CN109292734A - A kind of room temperature flexible gas sensor and preparation method thereof based on polycrystalline micro wire grain boundary effect - Google Patents
A kind of room temperature flexible gas sensor and preparation method thereof based on polycrystalline micro wire grain boundary effect Download PDFInfo
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- CN109292734A CN109292734A CN201811120435.4A CN201811120435A CN109292734A CN 109292734 A CN109292734 A CN 109292734A CN 201811120435 A CN201811120435 A CN 201811120435A CN 109292734 A CN109292734 A CN 109292734A
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Abstract
A kind of room temperature flexible gas sensor and preparation method thereof based on polycrystalline micro wire grain boundary effect, belongs to flexible electronic sensor technical field.It is made of fexible film substrate, polycrystalline micro wire and electrode, polycrystalline micro wire is located at fexible film substrate, electrode be strip structure and be located at polycrystalline micro wire on, the both ends of polycrystalline micro wire be separately connected electrode and electrode perpendicular to polycrystalline micro wire radial direction.The polycrystalline micro wire is with highly sensitive and broad stopband metal oxide semiconductor material zinc germanate, indium sesquioxide or zinc oxide of fast-response speed.In the present invention, there are a large amount of defects for polycrystalline micro wire, are conducive to the absorption of gas, and the sensitive mechanism to object gas ammonia is effectively explained by microcosmic atom angle.The present invention improves electrology characteristic, catalytic activity and the mechanical stability of material, can be widely used in wearable electronic field by the polycrystalline micro wire of building grain boundary structure.
Description
Technical field
The invention belongs to flexible electronic sensor technical fields, and in particular to a kind of based on polycrystalline micro wire grain boundary effect
Room temperature flexible gas sensor and preparation method thereof.
Background technique
Currently, exploitation has weight to the development of flexible electronic device with the functional material that high efficiency and stabilization signal export
Want meaning.Using polycrystalline material, there are electronic structure, catalytic activity and mechanics that a large amount of defect can effectively influence material
The features such as performance, provides new thinking for many applications.Therefore, building grain boundary structure, which just becomes, develops high-performance nano material
Effective means.Although the introducing of grain boundary structure has been widely used in creating new physicochemical properties, and exists
Successful proof has been obtained in the fields such as energy, catalysis, electronics and sensor.However, relevant be reported in flexible electronic field
Relatively fewer.
At present, the most important challenge of flexible chamber wet body sensor is that sensitivity is low and stability is poor, i.e., sensitive
Layer surface activity is low, be unfavorable for gas molecule absorption and gas and the stability of sensitive layer surface interaction it is poor.These
Limitation inevitably leads to the low working efficiency of device.Therefore, people's sensing more active, more durable to exploitation is excited
The interest of material.Relative to monocrystal material, grain boundary structure is introduced in polycrystalline material, device can be effectively improved to gas to be measured
The sensitive property and mechanical stability of body.Due to the presence of crystal boundary, there are a large amount of trapping states in nano material, and hang
Chemical bond then will form deep defect state, and significantly affect the gas absorption and electric charge transfer of sensor.Recently, the U.S. she
The Amin Salehi-Khojin professor in Li Nuo university Chicago branch school et al. (Nature Communication 2014,5,
4911) it reports and introduces grain boundary structure in carbon based gas sensing material, gas molecule can be promoted to assemble and accelerate charge turn
It moves, to improve sensitivity (828%) of the device to target gas molecules dimethyl methyl phosphonate sour (DMMP).Although crystal boundary draws
Enter the recognition capability for greatly improving device to target gas molecules, but above-mentioned work its rigid substrate is not suitable for applying
In wearable electronic system.In addition, crystal boundary is deposited other than the introducing of crystal boundary is to the raising of the electronics and catalytic performance of material
It is influenced significantly having on mechanical property.For flexible electronic devices, usually on the surface of different structure, device was being used
Deformation occurs for meeting in journey, and unlike monocrystal material, polycrystalline material has a large amount of crystal boundary when deformation occurs, grain boundaries
Particle can hinder dislocation motion, to increase the mechanical tenacity of device.For this purpose, invent it is a kind of i.e. with highly sensitive, fast-response,
Stablize the characteristics such as good, while the flexible gas sensor that the mechanical flexibility that can have had can be contacted with different objects is flexible
One direction of electronics development.
