CN101042363A - polyaniline nanometer oxidate compound film micro-gas sensors array and method for making same - Google Patents
polyaniline nanometer oxidate compound film micro-gas sensors array and method for making same Download PDFInfo
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Abstract
This invention discloses one polyaniline or nanometer oxidation compound film gas sensor array, which comprises more than two compound film micro gas sensor unit integrated into one same base. The invention is characterized by the following: the said compound micro gas sensor unit comprises base slice, cross electrode, the compound film and conductive wires; the compound film has aniline single part, mixture acid liquid, oxidation acid and disperse agent and inorganic oxidation gel or powder.
Description
Technical field
The present invention relates to organic-inorganic nanocomposite gas sensor field, be specifically related to polyaniline/nanometer oxidate compound film micro-gas sensors array and preparation method thereof.
Background technology
Gas sensor all has important application prospects at aspects such as environment measuring, chemical gas detection and food industry, and it is also imperative therefore to develop the high-performance sensors with high sensitivity, high selectivity and good stability.Everything has all proposed new higher requirement to the core-gas sensitive of gas sensor.Single inorganic semiconductor material or conducting polymer gas sensitive exist shortcomings such as the low and stability of low-response, poor selectivity, sensitivity is not good enough, and being undertaken compound by different modes the organic-inorganic gas sensitive is the effective ways that address these problems.Because Organic can be brought into play inorganic nano-particle self characteristics and interparticle cooperative effect, the advantage that has organic material itself again, therefore can improve the processability of material to a certain extent, change sensitivity, the selectivity of single gas sensitive, and obtain the new gas-sensitive property that homogenous material does not possess.The development of gas sensitive has at present presented by the trend of homogenous material to the compound substance development.
Conducting polymer materials such as polypyrrole, polythiophene and polyaniline have susceptibility to specific gas at normal temperatures.Wherein polyaniline is used widely and is become the conducting polymer materials that is hopeful to obtain at present practical application most with advantages such as its unique mechanism of doping effect, reversible oxidation-reduction characteristic, good stable and raw material are cheap and easy to get and in many-sides such as rechargeable battery, chemical sensors.Inorganic semiconductor nano particle and polyaniline are made nano composite material, its photoelectric properties and gas-sensitive property etc. are compared with pure polyaniline all and are changed to some extent, so polyaniline nano-composite material demonstrates tempting application prospect at aspects such as sensitive material, energy storage materials.
Relevant report and patent of invention about polyaniline composite material are more, and wherein application for a patent for invention prospectus CN 1718612A and CN 1821315A have reported inorganic oxide conductive powder/polyaniline conductive polymer material and polyaniline cladding titanium dioxide compound substance and preparation method thereof respectively.But the report of p-poly-phenyl amine compound substance concentrates on the preparation of compound substance mostly and characterizes at present, then report in the preparation of polyaniline laminated film and gas sensor application facet less, (Ram, M.K. such as Ram, Yavuz, O., Lahsangah, V., Aldissi.M., Sens.Actuators B, 2005,106:750) reported that polyaniline/tin ash (titania) self assembly laminated film is at room temperature to CO and SO
2Susceptibility, (A.Z.Sadek, W.Wlodarski, K.Shin such as A.Z.Sadek, R.Bkaner, K.Kalantar-zadeh, Nanotechnology, 2006,17:4488) reported based on the gas sensor of polyaniline/indium oxide compound substance, be mainly used in CO, H
2And NO
2Detection.Parvatikar etc. (N.Parvatikar, S.Jain, S.Khasim, M.Revansiddappa, S.V Bhoraskar, M.V.N.Ambika Prasad, Sens.Actuators B, 2006,114:599) reported the compound humidity sensor of polyaniline/tungsten oxide.
