CN102768227A - Production method of dye-sensitized TiO2 film based gas sensor - Google Patents
Production method of dye-sensitized TiO2 film based gas sensor Download PDFInfo
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- CN102768227A CN102768227A CN2012101886754A CN201210188675A CN102768227A CN 102768227 A CN102768227 A CN 102768227A CN 2012101886754 A CN2012101886754 A CN 2012101886754A CN 201210188675 A CN201210188675 A CN 201210188675A CN 102768227 A CN102768227 A CN 102768227A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
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Abstract
The invention discloses a production method of a dye-sensitized TiO2 film based gas sensor. The method comprises steps of: choosing a substrate suitable for subsequent film plating; preparing electrodes on the substrate through a film plating method; preparing a nanocrystalline TiO2 film on the substrate with electrodes by a magnetron sputtering method; selecting a suitable dye sensitizing material according to gas to be tested and dissolving the dye sensitizing material in a compatible solvent to prepare a dye solution; immersing the nanocrystalline TiO2 film into the dye solution for 12-8 h; taking out the nanocrystalline TiO2 film; removing impurities with ethanol; and drying and baking in an oven at 30-80 DEG C for 1-5 h. According to the invention, the nanocrystalline TiO2 film is employed as the substrate material, and the dye sensitizing material is employed as a sharpening material; dye molecules encapsulate the TiO2 molecules while filling gaps between the TiO2 crystals; and the gas sensor can be used for qualitative and quantitative analysis on gas at room temperature through changes of the sensor resistance, and has high sensitivity and wide detection range.
Description
Technical field
The present invention relates to a kind of method for making of gas sensor, refer in particular to and be used in magnetron sputtering titania (TiO
2) add the method for making of the gas sensor of pigment in the gas sensitization film.
Background technology
In recent years, along with development of science and technology, people are increasingly high to requiring of detecting of harmful gas, and are also more and more to the demand of gas sensor.Present gas sensor exists the not high enough deficiency of light concentration gas detection sensitivity mostly.For overcoming above weak point, in gas sensor, mix other metal or oxide addition, preparation composite metal oxide gas-sensing material etc. has been obtained comparatively ideal effect.Wherein, TiO
2Film has high index of refraction; Characteristics such as high-k; For example: Chinese patent number is called the preparation method of titanium dioxide porous film for ZL201010206483.2, name, and Chinese patent ZL200510012254.6, name are called the preparation method that electrophoretic deposition low temperature prepares TiO 2 nanocrystal porous film electrode.Magnetron sputtering method prepares nanocrystalline TiO
2Thin-film technique is simple, the nanocrystalline TiO that makes
2Film is evenly distributed, controllable thickness, surface area big, strong adhesion, do not ftracture; In large-scale industrial production, be more prone to control the quality of product; And reduce comprehensive production cost, but this gas sensor needs could work under the high temperature (200 ℃ ~ 600 ℃)
After being meant those and base material combines, can effectively improve dye-sensitized material the pigment of base material electric conductivity; Comprise synthetic dyestuff sensitized material and natural colouring matter sensitized material; Synthetic dyestuff sensitized material such as metal organic complex and organic compound; The color composition of natural colouring matter sensitized material is anthocyanidin mostly, and they all can present various colors under different pH values or in the different oxidation restoring system.
Summary of the invention
It is a kind of based on dye-sensitized nanocrystalline TiO that the present invention provides
2The gas sensor method for making of film is with dye-sensitized material and nanocrystalline TiO
2Film combines, and the gas sensitivity of made is high and can at room temperature work.