Summary of the invention
The disadvantage that the purpose of the present invention is overcome monocrystalline micro wire semiconductor material intrinsic as sensitive material, proposes one kind
Polycrystalline micro wire with grain boundary effect, making it not only has high electronics and catalytic activity, but also the machinery that can be provided simultaneously with is soft
Property；It is micro- by polycrystalline the present invention also provides the room temperature high-performance flexible gas sensor based on grain boundary effect polycrystalline micro wire
Rice noodles are prepared.
Micro wire of the present invention is polycrystalline material, and there are a large amount of grain boundary structure, the grain boundary structure is grain
The homojunction that son is formed with particle.
Preferably, the polycrystalline micro wire is with highly sensitive and fast-response speed broad stopband metal-oxide semiconductor (MOS)
Material.
Preferably, the broad stopband metal oxide semiconductor material with highly sensitive and fast-response speed is zinc germanate
(Zn2GeO4), indium sesquioxide (In2O3) or zinc oxide (ZnO)；
Preferably, the polycrystalline micro wire is made of nanoparticle, and the diameter of the nanoparticle is 5~50nm,
The diameter of the polycrystalline micro wire is 3~15 μm.
The present invention also provides a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect, by
Fexible film substrate, polycrystalline micro wire and electrode composition, polycrystalline micro wire are located at fexible film substrate, and electrode is strip knot
Structure and be located at polycrystalline micro wire on, the both ends of polycrystalline micro wire be separately connected electrode and electrode perpendicular to polycrystalline micro wire diameter
To direction.
Preferably, when sensor is exposed in ammonia to be measured, there is a large amount of lack in the polycrystalline micro wire grain boundaries
It falls into, is conducive to ammonia gas absorption in grain boundaries, and accelerate the transfer of electronics, to improve device sensitivity；When external force is applied to
When device both ends, due to the grain boundary structure between particle and particle, the dislocation motion between particle is effectively prevented, material table is reduced
Face stress dynamics, improves the mechanical flexibility of material, to increase the mechanical stability of device.I.e. grain boundary structure plays adjusting micron
Line electronic structure and catalytic performance, be conducive to object gas ammonia gas absorption on the surface of the material with accelerate electronics transfer, and play
Mechanical performance, dispersion ambient pressure are adjusted in the effect on polycrystalline micro wire surface, improves the mechanical flexibility of polycrystalline micro wire.
The present invention also provides a kind of room temperature high-performance flexible gas sensors based on polycrystalline micro wire grain boundary effect
Preparation method, its step are as follows:
(1) 40~80 μm of thickness of the poly- naphthalate of flexible material (PI) is used into ethyl alcohol, acetone, water successively respectively
It is cleaned by ultrasonic surface 10~30 minutes, drying obtains fexible film substrate；
(2) polycrystalline metal oxide micro wire is prepared: by 0.05~2.0g metallic oxide precursor object (zinc acetate (Zn
(CH3COO)2·2H2O) and oxygroup germanium, indium nitrate (In (NO)3·6H2) or zinc acetate (Zn (CH O3COO)2·2H2O) etc.) and
The polyvinylpyrrolidone (PVP) of 0.5~10.0g be added to 10~50mL mixed solution (dimethylformamide (DMF), water and
The mixing (volume ratio is 1:1~2) of ethyl alcohol, water) in, it is stirred 6~30 hours under 300~1500rpm revolution, obtains Static Spinning
Silk solution；Then the electrostatic spinning solution is added in the syringe of 30~100mL, it will be quiet by near field electrostatic spinning method
Electrospun solution is printed upon on poly- naphthalate (PI) fexible film substrate that step (1) obtains, wherein syringe needle
The distance for the fexible film substrate that head is obtained apart from step (1) is 0.5~2.0mm, and electrostatic spinning voltage is 1~3kV, is then existed
It is calcined 1~20 hour under 300~400 DEG C of air atmospheres, obtains the polycrystalline metal oxide micro wire that diameter is 3~15 μm；It should
Polycrystalline metal oxide micro wire is made of nanoparticle, and diameter of nano particles is 5~50nm, and electrostatic spinning apparatus is referring to China
Patent CN105702772A；
(3) surface of the polycrystalline metal oxide micro wire obtained in step (2) deposits to obtain two by surface deposition
Strip silver (Ag) electrode a separate and perpendicular with the radial direction of polycrystalline metal oxide micro wire, strip silver
(Ag) spacing between electrode is 20~100 μm, strip silver (Ag) electrode with a thickness of 80~150nm, to obtain based on more
The room temperature flexible gas sensor of brilliant micro wire grain boundary effect.