Yet though polyaniline/inorganic semiconductor compound substance is used for every performance that gas sensor can improve sensor, researchers such as A.Z.Sadek point out that the polyaniline composite material sensor still exists problems such as cross-sensitivity and poor stability.Gas sensor array is the effective way that solves the pure gas sensor decussation sensitivity.At present the gas sensor array of bibliographical information generally is by (i) commercial gas sensor (Santiago Marco, Arturo Ortega, Antonio Pardo, Josep Samitier, IEEE Transactionson Instrumentation and Measurement, 1998,47 (1): 316); (ii) based on different semiconductor materials or contain gas sensor (Dae-sik Lee, Duk-Dong Lee, the Sang-Woo Ban of the semiconductor material of different dopant, Minho Lee, Youn Tae Kim, IEEE Sensors Journal, 2002,2 (3): 1; Deng Junyong, Feng Yongjian, Wu Qinghai, sensor technology, 2002,21 (8): 44); (iii) based on the gas sensor of different polymkeric substance and polymkeric substance/carbon black composite material (Frank Zee, Jack W.Judy, Sens.Actuators B, 2001,72:120) wait gas sensor unit to constitute.Aspect the patent of invention of gas sensor array, application for a patent for invention prospectus CN 1542444A has reported the gas sensor array that is made of than different indium and tin oxide film gas sensors indium tin, be used to differentiate comprise several frequently seen indoor polluted gas such as benzene,toluene,xylene and methyl alcohol, application for a patent for invention prospectus CN 1635372A has reported that then electronic polymer field effect gas transducer array is to NO
XThe detection of mixed gas.But the research for preparing polyaniline/nanometer oxidate compound film gas sensor unit and make up gas sensor array with different nano-oxides does not then appear in the newspapers as yet, does not have the application of related invention patent yet.
Summary of the invention
Technical matters to be solved by this invention is how a kind of polyaniline/nanometer oxidate compound film micro-gas sensors array is provided, this array can solve the single semiconductor or the selective problems of conductive polymer sensors, has higher sensitivity simultaneously and responds recovery characteristics faster; The present invention also provides the preparation method of this array, and this preparation method is easy to operation.
Technical matters proposed by the invention is to solve like this: construct a kind of polyaniline/nanometer oxidate compound film micro-gas sensors array, it is to be integrated in the same substrate by the polyaniline more than 2/nanometer oxidate compound film micro-gas sensors unit to constitute, it is characterized in that: described polyaniline/nanometer oxidate compound film micro-gas sensors unit comprises substrate, interdigital electrode, polyaniline/nanometer oxidate compound film and conductive lead wire, wherein polyaniline/nanometer oxidate compound film has by following raw material and makes: aniline monomer, dopant acid solution, the oxygenant acid solution, spreading agent and inorganic oxide sol or powder.
According to polyaniline/nanometer oxidate compound film micro-gas sensors array provided by the present invention, it is characterized in that, at least comprise two dissimilar polyanilines/nanometer oxidate compound film micro-gas sensors unit in each array, the difference of this polyaniline/nanometer oxidate compound film micro-gas sensors unit is that its polyaniline/nanometer oxidate compound film made by following different raw material:
A, aniline monomer, dopant acid solution, oxygenant acid solution and nano titanic oxide sol;
B, aniline monomer, dopant acid solution, oxygenant acid solution and nano oxidized imperial mandate colloidal sol;
C, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nano tin dioxide powder;
D, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nano indium oxide powder;
E, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nanometer tungsten oxide powder.
According to polyaniline/nanometer oxidate compound film micro-gas sensors array provided by the present invention, it is characterized in that the mol ratio of aniline monomer and oxygenant is 1; Dopant acid solution is the hydrochloric acid solution of 2.0M; The weight percentage of inorganic oxide sol is 0.05～1%, and the mass ratio of inorganic oxide powder and aniline monomer is 0.020～0.030: 0.5～2; Described oxygenant is an ammonium persulfate; Described spreading agent is a neopelex.
According to polyaniline/nanometer oxidate compound film micro-gas sensors array provided by the present invention, it is characterized in that described substrate is the silicon chip of 5mm * 8mm, described interdigital electrode material is a gold, its electrode separation and width are 50 μ m.
A kind of preparation method of polyaniline/nanometer oxidate compound film micro-gas sensors array is characterized in that, may further comprise the steps:
(1), utilization standard semiconductor technology prepares interdigital electrode on substrate;
(2), partly adopt the polyaniline/nano-oxide composite sensing film of electrostatic force self assembly and in-situ polymerization sedimentation growth high electrical conductivity, draw lead at two electrode tips in interdigital electrode;
(3), the polyaniline/nanometer oxidate compound film micro-gas sensors unit that will use different nano-oxides to prepare is integrated in the same substrate and constitutes micro-gas sensors array.
Preparation method according to polyaniline/nanometer oxidate compound film micro-gas sensors array provided by the present invention, it is characterized in that, adopt the polyaniline/nano-oxide composite sensing film of electrostatic force self assembly and in-situ polymerization sedimentation growth high electrical conductivity may further comprise the steps in the step (2): 1. plane interdigital electrode formula device to be put into polydiene propyl ammonium chloride aqueous solution and soak 6～12min, take out the back and use deionized water wash, dry up with nitrogen again; 2. again substrate is immersed 7～13min in the poly (sodium 4-styrenesulfonate) solution, take out the back with deionized water wash and dry up; 3. temperature joins inorganic nanometer oxide colloidal sol or the powder of handling in the dopant acid solution in 0～25 ℃, and then aniline monomer is added wherein, at last oxidizing agent solution is added drop-wise to said mixture and reacts; 4. mixed liquor leaves standstill 3～10min, filters with organic filtrator; 5. the substrate after will handling is immersed in the filtrate, takes out behind 15～25min, dries naturally under the room temperature condition.
