CN105136869B - Polyaniline/ferric oxide nano composite resistance type material sensors and preparation method thereof - Google Patents
Polyaniline/ferric oxide nano composite resistance type material sensors and preparation method thereof Download PDFInfo
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- CN105136869B CN105136869B CN201510506166.5A CN201510506166A CN105136869B CN 105136869 B CN105136869 B CN 105136869B CN 201510506166 A CN201510506166 A CN 201510506166A CN 105136869 B CN105136869 B CN 105136869B
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Abstract
The invention discloses a kind of polyaniline/ferric oxide nano composite resistance type sensor and preparation method thereof, the gas sensor includes the ceramic matrix set gradually, interdigital gold electrode and gas sensitive, described gas sensitive material is made up of polyaniline/ferric oxide nano compound, sensor can be greatly improved at room temperature to the response sensitivity of gas in the p n knot effects that wherein p types polyaniline is formed with n type iron oxide interface, accelerate response, and improve stability, and polyaniline can significantly reduce the resistance of element, conveniently realize the test for sensor resistance response characteristic.The sensor has very high response sensitivity, good recovery to ammonia at room temperature, and responds comparatively fast, and stability is good, can be widely applied to the accurate measurement and control of ammonia concentration in industrial and agricultural production process and atmospheric environment.Present invention also offers the method for preparing the sensor, this method technique is simple, cost is low, is particularly suitable for producing in batches.
Description
Technical field
The present invention relates to sensor field, and in particular to a kind of hypersensitivity polyaniline/iron oxide resistor-type material gas
Body sensor and preparation method thereof.
Background technology
Metal oxide semiconductor has great scientific research value and actual techniques application value.More conventional has
SnO2、ZnO、TiO2、Fe2O3Deng.These metal oxides are mostly the n-type multifunctional semiconductor with wide energy band, are had very excellent
Different electrical properties, photocatalysis property, electrochemical properties, optical and electrical properties, gas sensing, humidity sensor, optical property etc.
（L.b. Luo, F.x. Liang and J.s. Jie, Nanotechnology, 2011, 22, 485701; M.
Batzill, K. Katsiev, J. M. Burst, U. Diebold, A. M. Chaka and B. Delley,
Physical Review B, 2005, 72, 165414; H. Zhang, Q. He, X. Zhu, D. Pan, X. Deng
and Z. Jiao, CrystEngComm, 2012, 14, 3169-3176.）.Due to these excellent properties, research work
Persons expand the research in every field application, such as solar cell, super capacitor to the metal oxide semiconductor
Device, optoelectronic device, transistor, lithium ion battery, humidity sensor and gas sensor etc..
The preparation method for the semiconductor oxide ferrum nano material that presently, there are mainly has atomic layer deposition method, thermal evaporation skill
Art, calcining, electrochemical synthesis, sol-gel process, chemical vapour deposition etc., it is more special that these methods generally require
Technology, large-scale instrument, high-temperature process etc., cost is higher and energy resource consumption is larger.In addition, the semiconductor oxide being prepared
Ferrum nano material is generally required after disperse again, redeposited in could be used to prepare electronic device in substrate.Therefore, partly lead
Body iron oxide nano material prepares intermediate demand to device and carries out transfer step, so, the process for not only increasing device preparation,
And if nano material dispersed and deposition control are bad in preparation process, can also influence the uniformity of device, and
Production cost can be increased.In addition, on the one hand, the preparation method of conventional semiconductor oxide ferrum nano material is usually required at high temperature
Reason, and flexible organic and polymer material substrate can not often be resistant to high temperature, which has limited the use of flexible polymer substrate, gives
The development and application of flexible photoelectric device bring difficulty.On the other hand, process is disperseed and deposited above the device of preparation again
Often exist and imperfect problem is combined between nano material and substrate, it larger contact impedance and influence is present
Charge transfer process, the performance of the photoelectric functional device of preparation will be adversely affected.
But it is not generally especially high to use the gas sensitivity prepared by these conductor oxidates, such as I
Before patent application（The method of low-temperature original position growth nanostructured metal oxide semiconductor and application, CN104807859A）
In the tin ash mentioned and polypyrrole composite gas sensor sensitivity only less than 80%, and to the choosing of organic vapor
The detection of selecting property is had any problem.The present invention proposes the gas sensor of hypersensitivity, and have its preparation process for these deficiencies
Body, instantiation, and obtained sensor has extraordinary selectivity.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide polyaniline/ferric oxide nano composite resistance type material sensors and
Its preparation method.