The present invention has the characteristics that compared with prior art and advantage:
(1) present invention by simple near field electrostatic spinning technology obtains polycrystalline micro wire, and preparation method is simple, the period compared with
It is short, it can be mass-produced, suitable for the preparation of Multimetal oxide micro-/ nano line and organic material micro-/ nano line, be conducive to
Industrialized production.
(2) present invention is by the polycrystalline micro wire of building grain boundary structure, improve the electrology characteristic of material, catalytic activity and
Mechanical stability can be widely used in wearable electronic field.
(3) in the present invention, polycrystalline micro wire is conducive to the absorption of gas there are a large amount of defect, and passes through microcosmic original
Subangle effectively explains the sensitive mechanism to object gas ammonia.
(4) present invention directly demonstrates the presence of grain boundary structure by quantitative Study on Mechanical Properties and linear meta analysis,
The mechanical flexibility that material can be increased becomes the strong evidence of wearable electronic mechanical flexibility.
Detailed description of the invention:
Fig. 1: the polycrystalline zinc germanate (Zn of the embodiment of the present invention 12GeO4) micro wire room temperature flexible gas sensor microstructure
Schematic diagram；
Each section title are as follows: poly- naphthalate (PI) fexible film substrate 1 is existed using near field electrostatic spinning technology
The polycrystalline micro wire 3 that poly- 1 surface of naphthalate (PI) fexible film substrate directly prints, then in polycrystalline micro wire 3
Both ends are using silver-colored (Ag) electrode 2 of strip of surface deposition deposition and object gas ammonia 4 to be identified.
Fig. 2: (it can be seen that material is made of the crystal grain of different orientation, this is just said polycrystalline prepared by the embodiment of the present invention 1
Bright is polycrystalline material) zinc germanate (Zn2GeO4) micro wire TEM photo；
Fig. 3: polycrystalline zinc germanate (Zn prepared by the embodiment of the present invention 12GeO4) micro wire grain boundary structure HRTEM photo；
Fig. 4: polycrystalline zinc germanate (Zn prepared by the embodiment of the present invention 12GeO4) and monocrystalline zinc germanate (Zn2GeO4)(Nano
Research 2015,8,2162) to the sensitivity curve of target ammonia；
Wherein curve 1 represents polycrystalline zinc germanate (Zn2GeO4) device；Curve 2 represents monocrystalline zinc germanate (Zn2GeO4) device.
Fig. 5: theoretical proof polycrystalline zinc germanate (Zn in the embodiment of the present invention 12GeO4) micro wire has object gas ammonia
High suction-operated schematic diagram；
Wherein: being (a) target gas molecules ammonia and monocrystalline and polycrystalline zinc germanate (Zn2GeO4) intermolecular distance on surface shows
It is intended to, (b) is adsorbed on monocrystalline and polycrystalline zinc germanate (Zn for target gas molecules2GeO4) material surface adsorption energy column diagram.
Fig. 6: polycrystalline zinc germanate (Zn in the embodiment of the present invention 12GeO4) micro wire Young's modulus and linear element analysis chart；
Wherein: (a) being polycrystalline zinc germanate (Zn2GeO4) micro wire Young's modulus figure；It (b) is polycrystalline zinc germanate
(Zn2GeO4) the micro wire surface of micro wire in the bent state stress linear element analysis chart.