Preparation method according to polyaniline/nanometer oxidate compound film micro-gas sensors array provided by the present invention is characterized in that:
The disposal route of A, nano inorganic oxide powder is: neopelex is joined in the watery hydrochloric acid in proportion, and tin ash, indium oxide or tungsten oxide nano-powder are added in the back that stirs; This mixing suspension is high-speed stirred 10～30min at first, and then puts into supersonic wave cleaning machine sonic oscillation 20～40min;
The disposal route of B, nano inorganic oxide colloidal sol is: add a certain amount of deionized water dilution nano titanic oxide sol and nano oxidized imperial mandate colloidal sol, put into supersonic wave cleaning machine sonic oscillation 10～20min then.
Beneficial effect of the present invention is: set about from the organic-inorganic nanocomposite angle, in the process of chemical oxidising polymerisation polyaniline, add an amount of inorganic oxide Nano sol or powder, because nano particle plays a part original position adsorpting polymerization carrier, therefore aniline monomer is adsorbed on nanoparticle surface, the oxygenant trigger monomer carries out polymerization in nanoparticle surface, caused the limited growth of polyaniline around nano particle, thereby make the big molecule of polyaniline or its segment more regular in order in the arrangement of nanoparticle surface, improved the conductivity of film, so the output signal of the polyaniline/nanometer oxidate compound film micro-gas sensors array of the present invention's proposition is easy to gather and further handle.Simultaneously, polyaniline/nanometer oxidate compound film microsensor response is fast, easily recovers, and is highly sensitive.By selecting different nano-oxides to form polyaniline laminated film gas sensor array, can satisfy the accurately detection and Identification fast of mixed gas.The present invention is the cell formation gas sensor array with polyaniline/nanometer oxidate compound film micro-gas sensors, the binding pattern recognition technology has solved the problems such as resolving power difference of the baseline wander of single polyaniline laminated film gas sensor, mixed gas well.Preparation method of composite film is rationally simple, easily operation.
Description of drawings
Fig. 1 be micro-gas sensors array provided by the present invention floor map;
Fig. 2 is the floor map of gas sensor unit provided by the present invention;
Wherein, wherein, the 1st, array substrate; The 2nd, gas sensor unit; The 21st, substrate; The 22nd, interdigital electrode; The 23rd, polyaniline/nanometer oxidate compound film; The 24th, solder joint; The 25th, lead-in wire.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and specific embodiment.
As Fig. 1, shown in Figure 2, polyaniline/nanometer oxidate compound film micro-gas sensors array unit 2 that the present invention proposes is by substrate 21, interdigital electrode 22, polyaniline/nano-oxide composite sensing film 23 and conduction exit (comprising lead-in wire 25 and solder joint 24) are formed, substrate is the silicon chip of 5mm * 8mm, utilization standard semiconductor technology prepares interdigital electrode on silicon chip, electrode material is a gold, electrode separation and width are 50 μ m, partly adopt the polyaniline/nano-oxide composite sensing film of electrostatic force self assembly and in-situ polymerization sedimentation growth high electrical conductivity in interdigital electrode, draw lead at two electrode tips.Polyaniline/nanometer oxidate compound film micro-gas sensors the unit of the different nano-oxides of utilization preparation is integrated in the same substrate 1 constitutes micro-gas sensors array.
Polyaniline/nanometer oxidate compound film that the present invention proposes has following raw material: aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and inorganic oxide sol or powder.Wherein the mol ratio of aniline monomer and oxygenant is 1; Dopant acid solution is the hydrochloric acid solution of 2.0M; Described inorganic oxide sol or powder refer to nano titanic oxide sol, nano oxidized imperial mandate colloidal sol, nano tin dioxide powder, nano indium oxide powder and nanometer tungsten oxide powder; The weight ratio of preferred oxide sol is 0.1%, and the mass ratio of preferred oxide powder and aniline monomer is 0.025: 1; Described oxygenant refers to ammonium persulfate; The spreading agent of indication is a neopelex.