The present invention adopts the following technical scheme that：
A kind of polyaniline/ferric oxide nano composite resistance type material sensors, including ceramic matrix, interdigital gold electrode are gentle
Quick material, connects leaded on described interdigital gold electrode, has interdigital gold electrode in described ceramic matrix surface deposition,
The ceramic matrix and interdigital gold electrode surfaces deposition have gas sensitive, and described gas sensitive is by polyaniline/ferric oxide nano
Compound forms.
The interdigital gold electrode of described ceramic matrix surface deposition is 5~16 pairs, and the interdigital width of interdigital gold electrode is 20
~200 μm, interdigital gap is 20~200 μm.
The thickness of described gas sensitive is 50~600 nm.
Described polyaniline/ferric oxide composite material is the oxidation obtained by electrostatic spinning auxiliary water heat-treating methods
Prepared by iron nanometer sheet and the water-soluble polyaniline of polystyrolsulfon acid doping.
A kind of preparation method according to the sensor, specifically comprise the following steps：
1) prepare semiconductor oxide iron presoma and the mixed solution of spinning-aid agent obtains spinning solution, spinning solution is passed through quiet
The method of Electrospun forms nanofibres deposit to after substrate surface, naturally dry；
2) deposition obtained in the step 1) has the substrate of nanofiber by hydro-thermal process, obtains in substrate
The semiconductor oxide iron with nanostructured of growth in situ；
3) polyaniline adulterated in the resulting strata styrene sulfonic acid of semiconductor oxide iron surface dip-coating one, obtains institute
State sensor.
Step 1）Described in semiconductor oxide iron precursor concentration be 10 ~ 300 mg/mL, the spinning-aid agent concentration is 40 ~
100 mg/mL, flow velocity preferably 0.1 ~ 10 mL/h of the electrostatic spinning；Receive distance preferably 5 ~ 30 cm；Spinning voltage is excellent
Elect 5 ~ 30 kV as；It is preferably 0.5 ~ 60 min to receive the time.
Step 2）Described in hydro-thermal process temperature be preferably 120 ~ 180 DEG C；Hydrothermal conditions are preferably 6 ~ 24 h.
The beneficial effects of the invention are as follows：
1. the invention provides a kind of equipment is simple, step is convenient, energy consumption is low, in any substrate semiconductor-on-insulator iron oxide
Growth in situ, especially growth in situ on a flexible substrate, the semiconductor oxide iron nanometer for the advantages that being easy to prepare flexible device
The growing method of structure, the semiconductor oxide iron application field has been widened significantly, turn into the semiconductor oxide iron each
A kind of necessary means of the preparation nanostructured of application field.
2. the preparation method is that low-temperature epitaxy（120-180℃）, this method has that controllability is good, reaction condition
Gently, the semiconductor oxide iron nanostructure growth is uniform, and energy-output ratio is less, can reduce environmental pollution etc. many excellent
Point, particularly, cryogenic conditions are especially suitable for the direct easy preparation of flexible device.
3. the preparation method is that growth in situ, can realize nanostructured semiconductor oxide iron material in difference
Preparation in situ in substrate, then can reduce preparation section, directly obtain required photoelectric functional device, and the original of nano material
Position growth is also beneficial to promote the combination of material and substrate, reduces contact impedance, promotes electric charge transfer, improves stability etc..From
And promote application of the nanostructured semiconductor oxide iron in function element.The semiconductor oxide iron nanostructured and substrate,
It is Ohmic contact between semiconductor oxide iron nanostructured and conducting polymer, prepared sensor can be effectively improved
Sensitivity, repeatability and stability.
4. the present invention uses method of electrostatic spinning, in-situ deposition contains the nanofiber of metal salt directly in substrate, then
Pass through lower temperature（Less than 180 DEG C）Hydro-thermal process so that contained metal salt converted in-situ is nano junction in nanofiber
Structure iron oxide.Hereby it is achieved that nanostructured iron oxide in water-heat process in the direct low-temperature original position growth of substrate surface, and
Significantly enhance its binding ability with substrate.
5. the present invention prepared the semiconductor oxide iron nanostructured comprising this method with conducting polymer it is compound after
With very superior gas sensitization performance（High sensitivity, recovery are good, selectivity is good）The advantages that gas sensor.