Fig. 7: polycrystalline zinc germanate (Zn is based in the embodiment of the present invention 12GeO4) micro wire flexible gas sensor bending and
To the response recovery curve of object gas ammonia under flat state；
Wherein: 1 represents bending state；2 represent flat state.
Fig. 8: the polycrystalline indium sesquioxide (In of the embodiment of the present invention 2 and the preparation of case study on implementation 32O3) micro wire and polycrystalline oxygen
Change zinc (ZnO) micro wire device to the sensitivity curve of object gas ammonia；
Its medium sensitivity is defined here as the variation of Opposed Current: △ I/I0, △ I=I-I0, wherein I0Exist for sensor
Initial current in air, I are electric current of the sensor after contact target gas molecule ammonia.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
Embodiment 1:
(1) poly- naphthalate (PI) material of flexibility that purchase commercial thickness is 50 μm, respectively with ethyl alcohol, acetone,
Water is successively cleaned by ultrasonic fexible film substrate surface 20 minutes, and drying obtains fexible film substrate；
(2) polycrystalline zinc germanate (Zn is prepared2GeO4) micro wire: by the zinc acetate (Zn (CH of 0.1g3COO)2·2H2O) and
The germanium of the oxygroup ([Ge (OEt) of 0.7g4]) be added in dimethylformamide (DMF) solution of 20mL, then it is added 5.7g's
Polyvinylpyrrolidone (PVP) stirs 15 hours under 1000rpm revolution.Mixed solution is added in the syringe of 50mL,
Electrostatic spinning solution is printed upon poly- naphthalate (PI) flexibility that step (1) obtains by near field electrostatic spinning method
In film-substrate, poly- naphthalate (PI) fexible film substrate that wherein syringe needle is obtained apart from step (1) away from
From for 1.5mm, electrostatic spinning voltage is 1.6kV, then calcines 15 hours under 380 DEG C of air atmospheres and obtains polycrystalline zinc germanate
(Zn2GeO4) micro wire, polycrystalline zinc germanate (Zn2GeO4) micro wire diameter be 12 μm, zinc germanate (Zn2GeO4) micro wire is more
Brilliant, and polycrystalline zinc germanate (Zn2GeO4) micro wire is made of nanoparticle, diameter of nano particles 30nm, as shown in Figure 2；
(3) the polycrystalline zinc germanate (Zn obtained in step (2)2GeO4) micro wire surface deposits to obtain by surface deposition
Two are separate, and with zinc germanate (Zn2GeO4) micro wire silver-colored (Ag) electrode of the perpendicular strip of radial direction, strip
Spacing is 60 μm between shape silver (Ag) electrode；Thickness of electrode is 100nm, to obtain of the present invention based on polycrystalline zinc germanate
(Zn2GeO4) micro wire grain boundary effect room temperature flexible gas sensor.
Embodiment 2
(1) poly- naphthalate (PI) material of flexibility that purchase commercial thickness is 50 μm, respectively with ethyl alcohol, acetone,
Water is successively cleaned by ultrasonic fexible film substrate surface 20 minutes, and drying obtains fexible film substrate；
(2) polycrystalline indium sesquioxide (In is prepared2O3) micro wire: by the indium nitrate (In (NO) of 0.1g3·6H2) and 3.0g O
Polyvinylpyrrolidone (PVP) be added in the water of 26mL and the mixed solution of ethyl alcohol (volume ratio 5:8), then 500rpm
It is stirred 15 hours under revolution.Mixed solution is added in the syringe of 50mL, by near field electrostatic spinning method by Static Spinning
Silk solution be printed upon on poly- naphthalate (PI) fexible film substrate that step (1) obtains, wherein syringe needle away from
Poly- naphthalate (PI) the fexible film substrate distance obtained from step (1) is 1.5mm, and electrostatic spinning voltage is
Then 1.6kV is calcined 2 hours under 400 DEG C of air atmospheres and is obtained polycrystalline indium sesquioxide (In2O3) micro wire；Polycrystalline three aoxidizes
Two indium (In2O3) micro wire diameter be 10 μm, indium sesquioxide (In2O3) micro wire is polycrystalline, and polycrystalline indium sesquioxide
(In2O3) micro wire is made of nanoparticle, diameter of nano particles 40nm；
(3) the polycrystalline indium sesquioxide (In obtained in step (2)2O3) micro wire surface deposited by surface deposition
It is separate to two, and with zinc germanate (Zn2GeO4) micro wire silver-colored (Ag) electrode of the perpendicular strip of radial direction, it is long
Spacing is 60 μm between strip silver (Ag) electrode；Thickness of electrode is 100nm, to obtain of the present invention based on three oxygen of polycrystalline
Change two indium (In2O3) micro wire grain boundary effect room temperature flexible gas sensor.
