CN101363807A - Organic gas sensor and method for making same - Google Patents
Organic gas sensor and method for making same Download PDFInfo
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- CN101363807A CN101363807A CNA2008100460283A CN200810046028A CN101363807A CN 101363807 A CN101363807 A CN 101363807A CN A2008100460283 A CNA2008100460283 A CN A2008100460283A CN 200810046028 A CN200810046028 A CN 200810046028A CN 101363807 A CN101363807 A CN 101363807A
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Abstract
The invention discloses an organic gas sensor and a structure thereof. The organic gas sensor comprises a base plate, a first electrode, a medium layer, a sensitive film layer, a second electrode and a third electrode, wherein the medium layer in the sensor adopts organic functional material, and the sensor can be divided into top contact type and bottom contact type according to the position difference of the film layer and the electrodes in the structure of the sensor. The invention has the advantages that the integration level, the response speed and the response precision of the gas sensor are improved, the production technique of the common gas sensor is optimized, the technological requirement is reduced, the performances are enhanced, the production cost of the gas sensor is greatly reduced, and the reliability of the equipment is greatly improved.
Description
Technical field
The present invention relates to sensor technical field, be specifically related to a kind of organic gas sensor and preparation method thereof.
Background technology
Quick development of modern science and technology such as measurement, control and robotization have greatly promoted the progress of infotech, and human society has stepped into the information age.Sensor technology as one of three big pillars of infotech is main means of obtaining information, is bringing into play more and more important effect in modern science and technology.Sensor has obtained using widely at aspects such as scientific research and industrial and agricultural production, environmental protection, health care, security protections.
Sensor is a kind ofly can do in order to mode optionally thereby specific material to be analyzed to be produced response to the device that amalyzing substances qualitatively or quantitatively determines by certain, can be used to detect one or more specific materials.
At present, the development trend of gas sensor concentrates on: 1, improve sensitivity and serviceability, and make its microminiaturization, and can combine with the application complete machine.2, strengthen reliability, possess multiple function, first develop the MEMS technology, on-the-spot transmitter and the Intelligence sensor that is suitable for of development.Current research focus is exactly the exploitation of new gas sensitive and manufacture craft and the design of new structure.Develop new gas sensitization membrane material,, make these new materials have high sensitivity, high selectivity, high stability gas with various as compound and mixed type semiconductor air-sensitive material, macromolecule gas sensitive.Because the organic polymer sensitive material has advantages such as material is abundant, cost is low, filming technology is simple, be easy to work with other technical compatibility, at normal temperatures.In addition, can also continue to use traditional action principle and some new effect, preferentially use crystalline material, adopt advanced process technology and microstructure design, development novel sensor and sensing system.
Use the key component of certain organic material fabricate devices in the organic gas sensor, because organic material is that material selects to provide broad scope with its intrinsic diversity, by to the design of organic molecular structure, assemble and cut out, can satisfy many-sided different needs and be easy to realize large-area preparation, the simple process preparation, economical with materials cost and equipment cost.
Believe to be accompanied by new material, new technology and The application of new technique that the performance of gas sensor more becomes to improving also can satisfy people's miniaturization, polyfunctional composite request.Believe along with the success of new material developments such as nanometer technology, thin film technique, the integrated application of micromechanics and microelectric technique, computer technology etc., the intelligent gas sensor of high-performance that possesses the multiple gases monitoring function will occur in the near future.
Summary of the invention
Technical matters to be solved by this invention is how a kind of organic gas sensor and preparation method thereof is provided, this gas sensor has adopted new structure, use the mixed film of single or multiple responsive thin material, simplified the manufacture craft of gas sensor, increased the integrated level of gas sensor, can further reduce cost and technological requirement.
Technical matters proposed by the invention is to solve like this: a kind of organic gas sensor is provided, comprise substrate, first electrode, dielectric layer, sensitive thin film layer, second electrode and third electrode, it is characterized in that described dielectric layer is a high-molecular organic material, this high-molecular organic material is:
1. one or more in polyvinyl pyrrolidone (PVP), polymethylmethacrylate (PMMA), polystyrene (PS) and the polyvinyl alcohol (PVA) (PVA);
2. or ultra-violet curing glue, comprise the free radical type ultraviolet photo-curing cementing agent, cation type ultraviolet photo-curing cementing agent and their mixed system.
According to organic gas sensor provided by the present invention, it is characterized in that described dielectric layer film thickness is 1nm～500nm, the best is 60nm.
