic anhydride, specific steps；Above-mentioned solution is transferred in centrifuge tube, with 5000rpm in supercentrifuge
Revolving speed under be centrifuged 20min, remove supernatant later, add the concussion of suitable dehydrated alcohol, centrifugation, this process repeats 6
It is secondary.Finally the powder under being centrifuged is dried for 60 DEG C in N2 protective atmosphere, obtained two-dimentional acidic surface class graphene Ti3C2Tx
Be multilayer porous structure, particularly.Its surface modification has carboxylic acid functional.
It is hydrophobic template and water-based ink used in following implementations, substrate is by taking filter paper as an example.Made in following embodiments
Water-based ink can be ordinary ink in the market, be also possible to directly be fabricated to stable hang with water and hydrophily pigment
Turbid.
In conjunction with attached drawing 5, the preparation process of flexible alkaline gas sensing chip is as follows:
Filter paper is fixed on A4 paper, is placed in laser printer, with computer editing's pattern, is all compiled as outside pattern
Print area, it is entirely hydrophobic graphite outside pattern that by laser printer types, obtaining area of the pattern, which is still filter paper,.It will beat
Printed template is placed on pressurizing device, low pressure can be formed below template, low pressure size is according between hydrophobic material and ink
Repulsive force depending on, generally can smoothly be flowed down with ink best without being adsorbed as by low pressure.Template wants slant setting, convenient
Next step ink rinses.Above-mentioned ink is hydrophilic liquid, and ink is toppled over above template.Hydrophobic region ink flows directly to
Lower section, and filter paper area of the pattern absorbs ink, moisture is drained under low pressure, in ink, and pattern is colored, as shown in Figure 5.
Embodiment 1, response of the flexible alkaline gas sensing chip to alkaline gas:
The sensing chip prepared is put into gas detection bottle, as shown in Figure 7.Sensing chip is accessed by welding lead
Electrochemical work station, model CH1660E, Shanghai Chen Hua Instrument Ltd., method use current versus time curve, setting output
Voltage it is constant be 1.0V, to induction chip carry out constant potential scanning, obtained current versus time curve only with the resistance of chip
Change related, specific experiment process is as follows:
Air inlet and gas vent are first opened, is closed after being passed through N2 2min from air inlet.Make the atmosphere that N2 is in entire gas cylinder
In, ammonia is injected into gas from intermediate injection port with micro syringe.After chip reaches stable to concentration, then it is passed through
N2 eliminates the inductive signal of chip come the ammonia being discharged in bottle.As shown in figure 8, injection various concentration gas, the response of chip
Situation.The chip has preferable selectivity to alkaline gas containing amino, as shown in figure 9, the response to different gas changes hair
Now NH3 is responded by force, other gases are responded weak.
Embodiment 2, the response for organic amine gas that flexible alkaline gas sensing chip distributes food spoilage:
According to the chip connection method in embodiment 1, chip is connected into electrochemical workstation.
Air inlet and gas vent are first opened, is closed after being passed through N2 2min from air inlet.Make the atmosphere that N2 is in entire gas cylinder
In, the stale hairtail of one fritter is protruded into bottle from bottom ports with spoon.Chip reaches concentration stablize after, then by logical N2 come
The ammonia in bottle is discharged to eliminate the inductive signal of chip.The response for the gas that hairtail block is released for chip as shown in Figure 10
Situation.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of flexibility alkaline gas sensing chip, specifically includes flexible material, conductive silver glue, the Copper thin film of 2 one-side band glue；
Flexible material entirely senses primitive and electrode as the substrate-loading of entire chip, and chip surface is two-dimentional acidic surface class graphite
Alkene Ti3C2Tx, two panels Copper thin film are affixed on above sensing primitive, will be sensed primitive by conductive silver glue and are connected with Copper thin film, exposed
Pad of the copper electrode as conducting wire.
2. a kind of flexible alkaline gas sensing chip according to claim 1, which is characterized in that the acid table of the two dimension
Noodles graphene Ti3C2Tx is specifically included:
The two-dimentional acidic surface class graphene Ti3C2Tx using succinic anhydride under anhydrous liquid environment with class graphene
The hydroxyl on the surface Ti3C2Tx reacts open loop, and carboxylic acid function is rolled into a ball modification in class grapheme material surface, forms acidic surface class stone
Black alkene Ti3C2Tx.
3. a kind of flexible alkaline gas sensing chip according to claim 1, it is characterised in that: the flexible material is
The similar materials material such as filter paper or cloth；Template is the flexible material when preparation, and surface makes galley with hydrophobic material
When to correspond to ink be water-based material, it is oily material that surface, which corresponds to ink when making galley with water wetted material,.
4. a kind of preparation method of flexibility alkaline gas sensing chip, specifically comprises the following steps:
(1) two-dimentional acidic surface class graphene Ti3C2Tx is prepared；
(2) flexible alkaline gas sensing chip is prepared.
5. a kind of preparation method of flexible alkaline gas sensing chip according to claim 3, which is characterized in that described
Step (1) specifically includes:
The succinic anhydride of the two-dimentional class graphene Ti3C2Tx powder of 0.5mg and 1.9g is successively poured into dehydrated alcohol, magnetic is put into
Son seals bottleneck with sealed membrane；It is stirred at room temperature with the speed of 500r, post-processing in a length of 24 hours is to remove not when stirring
Above-mentioned solution is transferred in centrifuge tube by the succinic anhydride of reaction, to be centrifuged under the revolving speed of 5000rpm in supercentrifuge
20min removes supernatant later, adds suitable dehydrated alcohol concussion, and centrifugation repeats this process 6 times；It finally will be under centrifugation
Powder in N2 protective atmosphere 60 DEG C drying, obtaining surface modification has carboxylic acid functional, with multilayer porous structure, particularly two dimension
Acidic surface class graphene Ti3C2Tx.
6. a kind of preparation method of flexible alkaline gas sensing chip according to claim 3, which is characterized in that described
Step (2) specifically includes:
Filter paper is fixed on A4 paper, is placed in laser printer, with computer editing's pattern, all is compiled as printing outside pattern
Region, it is entirely hydrophobic graphite outside pattern that by laser printer types, obtaining area of the pattern, which is still filter paper,；It will be printed
Template be placed on pressurizing device, low pressure is formed below template, low pressure size is according to the repulsive force between hydrophobic material and ink
Depending on, it generally can smoothly be flowed down with ink best without being adsorbed as by low pressure；Template slant setting, for hydrophily ink
Water topples over ink above template, and hydrophobic region ink flows directly to lower section, and filter paper area of the pattern absorbs ink, low
It depresses, moisture is drained in ink, and pattern is colored.
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Cited By (3)
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| CN110095509A (en) * | 2019-05-27 | 2019-08-06 | 电子科技大学 | Ti3C2Tx/ polyaniline laminated film ammonia gas sensor and the preparation method and application thereof |
| CN110672670A (en) * | 2019-10-18 | 2020-01-10 | 吉林大学 | Planar flexible room temperature NO based on three-dimensional MXene folded ball/ZnO composite material2Sensor and preparation method thereof |
| CN115078489A (en) * | 2022-05-31 | 2022-09-20 | 复旦大学 | Bionic sensing device integrating smell sense and vision and preparation method thereof |
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| CN109211985B (en) | 2020-12-04 |
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