Embodiment 3
(1) poly- naphthalate (PI) material of flexibility that purchase commercial thickness is 50 μm, respectively with ethyl alcohol, acetone,
Water is successively cleaned by ultrasonic fexible film substrate surface 20 minutes, and drying obtains fexible film substrate；
(2) polycrystalline Zinc oxide (ZnO) micro wire is prepared: by the zinc acetate (Zn (CH of 1.5g3COO)2·2H2) and 2.0g O
Polyvinylpyrrolidone (PVP) is added in the aqueous solution of 20mL, is then stirred 20 hours under 420rpm revolution.By mixed solution
Be added in the syringe of 50mL, by near field electrostatic spinning method by electrostatic spinning solution be printed upon that step (1) obtains it is poly-
On naphthalate (PI) fexible film substrate, poly- dioctyl phthalate second two that wherein syringe needle is obtained apart from step (1)
Alcohol ester (PI) fexible film substrate distance is 1.0mm, and electrostatic spinning voltage is 2.0kV, is then calcined under 400 DEG C of air atmospheres
Obtain within 2 hours polycrystalline Zinc oxide (ZnO) micro wire；The diameter of polycrystalline Zinc oxide (ZnO) micro wire is 5 μm, and zinc oxide (ZnO) is micro-
Rice noodles are polycrystallines, and polycrystalline Zinc oxide (ZnO) micro wire is made of nanoparticle, diameter of nano particles 15nm；
(3) it deposits to obtain two by surface deposition in polycrystalline Zinc oxide (ZnO) the micro wire surface that step (2) obtains
It is separate, and with zinc germanate (Zn2GeO4) micro wire silver-colored (Ag) electrode of the perpendicular strip of radial direction, strip silver
(Ag) spacing is 60 μm between electrode；Thickness of electrode is 100nm, to obtain of the present invention based on polycrystalline Zinc oxide
(ZnO) the room temperature flexible gas sensor of micro wire grain boundary effect.
Polycrystalline zinc germanate (Zn2GeO4) micro wire room temperature flexible gas sensor performance test
The 4200-SCS semiconductor analysis instrument of U.S.'s Keithley company production is chosen in air-sensitive performance test, by device both ends electricity
Pole is connected by conducting wire with test equipment, and sensitive layer surface and under test gas occurs by being exposed in object gas ammonia gas
Redox reaction captures electronics, so that the electric current of device changes.Polycrystalline zinc germanate (Zn2GeO4) micro wire has
Typical grain boundary structure, as shown in figure 3, the physical and chemical performance of sensitive layer can be effectively improved.With based single crystal material
Flexible gas sensor is compared, and polycrystalline zinc germanate (Zn is based on2GeO4) device of micro wire shows target gas molecules ammonia
High inspiration characteristic, as shown in figure 4, sensitivity is 6.5 times of single crystal device to the object gas ammonia of 100ppm.Pass through
DFT calculates (Fig. 5) and obtains, target gas molecules and polycrystalline zinc germanate (Zn2GeO4) intermolecular distance on micro wire surface is far smaller than
Monocrystal material surface, and adsorption energy is greater than absorption of the monocrystal material to gas, illustrates based on polycrystalline zinc germanate (Zn2GeO4) micron
The device of line shows a high activity to object gas ammonia.By quantitative mechanical performance and linear element theory analysis, such as
Shown in Fig. 6, it is shown as polycrystalline zinc germanate (Zn2GeO4) Young's modulus of micro wire is 0.4GPa, far smaller than monocrystal material is said
Bright polycrystalline zinc germanate (Zn2GeO4) micro wire have better mechanical flexibility.Pass through performance test (Fig. 7 institute under being bent to it
Show), the sensitivity of 200ppm object gas ammonia is reduced there is no apparent, sensor is to detection target gas molecules ammonia
With a good mechanical stability.