According to organic gas sensor provided by the present invention, it is characterized in that, in the following material of described sensitive thin film layer material one or more: polysiloxane-based sensitive material, poly-silicon-carbon alkanes sensitive material, organic phosphine poison sensitive material, semiconductor ceramic material, with hexafluoroisopropanol (HFIP) is that sensitive group and polysiloxane are the material of skeleton, in oligomerization dimethyl siloxane chain, introduce the organic/inorganic mixed type multipolymer that the fluoro bisphenol group forms, polypyrrole, polythiophene, polyaniline, polyaniline/nano-oxide compound substance, as polyaniline/tin ash, polyaniline/titania, polyaniline/indium oxide, polyaniline/tungsten oxide, poly-(oxygen { methyl (4-hydroxyl-4, two (the three fluoro methyl) but-1-enes-1-alcohol of 4-) methylene siloxane }) SXFA, copolymerization carbon siloxane BSP3.
According to organic gas sensor provided by the present invention, it is characterized in that the molecular structural formula of described polyvinyl pyrrolidone is (I), the molecular structural formula of polymethylmethacrylate is (II), the polystyrene molecular structural formula is (III), and the molecular structural formula of polyvinyl alcohol (PVA) is (IV):
According to organic gas sensor provided by the present invention, it is characterized in that described free radical type ultraviolet photo-curing cementing agent comprises base resin, monomer, light trigger and photosensitizer and auxiliary agent; Described cation type ultraviolet photo-curing cementing agent comprises cationic monomer, thinning agent and cation light initiator.
According to organic gas sensor provided by the present invention, it is characterized in that described base resin comprises unsaturated polyester resin, acrylic resin and polythiol-polyenoid system; Described monomer comprises styrene and derivant, simple function group or multi-functional acrylate; Described light trigger comprises styrax and derivant benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether and acetophenone derivative; Photosensitizer comprises benzophenone, thia anthraquinone and Michler's keton, and auxiliary agent comprises plastifier, thixotropic agent, filling agent, antistatic agent, fire retardant and coupling agent; Described cationic monomer comprises various epoxy resin or modified epoxy or fluorine-containing and not fluorine-containing hybrid resin or aliphatics and bis-phenol D-type blending epoxy; Described thinning agent comprises various active epoxy diluent resins and various cyclic ethers, cyclic lactone, the vinyl ether monomers thinning agent as light-cured resin; Described cation light initiator has diaryl group iodized salt, triaryl salt compounded of iodine, triaryl sulfonium salts, triaryl selenium salt.
According to organic gas sensor provided by the present invention, it is characterized in that described acrylic resin comprises polyester-acrylate, epoxy-acrylate, carbamate-acrylate and polyethers-acrylate.
According to organic gas sensor provided by the present invention, it is characterized in that described polythiol-polyenoid system comprises the material of following structural formula:
According to organic gas sensor provided by the present invention, it is characterized in that base resin comprises unsaturated polyester resin, acrylic resin and polythiol-polyenoid system; Monomer comprises styrene and derivant, simple function group and multi-functional acrylate; Light trigger comprises styrax and derivant benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether and acetophenone derivative; Photosensitizer comprises benzophenone, thia anthraquinone and Michler's keton; Auxiliary agent comprises plastifier, thixotropic agent, filling agent, antistatic agent, fire retardant and coupling agent.
According to organic gas sensor provided by the present invention, it is characterized in that described first electrode, second electrode and third electrode are metal or conductive film; Substrate is silicon substrate, glass or flexible substrate.
According to organic gas sensor provided by the present invention, it is characterized in that described flexible substrate adopts a kind of material or thin metal or the glass in polyesters, the poly-phthalimide compound.
According to organic gas sensor provided by the present invention, it is characterized in that, sensor construction is a kind of in top contact, the bottom contact, wherein top contact structure constitute be parts from the bottom to the top, be followed successively by substrate, first electrode, dielectric layer, sensitive thin film layer and same aspect the and electrode and third electrode, bottom contact structure constitute be parts from the bottom to the top, be followed successively by substrate, first electrode, dielectric layer, at second electrode of same aspect and third electrode, sensitive thin film layer.
A kind of preparation method of organic gas sensor is characterized in that, may further comprise the steps:
1. earlier substrate is cleaned completely, it is dry to clean the back;
2. at surface preparation first electrode of substrate;
3. form the figure of first electrode;
4. on the substrate that is coated with first electrode, prepare the medium tunic;
5. the medium tunic that forms is carried out post-processed processing, promptly be heating and curing or ultra-violet curing;
6. on the medium tunic, continue preparation sensitive thin film layer;
7. on the sensitive thin film layer, prepare second electrode and third electrode then;
8. form second electrode, the third electrode pattern.