6. the I-V curve of the semiconductor oxide iron nanostructured and conducting polymer prepared by the present invention shows described partly to lead
Strong interaction between body ferric oxide nano structure and conducting polymer be present, this synergy can be utilized to improve
The charge migration of electric conductivity and promotion at room temperature at room temperature, there is very close synergy in the two, while with tunnelling
Effect, and between the semiconductor oxide iron nanostructured and substrate, semiconductor oxide iron nanostructured and conducting polymer
For Ohmic contact.Especially, the interface of p-type polyaniline and n-type ferric oxide nano piece forms p/n junction structures, with the detection gas such as ammonia
After body molecular action, cause the increase of dissipation layer width, resistance variations increase, while the activation energy and thing of gas absorption can be reduced
Adsorption enthalpy is managed, so that it is significantly improved for the response sensitivity of gas.
Brief description of the drawings
Fig. 1 is the surface topography by the growth in situ semiconductor oxide iron nanostructured obtained by the embodiment of the present invention
Stereoscan photograph；
Fig. 2 is shone by the ESEM of the surface topography of the gas sensor functional layer obtained by the embodiment of the present invention
Piece；
Fig. 3 is response test result figure of the sensor for low concentration ammonia of preparation of the embodiment of the present invention；
Fig. 4 is round robin test result figure of the embodiment of the present invention to 5 ppm ammonias；
Fig. 5 is selective result figure of the embodiment of the present invention to other common organic vapors,
Note：NH3For ammonia, concentration 10.7ppm；DEA is diethylamine, concentration 200ppm；EtOH is ethanol, and Ethe is
Ether, Acetone are acetone, and Methanol is methanol, and THF is tetrahydrofuran, and n-Hexane is n-hexane, and concentration is
5000ppm。
Embodiment
Further illustrate that method part of the invention is by electrostatic spinning and hydro-thermal process below in conjunction with drawings and examples
Two steps collectively constitute, and the electrostatic spinning spinning solution is that spinning-aid agent and iron oxide presoma collectively constitute.Described electrostatic
Spining technology enables to semiconductor oxide iron presoma to be deposited in the form of nanofiber on substrate surface, hydro-thermal process skill
Art can cause semiconductor oxide iron presoma to change in the presence of pressure and temperature, go out in substrate surface growth in situ
Semiconductor oxide iron nanostructured.Two steps one in front and one in back, complement each other, indispensable.The semiconductor oxygen that growth in situ goes out
Change iron nanostructured and substrate contact is good, Ohmic contact property is presented, it is especially soft particularly useful for making gas sensor
Property gas sensor.
Embodiment 1
The preparation method of the method for the present invention, comprises the following steps：
1. prepare the mixed solution of ferric trichloride and polyvinyl butyral resin, i.e. spinning solution, the concentration of the ferric trichloride
For 50 mg/mL, polyvinyl butyral resin concentration is 30 mg/mL；Wherein ferric trichloride can be that any one can be dissolved in spinning
Liquid solvent, and have with spinning-aid agent the metal salt of excellent compatibility, including but not limited to ferric trichloride, ferric nitrate；Polyvinyl alcohol contracts
Butyraldehyde can be any one or it is a variety of can spinning polymer, including but not limited to polyvinyl butyral resin, polyvinylidene fluoride
Alkene, polyvinyl chloride, polyvinyl alcohol；
2. by step 1. in electrostatic spinning liquid in flow velocity be 0.3 mL/h；It is 15 cm to receive distance；Spinning voltage is 8
kV；Receive and deposited under the electrospinning conditions that the time is 3 min in the form of nanofiber in ceramic bases；Wherein ceramic base
Bottom can be flexible material or rigid material, including but not limited to polyethylene terephthalate, polytetrafluoroethylene (PTFE), poly- third
Alkene, Kynoar, glass, ceramics, silicon chip, ito glass；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 135 DEG C the h of hydro-thermal process 8, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Using it is described 1.~4. the step of can film forming on a ceramic substrate, the biography as functional layer in this way is made
Sensor；The sensor surface figure as shown in figure 1, obtained semiconductor oxide iron nanostructured surface pattern as shown in Fig. 2
Semiconductor oxide iron nanostructured is evenly distributed, and size is homogeneous, and obtained sensor has excellent gas-sensitive property, to low dense
The response diagram for spending (1-10 ppm) ammonia is as shown in Figure 4, it can be seen that the ammonia concentration in methods described energy Sensitive Detection environment
Information, under 10 ppm concentration, using formula S=（R1-R0）/R0X 100% can calculate sensitivity S=3000% (note：R1It is logical
Enter the resistance value after ammonia, R0To be passed through the resistance value before ammonia).In addition, the response cycle figure of methods described as shown in figure 4,
It can be seen that it has good stability and recovery.To shown in the selective result figure 5 of other common organic vapors.