The process that utilization electrostatic force self assembly that the present invention proposes and in-situ polymerization sedimentation prepare laminated film is as follows: at first plane interdigital electrode formula device is put into polydiene propyl ammonium chloride aqueous solution and soak 6～12min (optimum 10min or 8min or 11min), take out the back and use deionized water wash, dry up with nitrogen again; Again substrate is immersed 7～13min (optimum 10min or 8min or 11min) in certain density poly-(sodium p styrene sulfonate) solution, take out the back with deionized water wash and dry up.Simultaneously, at a certain temperature, inorganic nanometer oxide colloidal sol or the powder of handling joined in the dopant acid solution, and then aniline monomer is added wherein, at last oxidizing agent solution is added drop-wise to said mixture and reacts.After mixed liquor leaves standstill some minutes, with organic filtrator filtration of 0.45 μ m.Substrate after handling is immersed in the filtrate, takes out behind the certain hour, dry naturally under the room temperature condition.
Nano sol and powder will pass through certain processing.The disposal route of nano-powder is: the disposal route of nano-powder is: neopelex is joined in the watery hydrochloric acid in proportion, and tin ash, indium oxide or tungsten oxide nano-powder are added in the back that stirs; This mixing suspension is high-speed stirred 10～30min (optimum has 20min or 15min or 25min) at first, and then puts into supersonic wave cleaning machine sonic oscillation 20～40min (optimum 30min or 25 or 35min); The disposal route of Nano sol is: add a certain amount of deionized water dilution nano titanic oxide sol and nano oxidized imperial mandate colloidal sol, put into supersonic wave cleaning machine sonic oscillation 10～20min (optimum 15min or 18min) then.
According to the present invention, oxidative polymerization is carrying out under 0～25 ℃ (optimum 10 ℃ or 8 ℃ or 12 ℃ or 25 ℃).The mixed solution time of repose is 3～10min (optimum 6min or 8min or 4min etc.), and substrate immerses time 15～25min (optimum 15min or 20min or 18min etc.).
Below be specific embodiments of the invention:
At first plane interdigital electrode formula unit component is as shown in Figure 2 carried out surface preparation.Interdigital electrode formula device is put into 1% polydiene propyl ammonium chloride aqueous solution soaked 10 minutes, take out the back and use deionized water wash, dry up with nitrogen again; Again substrate was immersed in poly-(sodium p styrene sulfonate) solution of 2mg/mL 10 minutes, and took out the back with deionized water wash and dry up.
Get 0.2mL TiO with transfer pipet
2Nano sol adds deionized water and is diluted to 0.1wt%; Ultrasonic 15min.Take by weighing the 0.1254g ammonium persulfate, be dissolved in the hydrochloric acid of 10mL2 mol/L.Temperature is in the time of 10 ℃, with the TiO of ultrasonic mistake
2Colloidal sol joins in the hydrochloric acid solution of 20mL2.0mol/L, then the 0.1mL aniline monomer is added wherein.Hydrochloric acid solution with ammonium persulfate slowly splashes in the mixed liquor at last, and the color of system is deepened gradually by light blue, changes into blackish green at last.After leaving standstill 6min, with organic filtrator filtration of 0.45 μ m.Pretreated interdigital electrode formula device is immersed in polyaniline/titania filtrate, and reaction 20min takes out the back and dries naturally in air, is placed in the pure nitrogen and tests behind the preservation 12h.
At first plane interdigital electrode formula unit component is as shown in Figure 2 carried out surface preparation.Interdigital electrode formula device is put into 1% polydiene propyl ammonium chloride aqueous solution soaked 10 minutes, take out the back and use deionized water wash, dry up with nitrogen again; Again substrate was immersed in poly-(sodium p styrene sulfonate) solution of 2mg/mL 10 minutes, and took out the back with deionized water wash and dry up.
0.1g is dissolved in the hydrochloric acid solution of 20mL 0.2mol/L with the spreading agent neopelex, and the back that stirs adds 0.144g SnO
2Nano-powder, and with magnetic stirrer high-speed stirred 20min, at this moment dispersed system is creamy white; And then put into supersonic wave cleaning machine sonic oscillation 30min.Take by weighing the 0.1254g ammonium persulfate, be dissolved in the hydrochloric acid of 10mL 2mol/L.Temperature joins the 0.1mL aniline monomer SnO of ultrasonic mistake in the time of 10 ℃
2In the colloidal sol, the hydrochloric acid solution with ammonium persulfate slowly splashes in the mixed liquor at last, and the color of system is deepened gradually by light blue, changes into blackish green at last.After leaving standstill 5min, with organic filtrator filtration of 0.45 μ m.Pretreated interdigital electrode formula device is immersed in polyaniline/tin ash filtrate, and reaction 20min takes out the back and dries naturally in air, is placed in the pure nitrogen and tests behind the preservation 12h.