A kind of preparation method of organic gas sensor is characterized in that, may further comprise the steps:
1. earlier substrate is cleaned completely, it is dry to clean the back;
2. at surface preparation first electrode of substrate;
3. form the figure of first electrode;
4. on the substrate of first electrode, prepare the medium tunic;
5. the medium tunic that forms is carried out post-processed processing, promptly be heating and curing or ultra-violet curing;
6. on the medium tunic, prepare second electrode and third electrode then;
7. form second electrode, the third electrode pattern;
8. at second electrode, continue preparation sensitive thin film layer on the third electrode.
Preparation method according to organic gas sensor provided by the present invention, it is characterized in that described dielectric layer and sensitive material layer are by vacuum evaporation, ionic group bundle deposition, ion plating, dc sputtering deposition, the RF sputter coating, ion beam sputtering deposition, ion beam assisted depositing, (wherein the plasma generator in the plasma reinforced chemical vapour deposition is a radio-frequency drive to plasma reinforced chemical vapour deposition, direct-current discharge, a kind of in microwave plasma and the electron cyclotron resonace), high density inductive coupling formula plasma source chemical vapor deposition (HD-ICP-CVD), catalyst chemical vapor deposition (Cat-CVD), magnetron sputtering, electroplate, spin coating, dip-coating, inkjet printing, roller coat, one or several modes in the LB film and forming.
Gas sensor provided by the present invention, novel structure, sensitive thin film layer can be the THIN COMPOSITE retes that single sensitive thin film or multiple sensitive material form, and help the integrated of multiple gases sensor; Dielectric layer adopts the organic media material to help simplifying preparation technology, and organic material can adopt the method for spin coating, saves cost and time, and the organic material kind is more and be easy to current material is carried out improved properties; The sensor of this structure itself is beneficial to integrated, forms sensor array; Device is ultra-thin, and volume is little, and is in light weight, and the preparation method is rationally simple, easy operating; Improved response speed and response accuracy, and optimized the manufacture craft of general gas sensor, reduced technological requirement, improved its performance, significantly reduced the preparation cost of gas sensor, this technology is significant to the manufacture craft of sensor.
Description of drawings
Fig. 1 is a top provided by the present invention contact gas sensor configuration synoptic diagram;
Fig. 2 is a bottom provided by the present invention contact gas sensor configuration synoptic diagram;
Wherein, 1, substrate, 2, first electrode, 3, dielectric layer, 4, the sensitive thin film layer, 5, second electrode, 6, third electrode.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and embodiment.
Technical scheme of the present invention provides a kind of organic gas sensor, and as illustrated in fig. 1 and 2, the structure of device comprises substrate 1, the first electrode 2, dielectric layer 3, sensitive thin film layer 4, the second electrode 5, third electrode 6.
Wherein the molecular structural formula of polyvinyl pyrrolidone is (I), and the molecular structural formula of polymethylmethacrylate is (II), and the polystyrene molecular structural formula is (III), and the molecular structural formula of polyvinyl alcohol (PVA) is (IV):
The free radical type ultraviolet photo-curing cementing agent comprises base resin, monomer, light trigger and photosensitizer and auxiliary agent, base resin comprises unsaturated polyester resin, acrylic resin and polythiol-polyenoid system, acrylic resin comprises polyester-acrylate, epoxy-acrylate, carbamate-acrylate and polyethers-acrylate, polythiol-polyenoid system comprises:
Polynary allylic compound commonly used has CH
2=CHCH
2O (CH
2CH
2CH
2O)
nCH
2CH=CH
2, cyanacrylate
HS (CH
2CH
2O)
2CH
2CH
2One or more of SH, monomer comprises styrene and derivant, simple function group or polyfunctional group (methyl) acrylate thereof, as methyl methacrylate, ethyl acrylate, acrylic acid propylene glycol ester, n-butyl acrylate, light trigger comprises styrax and derivant benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether and acetophenone derivative, photosensitizer has benzophenone, thia anthraquinone and Michler's keton, auxiliary agent comprises plastifier, thixotropic agent, filling agent, antistatic agent, fire retardant, coupling agent, as silicone couplet CH
2=CHSi (OCH
2CH
2OCH
3)
3Cation type ultraviolet photo-curing cementing agent comprises monomer, as various epoxy resin or modified epoxy or fluorine-containing and not fluorine-containing hybrid resin or aliphatics and bis-phenol D-type blending epoxy, various active epoxy diluent resins and various cyclic ethers, cyclic lactone, vinyl ether monomers are as the thinning agent of light-cured resin, and cation light initiator has diaryl group iodized salt, triaryl salt compounded of iodine, triaryl sulfonium salts, triaryl selenium salt; Their mixed system comprises the mixing of free radical type and cationic ultra-violet curing glue, as benzhydryl iodine hexafluorophosphate (DPI.PF
6) make light trigger, cause bisphenol A epoxide resin E
51Hybrid resin with acrylic ester prepolymer AE.