Embodiment 2
1. preparing the mixed solution of ferric nitrate and polyvinyl butyral resin, i.e. spinning solution, the concentration of the ferric nitrate is 10
Mg/mL, polyvinyl butyral resin concentration are 100 mg/mL；
2. step 1. in electrostatic spinning liquid in flow velocity be 0.1 mL/h；It is 5 cm to receive distance；Spinning voltage is 5 kV；
Receive and polyethylene terephthalate base is deposited in the form of nanofiber under the electrospinning conditions that the time is 30 min
On bottom；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 180 DEG C the h of hydro-thermal process 24,
Obtaining growth in situ has the substrate of semiconductor oxide iron nanostructured, and method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Resistance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 170 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 2900%.
Embodiment 3
1. preparing the mixed solution of ferric nitrate and polyvinyl chloride, i.e. spinning solution, the concentration of the ferric nitrate is 300 mg/
ML, polyvinyl chloride concentration are 40 mg/mL；
2. by step 1. in electrostatic spinning liquid in flow velocity be 1 mL/h；It is 30 cm to receive distance；Spinning voltage is 30
kV；Receive and deposited under the electrospinning conditions that the time is 30 min in the form of nanofiber in polytetrafluoroethylene (PTFE) substrate；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 120 DEG C the h of hydro-thermal process 6, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 200 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 2900%.
Embodiment 4
1. preparing the mixed solution of ferric nitrate and polyvinyl chloride, i.e. spinning solution, the concentration of the ferric nitrate is 300 mg/
ML, polyvinyl chloride concentration are 40 mg/mL；
2. by step 1. in electrostatic spinning liquid in flow velocity be 10 mL/h；It is 30 cm to receive distance；Spinning voltage is 30
kV；Receive and deposited under the electrospinning conditions that the time is 0.5 min in the form of nanofiber in polypropylene substrate；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 180 DEG C the h of hydro-thermal process 6, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 100 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 3100%.
Embodiment 5
1. preparing the mixed solution of ferric trichloride and polyvinyl chloride, i.e. spinning solution, the concentration of the ferric trichloride is 300
Mg/mL, polyvinyl chloride concentration are 40 mg/mL；
2. by step 1. in electrostatic spinning liquid in flow velocity be 1 mL/h；It is 30 cm to receive distance；Spinning voltage is 30
kV；Receive and deposited under the electrospinning conditions that the time is 0.5 min in the form of nanofiber in Kynoar substrate；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 120 DEG C the h of hydro-thermal process 24,
Obtaining growth in situ has the substrate of semiconductor oxide iron nanostructured, and method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 150 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 3000%.
Embodiment 6
1. preparing the mixed solution of ferric trichloride and vinylidene, i.e. spinning solution, the concentration of the ferric trichloride is 85
Mg/mL, poly- Kynoar concentration are 40 mg/mL；
2. step 1. in electrostatic spinning liquid in flow velocity be 0.2 mL/h；It is 15 cm to receive distance；Spinning voltage is 8
kV；Receive and deposited under the electrospinning conditions that the time is 3 min in the form of nanofiber in substrate of glass；
3. step 2. in obtained by the deposition substrate that has nanofiber dry after at 135 DEG C the h of hydro-thermal process 8, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 200 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 3050%.
Embodiment 7
1. prepare the mixed solution of ferric trichloride and polyvinyl butyral resin, i.e. spinning solution, the concentration of the ferric trichloride
For 85 mg/mL, polyvinyl butyral resin concentration is 40 mg/mL；
2. step 1. in electrostatic spinning liquid in flow velocity be 0.2 mL/h；It is 15 cm to receive distance；Spinning voltage is 8
kV；Receive and deposited under the electrospinning conditions that the time is 3 min in the form of nanofiber in silicon chip substrate；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 135 DEG C the h of hydro-thermal process 8, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 100 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 3100%.
