CN102654480A - Method for making sensitive membrane of surface acoustic wave sensor - Google Patents

Method for making sensitive membrane of surface acoustic wave sensor Download PDF

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Publication number
CN102654480A
CN102654480A CN2011100500691A CN201110050069A CN102654480A CN 102654480 A CN102654480 A CN 102654480A CN 2011100500691 A CN2011100500691 A CN 2011100500691A CN 201110050069 A CN201110050069 A CN 201110050069A CN 102654480 A CN102654480 A CN 102654480A
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China
Prior art keywords
sensitive membrane
acoustic wave
surface acoustic
wave sensor
mixed solution
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CN2011100500691A
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Chinese (zh)
Inventor
李冬梅
汪幸
刘明
周文
侯成诚
闫学锋
谢常青
叶甜春
霍宗亮
龙世兵
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Institute of Microelectronics of CAS
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Institute of Microelectronics of CAS
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Application filed by Institute of Microelectronics of CAS filed Critical Institute of Microelectronics of CAS
Priority to CN2011100500691A priority Critical patent/CN102654480A/en
Publication of CN102654480A publication Critical patent/CN102654480A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for making a sensitive membrane of a surface acoustic wave sensor, comprising the steps of dropwise coating a mixed solution on a delay line of a dual-delay linear oscillator and then drying in vacuum to form the sensitive membrane, wherein the mixed solution is formed by evenly dispersing polyaniline (PAn) powder in a TiO2 colloid solution.. According to the method for making the sensitive membrane of the surface acoustic wave sensor, the polymerized sensitive membrane is made by adding the PAn powder to the TiO2 solution; and compared with a pure PAn sensor, the doped PAn/TiO2 sensor is improved in selectivity, sensitivity and detection quality to a certain extent.