The technical scheme that the present invention adopts is may further comprise the steps: the substrate of follow-up plated film is selected to be suitable in (1), on substrate, makes electrode through film plating process, and the substrate that is coated with electrode is prepared nanocrystalline TiO through magnetron sputtering method
2Film; (2) select suitable dye-sensitized material to the gas of required detection and with dye-sensitized material dissolves in compatible with it solvent, process pigment solution; (3) with said nanocrystalline TiO
2Film is put into said pigment solution and is soaked taking-up after 12 ~ 48 hours, with absolute ethyl alcohol impurity is rinsed well, in 30 ~ 80 ℃ of baking ovens, dries by the fire 1 ~ 5h after drying and gets final product.
Further, said magnetron sputtering method prepares nanocrystalline TiO
2The method of film is following: the substrate that will be coated with electrode is put into the base material objective table; With Titanium or titanium dioxide as the target platform; The distance of regulating between titanium target and the base material objective table is 20 ~ 30cm, and the speed of rotation of objective table is 4 ~ 8rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 20 ~ 250 ℃, and inert gas flow is 60 ~ 100sccm, and magnetron sputtering power is 80 ~ 120w, sputter 15 ~ 60min under 0.5 ~ 2.0Pa pressure.
Further; Said dye-sensitized material comprises synthetic dyestuff sensitized material and natural colouring matter sensitized material; When adopting the synthetic dyestuff sensitized material; The concentration of the pigment solution of processing is 0.1mol/L ~ 0.5mol/L, and when adopting the natural colouring matter sensitized material, the pigment solution water percentage is 60% ~ 80%.
Beneficial effect of the present invention: the present invention prepares nanocrystalline TiO with magnetron sputtering
2Film uses nanocrystalline TiO
2Film uses dye-sensitized material as intensifying the material gas sensor as base material; Dye-sensitized material is fixed in nanocrystalline TiO
2On the film, pigment molecular has wrapped up TiO
2Filled TiO in the time of molecule
2Gap between the crystal has changed TiO
2The lattice resistance of crystal; When strengthening it it can be worked at normal temperatures to the susceptibility of gas molecule; Can at room temperature pass through the variation qualitative, quantitative ground analytical gas of sensor resistance; Comparing with other gas sensor has the higher sensitivity and the sensing range of broad, and favorable reproducibility can detect the imperceptible gas concentration of people's sense of smell.
Description of drawings
Fig. 1 is the substrate synoptic diagram that is coated with electrode;
Fig. 2 is for scribbling nanocrystalline TiO
2The sensor synoptic diagram of film;
Fig. 3 is for scribbling nanocrystalline TiO
2The sensor synoptic diagram of film and pigment;
Among the figure: 1. substrate; 2. electrode; 3. nanocrystalline TiO
2Film; 4. uvea.
Embodiment
The method for making of gas sensor of the present invention comprises that substrate selection, making electrode, magnetron sputtering method prepare nanocrystalline TiO
2Fixing these five steps of film, dye-sensitized material chosen and dissolving, dye-sensitized material.
Substrate selects to be meant the substrate material of selecting to be suitable for follow-up plated film that substrate can be silicon chip, glass sheet, electro-conductive glass sheet or teflon plate.
Making electrode is meant on substrate 1 through film plating process making electrode 2.As making gold or platinum electrode, the substrate 1 that is coated with gold or platinum electrode 2 as shown in Figure 1 through screen printing technique.
Through plasma sputtering method nanocrystalline TiO of sputter on the substrate that is coated with gold or platinum electrode
2Film, magnetron sputtering method prepare nanocrystalline TiO
2The method of film is following: the substrate 1 that will be coated with electrode is put into the base material objective table; With Titanium or titanium dioxide as the target platform; The distance of regulating between titanium target and the base material objective table is 20 ~ 30cm, and the speed of rotation of objective table is 4 ~ 8rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 20 ~ 250 ℃, inert gas flow 60 ~ 100sccm, magnetron sputtering power 80 ~ 120w, under 0.5 ~ 2.0Pa pressure, sputter 15 ~ 60min obtains the nanocrystalline TiO that scribbles as shown in Figure 2
2The sensor of film 3.