Embodiment 8
1. preparing the mixed solution of ferric nitrate and polyvinyl butyral resin, i.e. spinning solution, the concentration of the ferric nitrate is 85
Mg/mL, polyvinyl butyral resin concentration are 40 mg/mL；
2. step 1. in electrostatic spinning liquid in flow velocity be 0.2 mL/h；It is 15 cm to receive distance；Spinning voltage is 8
kV；Receive and deposited under the electrospinning conditions that the time is 3 min in the form of nanofiber in ito glass substrate；
3. by step 2. in obtained by the deposition substrate that has nanofiber dry after at 135 DEG C the h of hydro-thermal process 8, obtain
There is the substrate of semiconductor oxide iron nanostructured to growth in situ, method is made；
4. by the step 3. obtained strata aniline of substrate dip-coating one with the semiconductor oxide iron nanostructured, system
Obtain gas sensor.
Impedance of the resulting method under the conditions of low concentration (≤10 ppm) is relatively low, less than 10 kilo-ohms, have to ammonia compared with
Good response, under 10 ppm concentration, its sensitivity reaches 3000%.
Above example is only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that reading
After the content of the invention lectured, those skilled in the art can make various changes or modifications to the present invention, these shapes of equal value
Formula equally falls within the application appended claims limited range.
Claims (4)
- A kind of 1. polyaniline/ferric oxide nano composite resistance type material sensors, it is characterised in that：Including ceramic matrix, interdigital Gold electrode and gas sensitive, connect leaded on described interdigital gold electrode, have fork in described ceramic matrix surface deposition Refer to gold electrode, have a gas sensitive in the ceramic matrix and interdigital gold electrode surfaces deposition, described gas sensitive by polyaniline/ Ferric oxide nano compound forms；The interdigital gold electrode of described ceramic matrix surface deposition is 5~16 pairs, and the interdigital width of interdigital gold electrode is 20~200 μm, interdigital gap is 20~200 μm；The thickness of described gas sensitive is 50~600 nm.
- 2. a kind of preparation method of polyaniline according to claim 1/ferric oxide nano composite resistance type material sensors, its It is characterised by：Described polyaniline/ferric oxide composite material is the oxygen obtained by electrostatic spinning auxiliary water heat-treating methods Prepared by change iron nanometer sheet and the water-soluble polyaniline of polystyrolsulfon acid doping, specifically comprise the following steps：1) prepare semiconductor oxide iron presoma and the mixed solution of spinning-aid agent obtains spinning solution, spinning solution is passed through into Static Spinning The method of silk forms nanofibres deposit to after substrate surface, naturally dry；2) deposition obtained in the step 1) has the substrate of nanofiber by hydro-thermal process, obtains in situ in substrate The semiconductor oxide iron with nanostructured of growth；3) polyaniline adulterated in the resulting strata styrene sulfonic acid of semiconductor oxide iron surface dip-coating one, obtains the biography Sensor.
- 3. the preparation method of polyaniline/ferric oxide nano composite resistance type material sensors according to claim 2, its feature It is：Step 1）Described in semiconductor oxide iron precursor concentration be 10 ~ 300 mg/mL, the spinning-aid agent concentration is 40 ~ 100 Mg/mL, flow velocity preferably 0.1 ~ 10 mL/h of the electrostatic spinning；Receive distance preferably 5 ~ 30 cm；Spinning voltage is preferably 5 ~30 kV ；It is preferably 0.5 ~ 60 min to receive the time.
- 4. the preparation method of polyaniline/ferric oxide nano composite resistance type material sensors according to claim 2, its feature It is：Step 2）Described in hydro-thermal process temperature be preferably 120 ~ 180 DEG C；Hydrothermal conditions are preferably 6 ~ 24 h.
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| CN107607590B (en) * | 2017-08-30 | 2019-11-08 | 吉林大学 | Based on the flower-shaped WO of PANI@3The flexible NH of sensitive material3Sensor and its application |
| CN108299641B (en) * | 2018-02-11 | 2020-11-03 | 黑龙江大学 | Preparation method of polyaniline/iron oxide composite material |
| CN109115839B (en) * | 2018-07-03 | 2020-11-20 | 华东师范大学 | In-tube growth doped or filled mesoporous polyaniline gas sensor and preparation method thereof |
| CN114917771B (en) * | 2022-04-28 | 2023-09-29 | 浙江大学 | Hollow fiber membrane flexible humidity sensor and efficient preparation method thereof |
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