Description

A kind of method of making the surface acoustic wave sensor sensitive membrane
Technical field
The present invention relates to surface acoustic wave (SAW) gas sensor device manufacturing technology field, particularly a kind of through in colloidal tio 2 solution, disperseing polyaniline powder to make the method for surface acoustic wave sensor sensitive membrane.
Background technology
Since the eighties, the development work of SAW gas sensor is risen gradually, can detect H at present 2S, NO 2, SO 2, NH 3Etc. multiple gases, the sensor that the utilization surface acoustic wave techniques is developed into can directly be exported digital signal, thereby has advantageous superiority.
The SAW gas sensor has been compared some remarkable advantages with the gas sensor of other kind; Such as gasmetry highly sensitive, precision is high, resolution is high, antijamming capability is strong and valid analysing range is big, and the SAW gas sensor can with logical device combine realize microminiaturized, integrated and intelligent.
The basic functional principle of SAW gas sensor mainly is the variation that causes SAW sensor electrical conductance and quality through the absorption that the sensitive membrane that the SAW device surface is covered is treated side gas; Thereby cause the change of the oscillation frequency of SAW oscillator, realize monitoring and measurement gas with this.Therefore want to produce the surface acoustic wave sensor device of high sensitivity and quality, wherein the special key of design and fabrication part of sensitive membrane.
The raising of Along with people's quality of life, to commercial production and living condition require increasingly highly, people are also increasing to the demand of gas sensor.The research and development of gas sensor, the especially research of toxic and harmful sensor obtain fast development especially.Ammonia is a kind of commercial Application toxic gas widely, and is colourless, and the pungency foul smell is arranged, and it has stimulation and corrosive attack to the upper respiratory tract of animal or human's body, and the volume fraction of the atmosphere pollution of on-site real-time monitoring often is low to moderate 10 -6Even 10 -9Level, this sensor that just requires to monitor dusty gas will have enough sensitivity and selectivity.
Conducting polymer is a research frontier that grows up the seventies in 20th century, because of its tempting application prospect receives extensive attention.Polypyrrole, polyaniline, polythiophene etc. have susceptibility to specific gas at normal temperatures; Wherein polyaniline (PAn) becomes the conducting polymer 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 property and raw material are cheap and easy to get and in the wide application of many-sides such as rechargeable battery, display device, chemical sensor; But it is single polyaniline is low as the sensor selectivity that membraneous material is prepared into; Working temperature is high, and applied value is not high.
Selectivity characteristic; High temperature not only influences the stablizing effect of sensor measurement, and can bring extra problems such as power attenuation, so can produce quick at normal temperatures; It is special important that the gas sensor of sensitive detection low concentration seems, this has higher requirement also for the making of film.
Summary of the invention
The technical matters that (one) will solve
In view of this, fundamental purpose of the present invention is to provide a kind of method of making the surface acoustic wave sensor sensitive membrane.
(2) technical scheme
For achieving the above object, the invention provides a kind of method of making the surface acoustic wave sensor sensitive membrane, this method is on a lag line of two delay line type oscillators, drips applying mixed solution and vacuum drying and forms, this mixed solution is at TiO 2Evenly disperse polyaniline PAn powder to form in the colloidal solution.This method specifically comprises:
Step 1: make TiO 2Colloidal solution;
Step 2: polyaniline PAn powder is added this TiO 2In the colloidal solution, form mixed solution;
Step 3: drip and to be coated with this mixed solution;
Step 4: vacuum drying forms sensitive membrane.
In the such scheme, make TiO described in the step 1 2Colloidal solution is through hydrolysis isopropyl titanate [Ti (OCH (CH 3) 2) 4] make.
In the such scheme, described in the step 2 polyaniline PAn powder is added this TiO 2Colloidal solution further utilizes stirring machine to stir, and polyaniline PAn powder is evenly disperseed.
In the such scheme, drip described in the step 3 and be coated with this mixed solution, specifically comprise: use micropipettor at normal temperatures on a lag line of two delay line type oscillators, drip this mixed solution that is coated with 50ul.
In the such scheme, vacuum drying described in the step 4 is a drying at least two hours in 60 ℃ vacuum drying chamber.
(3) beneficial effect
The method of this making surface acoustic wave sensor sensitive membrane provided by the invention is through adding TiO with the PAn powder 2Make polymerization sensitive membrane, the PAn/TiO after the doping in the solution 2Sensor is compared with pure PAn sensor, selectivity, and sensitivity also can improve with the detection quality.
Description of drawings
Fig. 1 is the process flow diagram of making surface acoustic wave sensor sensitive membrane provided by the invention; Wherein, 1 is piezoelectric base unit (piezoelectric monocrystal or film), and 2 is interdigital transducer IDT (Au or Pt), and 3 is the metallic film (Au or Pt etc.) on the travel path, and 4 is the chemical-sensitive film.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
The method of making surface acoustic wave sensor sensitive membrane provided by the invention is in the manufacture process of sonic surface wave gas sensors, on a lag line of two delay line type oscillators, drips applying mixed solution and vacuum drying and forms, and this mixed solution is at TiO 2Evenly disperse polyaniline PAn powder to form in the colloidal solution.
TiO 2Be a kind of weak n type metal oxide semiconductor, very high reaction sensitivity and very fast response time arranged, existing application more widely as gas sensor.Polyaniline (PAn) is with its unique mechanism of doping effect, the reversible many-sided application of oxidation-reduction characteristic, good stable property, and becomes the conducting polymer that is hopeful to obtain at present practical application most, and the sensitive membrane of producing through polymerization can make PAn/TiO 2Polymkeric substance is to NH 3Bigger response is arranged, and better choice property is accomplished low concentration NH with expectation at normal temperatures 3Carry out high-quality, sensitivity, the accurate detection.
The method of this making surface acoustic wave sensor sensitive membrane provided by the invention specifically comprises:
Step 1: make TiO 2Colloidal solution; Said making TiO 2Colloidal solution is through hydrolysis isopropyl titanate [Ti (OCH (CH 3) 2) 4] make;
Step 2: polyaniline PAn powder is added this TiO 2In the colloidal solution, form mixed solution; Said with this TiO of polyaniline PAn powder adding 2Behind the colloidal solution, further utilize stirring machine to stir, polyaniline PAn powder is evenly disperseed;
Step 3: drip and to be coated with this mixed solution, specifically comprise: use micropipettor at normal temperatures on a lag line of two delay line type oscillators, drip this mixed solution that is coated with 50ul;
Step 4: vacuum drying forms sensitive membrane; Wherein vacuum drying is a drying at least two hours in 60 ℃ vacuum drying chamber.
Embodiment
The embodiment of the invention provide at TiO 2Evenly disperse the PAn powder in the colloidal solution, make the method for sensitive membrane then through drop-coating, at first through hydrolysis 30ml isopropyl titanate [Ti (OCH (CH 3) 2) 4] make the stable TiO of about 200mL 2Colloidal sol, TiO 2The about 8nm of the size of colloidal particles, the PAn powder of adding 10mg-50mg, the powerful stirring evenly disperseed the PAn powder, forms mixed solution; Approximately drip the above-mentioned mixed solution that is coated with 10-50ul in the sensitizing range of sensor component lag line then, vacuum drying 2 hours forms the surface acoustic wave sensor sensitive membrane.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (6)