Sensitive thin film layer 4 is one or more in the following material among the present invention: polysiloxane-based sensitive material, poly-silicon-carbon alkanes sensitive material, organic phosphine poison sensitive material, semiconductor ceramic material, poly-(oxygen { methyl (4-hydroxyl-4, two (the three fluoro methyl) but-1-enes-1-alcohol of 4-) methylene siloxane }) SXFA, with hexafluoroisopropanol (HFIP) is that sensitive group and polysiloxane are a class material of skeleton, copolymerization carbon siloxane BSP3, in oligomerization dimethyl siloxane chain, introduce the organic/inorganic mixed type multipolymer that the fluoro bisphenol group forms, polypyrrole, polythiophene, polyaniline, polyaniline/nano-oxide compound substance is as polyaniline/tin ash, polyaniline/titania, polyaniline/indium oxide, polyaniline/tungsten oxide.
Below be specific embodiments of the invention:
As shown in Figure 1 in the structure, substrate 1 adopts the Si substrate, the ITO transparent conductive film that adopts the DC magnetron sputtering is as first electrode 2, adopt ultra-violet curing glue as dielectric layer 3, second electrode 5 adopts the Cr metallic film, third electrode 6 also adopts the Cr metallic film, and sensitive thin film layer 4 adopts polyaniline/nano-oxide compound substance.
The preparation method is as follows:
1. earlier the Si substrate is cleaned completely, clean the back and dry up with drying nitrogen;
2. the method by the DC magnetron sputtering prepares first electrode on the surface of Si substrate;
3. method etching ITO first electrode pattern by photoetching;
4. ultra-violet curing glue organic dielectric film on being coated with on the Si substrate of first electrode by the method spin coating of spin coating;
5. the organic dielectric film that forms is carried out ultra-violet curing and heated baking;
6. forming first electrode, the Si substrate of covering organic dielectric film is put into vacuum cavity and is prepared sensitive material polyaniline/nano-oxide compound substance;
7. evaporation Cr metal second electrode and Cr metal third electrode on the sensitive material film then;
8. form second electrode by photoetching, the third electrode pattern.
In the structure, substrate 1 adopts the Si substrate as shown in Figure 1, and the ITO transparent conductive film that adopts the DC magnetron sputtering is as first electrode 2, adopt ultra-violet curing glue as dielectric layer 3, second electrode 5 adopts the Cr metallic film, and third electrode 6 also adopts the Cr metallic film, and sensitive thin film layer 4 adopts SXFA.
The preparation of devices flow process is similar to embodiment 1.
As shown in Figure 1 in the structure, substrate 1 adopts the Si substrate, the ITO transparent conductive film that adopts the DC magnetron sputtering is as first electrode 2, adopt ultra-violet curing glue 3 as dielectric layer, second electrode 5 adopts the Cr metallic film as electrode layer, third electrode 6 also adopts the Cr metallic film as electrode layer, and sensitive thin film layer 4 adopts BSP3.
The preparation of devices flow process is similar to embodiment 1.
As shown in Figure 1 in the structure, substrate 1 adopts the Si substrate, the ITO transparent conductive film that adopts the DC magnetron sputtering is as first electrode 2, adopt polymethylmethacrylate as dielectric layer 3, second electrode 5 adopts the Cr metallic film, third electrode 6 also adopts the Cr metallic film, and sensitive thin film layer 4 adopts SXFA.
The preparation of devices flow process is similar to embodiment 1.
As shown in Figure 1 in the structure, substrate 1 adopts the Si substrate, the ITO transparent conductive film that adopts the DC magnetron sputtering is as first electrode 2, adopt polymethylmethacrylate 3 as dielectric layer, second electrode 5 adopts the Cr metallic film as electrode layer, third electrode 6 also adopts the Cr metallic film as electrode layer, and sensitive thin film layer 4 adopts BSP3.
The preparation of devices flow process is similar to embodiment 1.
Claims (10)
1. an organic gas sensor comprises substrate, first electrode, dielectric layer, sensitive thin film layer, second electrode and third electrode, it is characterized in that, described dielectric layer is a high-molecular organic material, and this high-molecular organic material is:
1. one or more in polyvinyl pyrrolidone, polymethylmethacrylate, polystyrene and the polyvinyl alcohol (PVA);
2. or ultra-violet curing glue, comprise the free radical type ultraviolet photo-curing cementing agent, cation type ultraviolet photo-curing cementing agent and their mixed system.