Dye-sensitized material chosen and dissolving comprise to the gas of required detection select suitable dye-sensitized material and with dye-sensitized material dissolves in suitable solvent.Select the stronger redox indicator of those sensitization property when detecting reducibility gas, indigo like phenosafraine, methylene blue, tetrasulfonic acid base, and with selected dye-sensitized material dissolves in compatible with it solvent, process pigment solution.Dye-sensitized material comprises synthetic dyestuff sensitized material and natural colouring matter sensitized material; When adopting the synthetic dyestuff sensitized material; The concentration of the pigment solution that forms is 0.1mol/L ~ 0.5mol/L; When adopting the natural colouring matter sensitized material, the dye-sensitized material of concentrated natural to make the pigment solution water percentage is 60% ~ 80%.
Dye-sensitized material fixing means is following: the nanocrystalline TiO that will process
2 Film 3 is put into the pigment solution of processing and is soaked taking-up after 12 ~ 48 hours, with absolute ethyl alcohol impurity is rinsed well, in 30 ~ 80 ℃ of baking ovens, dries 1 ~ 5h after in dry air, drying and gets final product, and obtains the nanocrystalline TiO that scribbles as shown in Figure 3
2The sensor of film and pigment, the 4th, uvea.
The present invention makes electrode 2 through the method with ion plating on substrate 1, prepares nanocrystalline TiO with magnetron sputtering method
2Film 3, dye-sensitized material is as intensifying the novel gas sensor of material.Nanocrystalline TiO
2 Film 3 helps the fixing of dye-sensitized material on the one hand, helps the enrichment of gas molecule on the other hand.Be adsorbed on nanocrystalline TiO
2Gas molecule on the film 3 makes the charge migration of the electric charge generative center ion of dye-sensitized material to part with after dye-sensitized material contacts, and the electric charge of transfer excites TiO
2The lattice resistance of crystal changes its susceptibility to gas.When therefore new gas sensor of the present invention and scent molecule reacted, its electric conductivity changed at normal temperatures.
6 embodiment of the present invention below are provided:
Present embodiment is to use synthetic dyestuff sensitized material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
1, selects wherein a kind of of silicon chip, glass sheet, electro-conductive glass sheet, teflon plate as substrate.
2, make gold or platinum electrode through serigraphy or plasma sputtering method, substrate 1 and electrode 2 as shown in Figure 1.
3, magnetron sputtering method prepares nanocrystalline TiO
2Film: substrate 1 is put into the base material objective table, and Titanium or titanium dioxide are as the target platform, and the distance of regulating between titanium target and the base material objective table is 20cm, and the speed of rotation of objective table is 4rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 20 ℃, inert gas flow 60sccm, magnetron sputtering power 80w, under 0.5Pa pressure, sputter 15min obtains the nanocrystalline TiO that scribbles as shown in Figure 2
2The sensor of film 3.
4, the selection of synthetic dyestuff sensitized material is an example with the methylene blue, selects methylene blue to be dissolved into the pigment solution that forms 0.1mol/L in the water as dye-sensitized material and with it.
5, dye-sensitized material is fixing: will process nanocrystalline TiO
2Film is put into the 0.1mol/L methylene blue solution and is soaked taking-up after 12 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 1h in 30 ℃ of baking ovens and promptly obtains required sensor as shown in Figure 3.In the present embodiment, if what select in the above-mentioned steps 4 is the formed solution of other synthetic dyestuff sensitized materials, this step method is constant.
Embodiment 2
Present embodiment is to use natural colouring matter dye material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
4, the extraction of the quick material of natural color and preparation: with the purple potato pigment is example, gets the purple potato of 10g and cleans, and is cut into the fourth shape and puts into tissue refiner and smash to pieces; Obtain slurries shape solution; Measure 10 milliliters of purple potatos with graduated cylinder and smash liquid to pieces, pour in the triangular flask, add 100 milliliter 1% citric acid again; Shake up, place 50 ℃ of thermostat water bath lixiviates 1 hour.After treating that raw material obviously fades, filter out extract with the qualitative filter paper of diameter 15cm, with the extract evaporation and concentration, being concentrated into water percentage is 60% with Rotary Evaporators, obtains required concentrated purple potato pigment solution.