Similar result can also obtain in embodiment 2 and embodiment 3 again, as shown in figure 8, being based on polycrystalline indium sesquioxide
(In2O3) gas sensor of micro wire and polycrystalline Zinc oxide (ZnO) micro wire has a high spirit to object gas ammonia
Sensitivity.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment
Content.So all do not depart from the lower equivalent or modification completed of spirit disclosed in this invention, the model that the present invention protects is both fallen within
It encloses.
Claims (6)
1. a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect, it is characterised in that: by flexibility
Film-substrate, polycrystalline micro wire and electrode composition, polycrystalline micro wire are located at fexible film substrate, electrode for strip structure and
On polycrystalline micro wire, the both ends of polycrystalline micro wire be separately connected electrode and electrode perpendicular to polycrystalline micro wire radial direction side
To；And fexible film substrate is the poly- naphthalate of flexible material, polycrystalline micro wire is with highly sensitive and fast-response speed
The broad stopband metal oxide semiconductor material of degree.
2. a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect as described in claim 1,
It is characterized by: broad stopband metal oxide semiconductor material is zinc germanate, indium sesquioxide or zinc oxide.
3. a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect as described in claim 1,
It is characterized by: polycrystalline micro wire is made of nanoparticle, the diameter of the nanoparticle is 5~50nm, and the polycrystalline is micro-
The diameter of rice noodles is 3~15 μm.
4. a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect as described in claim 1,
It is characterized by: fexible film substrate with a thickness of 40~80 μm.
5. a kind of room temperature high-performance flexible gas sensor based on polycrystalline micro wire grain boundary effect as described in claim 1,
It is characterized by: strip shaped electric poles are silver electrode, the spacing between silver electrode is 20~100 μm, electrode with a thickness of 80~
150nm。
6. a kind of room temperature high-performance flexible gas based on polycrystalline micro wire grain boundary effect described in Claims 1 to 5 any one
The preparation method of body sensor, its step are as follows:
(1) ethyl alcohol, acetone, water is used successively to be cleaned by ultrasonic 10~30 points of surface respectively the poly- naphthalate of flexible material
Clock, drying obtain fexible film substrate；
(2) polyvinylpyrrolidone of 0.05~2.0g metallic oxide precursor object and 0.5~10.0g is added to 10~50mL
In mixed solution, is stirred 6~30 hours under 300~1500rpm revolution, obtain electrostatic spinning solution；Then by the Static Spinning
Silk solution is added in the syringe of 30~100mL, and electrostatic spinning solution is printed upon step by near field electrostatic spinning method
(1) on the poly- naphthalate fexible film substrate obtained, flexible thin that wherein syringe needle is obtained apart from step (1)
The distance of film substrate is 0.5~2.0mm, and electrostatic spinning voltage is 1~3kV, then calcines 1 under 300~400 DEG C of air atmospheres
~20 hours, obtain polycrystalline metal oxide micro wire；
(3) surface of the polycrystalline metal oxide micro wire obtained in step (2) by surface deposition deposit to obtain two that
This is discrete, and the strip silver electrode perpendicular with the radial direction of polycrystalline metal oxide micro wire, to obtain based on polycrystalline
The room temperature flexible gas sensor of micro wire grain boundary effect.
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| CN110108759A (en) * | 2019-05-14 | 2019-08-09 | 电子科技大学 | It is a kind of based on polyaniline/metal oxide semiconductor nano compound film breathing ammonia gas sensor and preparation method thereof |
| CN113325041A (en) * | 2021-05-31 | 2021-08-31 | 吉林大学 | DMMP sensor based on gold-modified oxygen vacancy-rich tin dioxide and preparation method thereof |
| CN113325041B (en) * | 2021-05-31 | 2022-10-04 | 吉林大学 | DMMP sensor based on gold-modified oxygen vacancy-rich tin dioxide and preparation method thereof |
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