1. a method of making the surface acoustic wave sensor sensitive membrane is characterized in that, this method is on a lag line of two delay line type oscillators, drips applying mixed solution and vacuum drying and forms, and this mixed solution is at TiO 2Evenly disperse polyaniline PAn powder to form in the colloidal solution.
2. the method for making surface acoustic wave sensor sensitive membrane according to claim 1 is characterized in that, this method specifically comprises:
Step 1: make TiO 2Colloidal solution;
Step 2: polyaniline PAn powder is added this TiO 2In the colloidal solution, form mixed solution;
Step 3: drip and to be coated with this mixed solution;
Step 4: vacuum drying forms sensitive membrane.
3. the method for making surface acoustic wave sensor sensitive membrane according to claim 2 is characterized in that, makes TiO described in the step 1 2Colloidal solution is through hydrolysis isopropyl titanate [Ti (OCH (CH 3) 2) 4] make.
4. the method for making surface acoustic wave sensor sensitive membrane according to claim 2 is characterized in that, described in the step 2 polyaniline PAn powder is added this TiO 2Colloidal solution further utilizes stirring machine to stir, and polyaniline PAn powder is evenly disperseed.
5. the method for making surface acoustic wave sensor sensitive membrane according to claim 2 is characterized in that, drips described in the step 3 to be coated with this mixed solution, specifically comprises:
Use micropipettor at normal temperatures on a lag line of two delay line type oscillators, drip this mixed solution that is coated with 50ul.
6. the method for making surface acoustic wave sensor sensitive membrane according to claim 2 is characterized in that, vacuum drying described in the step 4 is a drying at least two hours in 60 ℃ vacuum drying chamber.
CN2011100500691A 2011-03-02 2011-03-02 Method for making sensitive membrane of surface acoustic wave sensor Pending CN102654480A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5252292A (en) * 1989-05-18 1993-10-12 Mitsutoshi Hirata Ammonia sensor
CN101042363A (en) * 2007-04-27 2007-09-26 电子科技大学 polyaniline nanometer oxidate compound film micro-gas sensors array and method for making same
CN101633779A (en) * 2009-08-21 2010-01-27 昆明理工大学 Conductive polyaniline composite electrode material and preparation method thereof
CN101936937A (en) * 2010-07-06 2011-01-05 电子科技大学 Micro-cantilever gas sensor and manufacturing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5252292A (en) * 1989-05-18 1993-10-12 Mitsutoshi Hirata Ammonia sensor
CN101042363A (en) * 2007-04-27 2007-09-26 电子科技大学 polyaniline nanometer oxidate compound film micro-gas sensors array and method for making same
CN101633779A (en) * 2009-08-21 2010-01-27 昆明理工大学 Conductive polyaniline composite electrode material and preparation method thereof
CN101936937A (en) * 2010-07-06 2011-01-05 电子科技大学 Micro-cantilever gas sensor and manufacturing method thereof

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Application publication date: 20120905