Claims (7)
1, a kind of polyaniline/nanometer oxidate compound film micro-gas sensors array, it is to be integrated in the same substrate by the polyaniline more than 2/nanometer oxidate compound film micro-gas sensors unit to constitute, it is characterized in that: described polyaniline/nanometer oxidate compound film micro-gas sensors unit comprises substrate, interdigital electrode, polyaniline/nanometer oxidate compound film and conductive lead wire, wherein polyaniline/nanometer oxidate compound film has by following raw material and makes: aniline monomer, dopant acid solution, the oxygenant acid solution, spreading agent and inorganic oxide sol or powder.
2, polyaniline/nanometer oxidate compound film micro-gas sensors array according to claim 1, it is characterized in that, at least comprise two dissimilar polyanilines/nanometer oxidate compound film micro-gas sensors unit in each array, the difference of this polyaniline/nanometer oxidate compound film micro-gas sensors unit is that its polyaniline/nanometer oxidate compound film made by following different raw material:
A, aniline monomer, dopant acid solution, oxygenant acid solution and nano titanic oxide sol;
B, aniline monomer, dopant acid solution, oxygenant acid solution and nano oxidized imperial mandate colloidal sol;
C, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nano tin dioxide powder;
D, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nano indium oxide powder;
E, aniline monomer, dopant acid solution, oxygenant acid solution, spreading agent and nanometer tungsten oxide powder.
3, polyaniline/nanometer oxidate compound film micro-gas sensors array according to claim 1 and 2 is characterized in that, the mol ratio of aniline monomer and oxygenant is 1; Dopant acid solution is the hydrochloric acid solution of 2.0M; The weight percentage of inorganic oxide sol is 0.05～1%, and the mass ratio of inorganic oxide powder and aniline monomer is 0.020～0.030: 0.5～2; Described oxygenant is an ammonium persulfate; Described spreading agent is a neopelex.
4, polyaniline/nanometer oxidate compound film micro-gas sensors array according to claim 1 is characterized in that, described substrate is the silicon chip of 5mm * 8mm, and described interdigital electrode material is a gold, and its electrode separation and width are 50 μ m.
5, a kind of preparation method of polyaniline/nanometer oxidate compound film micro-gas sensors array is characterized in that, may further comprise the steps:
(1), utilization standard semiconductor technology prepares interdigital electrode on substrate;
(2), partly adopt the polyaniline/nano-oxide composite sensing film of electrostatic force self assembly and in-situ polymerization sedimentation growth high electrical conductivity, draw lead at two electrode tips in interdigital electrode;
(3), the polyaniline/nanometer oxidate compound film micro-gas sensors unit that will use different nano-oxides to prepare is integrated in the same substrate and constitutes micro-gas sensors array.
6, the preparation method of polyaniline/nanometer oxidate compound film micro-gas sensors array according to claim 5, it is characterized in that, adopt the polyaniline/nano-oxide composite sensing film of electrostatic force self assembly and in-situ polymerization sedimentation growth high electrical conductivity may further comprise the steps in the step (2): 1. plane interdigital electrode formula device to be put into polydiene propyl ammonium chloride aqueous solution and soak 6～12min, take out the back and use deionized water wash, dry up with nitrogen again; 2. again substrate is immersed 7～13min in the poly (sodium 4-styrenesulfonate) solution, take out the back with deionized water wash and dry up; 3. temperature joins inorganic nanometer oxide colloidal sol or the powder of handling in the dopant acid solution in 0～25 ℃, and then aniline monomer is added wherein, at last oxidizing agent solution is added drop-wise to said mixture and reacts; 4. mixed liquor leaves standstill 3～10min, filters with organic filtrator; 5. the substrate after will handling is immersed in the filtrate, takes out behind 15～25min, dries naturally under the room temperature condition.
7, the preparation method of polyaniline/nanometer oxidate compound film micro-gas sensors array according to claim 6 is characterized in that:
The disposal route of A, nano inorganic oxide powder is: neopelex is joined in the watery hydrochloric acid in proportion, and tin ash, indium oxide or tungsten oxide nano-powder are added in the back that stirs; This mixing suspension is high-speed stirred 10～30min at first, and then puts into supersonic wave cleaning machine sonic oscillation 20～40min;
The disposal route of B, nano inorganic oxide colloidal sol is: add a certain amount of deionized water dilution nano titanic oxide sol and nano oxidized imperial mandate colloidal sol, put into supersonic wave cleaning machine sonic oscillation 10～20min then.
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