2. organic gas sensor according to claim 1 is characterized in that, described dielectric layer film thickness is 1nm～500nm.
3. organic gas sensor according to claim 1, it is characterized in that described sensitive thin film layer material is one or more in the following material: polysiloxane-based sensitive material, poly-silicon-carbon alkanes sensitive material, organic phosphine poison sensitive material, semiconductor ceramic material, be that sensitive group and polysiloxane are the material of skeleton, introduce organic/inorganic mixed type multipolymer, polypyrrole, polythiophene, polyaniline and polyaniline/nano-oxide compound substance that the fluoro bisphenol group forms in oligomerization dimethyl siloxane chain with the hexafluoroisopropanol.
4. organic gas sensor according to claim 1, it is characterized in that the molecular structural formula of described polyvinyl pyrrolidone is (I), the molecular structural formula of polymethylmethacrylate is (II), the polystyrene molecular structural formula is (III), and the molecular structural formula of polyvinyl alcohol (PVA) is (IV):
5. organic gas sensor according to claim 1 is characterized in that, described free radical type ultraviolet photo-curing cementing agent comprises base resin, monomer, light trigger and photosensitizer and auxiliary agent.
6. organic gas sensor according to claim 5 is characterized in that, base resin comprises unsaturated polyester resin, acrylic resin and polythiol-polyenoid system; Monomer comprises styrene and derivant, simple function group and multi-functional acrylate; Light trigger comprises styrax and derivant benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether and acetophenone derivative; Photosensitizer comprises benzophenone, thia anthraquinone and Michler's keton; Auxiliary agent comprises plastifier, thixotropic agent, filling agent, antistatic agent, fire retardant and coupling agent.
7. organic gas sensor according to claim 1 is characterized in that, first electrode, second electrode and third electrode are metal or conductive film; Substrate is silicon substrate, glass or flexible substrate.
8. organic gas sensor according to claim 7, it is characterized in that, sensor construction is a kind of in top contact and the bottom contact, wherein to constitute be that parts are followed successively by substrate, first electrode, dielectric layer, sensitive thin film layer and at second electrode and the third electrode of same aspect from the bottom to the top to top contact structure, bottom contact structure constitute be parts from the bottom to the top, be followed successively by substrate, first electrode, dielectric layer, at second electrode of same aspect and third electrode, sensitive thin film layer.
9. the preparation method of an organic gas sensor is characterized in that, may further comprise the steps:
1. earlier substrate is cleaned completely, it is dry to clean the back;
2. at surface preparation first electrode of substrate;
3. form the figure of first electrode;
4. on the substrate that is coated with first electrode, prepare the medium tunic;
5. the medium tunic that forms is heating and curing or ultra-violet curing;
6. on the medium tunic, continue preparation sensitive thin film layer;
7. on the sensitive thin film layer, prepare second electrode and third electrode then;
8. form second electrode, the third electrode pattern;
Wherein said dielectric layer and sensitive material layer are to form by one or several modes in vacuum evaporation, ionic group bundle deposition, ion plating, dc sputtering deposition, RF sputter coating, ion beam sputtering deposition, ion beam assisted depositing, plasma reinforced chemical vapour deposition, high density inductive coupling formula plasma source chemical vapor deposition, catalyst chemical vapor deposition, magnetron sputtering, plating, spin coating, dip-coating, inkjet printing, roller coat, the LB film.
10. the preparation method of an organic gas sensor is characterized in that, may further comprise the steps:
1. earlier substrate is cleaned completely, it is dry to clean the back;
2. at surface preparation first electrode of substrate;
3. form the figure of first electrode;
4. on the substrate of first electrode, prepare the medium tunic;
5. the medium tunic that forms is heating and curing or ultra-violet curing;
6. on the medium tunic, prepare second electrode and third electrode then;
7. form second electrode, the third electrode pattern;
8. at second electrode, continue preparation sensitive thin film layer on the third electrode;
Wherein said dielectric layer and sensitive material layer are to form by one or several modes in vacuum evaporation, ionic group bundle deposition, ion plating, dc sputtering deposition, RF sputter coating, ion beam sputtering deposition, ion beam assisted depositing, plasma reinforced chemical vapour deposition, high density inductive coupling formula plasma source chemical vapor deposition, catalyst chemical vapor deposition, magnetron sputtering, plating, spin coating, dip-coating, inkjet printing, roller coat, the LB film.
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