5, look quick material is fixing: the nanocrystalline TiO that will process
2Film is put into concentrated purple potato pigment solution and is soaked taking-up after 12 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 1h in 30 ℃ of baking ovens and promptly obtains required sensor as shown in Figure 3.In the present embodiment, if what extract in the step 4 is the formed solution of the quick material of other natural colors, this step method is constant.
Present embodiment is to use synthetic dyestuff sensitized material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
1, selects wherein a kind of of silicon chip, glass sheet, electro-conductive glass sheet, teflon plate as substrate.
2, make gold or platinum electrode through serigraphy or plasma sputtering method, like substrate among Fig. 11 and electrode 2.
3, magnetron sputtering method prepares nanocrystalline TiO
2Film: substrate is put into the base material objective table, and Titanium or titanium dioxide are as the target platform, and the distance of regulating between titanium target and the base material objective table is 25cm, and the speed of rotation of objective table is 6rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 100 ℃, inert gas flow 80sccm, magnetron sputtering power 100w, under 1.0Pa pressure, sputter 30min obtains the nanocrystalline TiO that scribbles as shown in Figure 2
2The sensor of film 3.
4, the selection of synthetic dyestuff sensitized material is an example with the methylene blue, selects methylene blue to be dissolved into the pigment solution that forms 0.25mol/L in the water as dye-sensitized material and with it.
5, dye-sensitized material is fixing: will process nanocrystalline TiO
2Film is put into the 0.25mol/L methylene blue solution and is soaked taking-up after 24 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 3h in 60 ℃ of baking ovens and promptly obtains required sensor shown in Figure 3.In the present embodiment, if selection is other in the step 4
SyntheticThe formed solution of dye-sensitized material, this step method is constant.
Embodiment 4
Present embodiment is to use natural colouring matter material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
4, the extraction of the quick material of natural color and preparation: with the purple potato pigment is example, gets the purple potato of 15g and cleans, and is cut into the fourth shape and puts into tissue refiner and smash to pieces; Obtain slurries shape solution; Measure 15 milliliters of purple potatos with graduated cylinder and smash liquid to pieces, pour in the triangular flask, add 150 milliliter 3% citric acid again; Shake up, place 55 ℃ of thermostat water bath lixiviates 1.5 hours.After treating that raw material obviously fades, filter out extract with the qualitative filter paper of diameter 15cm, with the extract evaporation and concentration, being concentrated into water percentage is 70% with Rotary Evaporators, obtains required concentrated purple potato pigment solution.
5, look quick material is fixing: the nanocrystalline TiO that will process
2Film is put into concentrated purple potato pigment solution and is soaked taking-up after 24 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 4h in 60 ℃ of baking ovens and promptly obtains required sensor shown in Figure 3.In the present embodiment, if what extract in the step 4 is the formed solution of the quick material of other natural colors, this step method is constant.
Embodiment 5
Present embodiment is to use synthetic dyestuff sensitized material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
1, selects wherein a kind of of silicon chip, glass sheet, electro-conductive glass sheet, teflon plate as substrate.
2, make gold or platinum electrode through serigraphy or plasma sputtering method, like substrate among Fig. 11 and electrode 2.
3, magnetron sputtering method prepares nanocrystalline TiO
2Film: substrate is put into the base material objective table, and Titanium or titanium dioxide are as the target platform, and the distance of regulating between titanium target and the base material objective table is 30cm, and the speed of rotation of objective table is 8rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 250 ℃, inert gas flow 100sccm, magnetron sputtering power 120w, under 2.0Pa pressure, sputter 60min.Obtain the nanocrystalline TiO that scribbles as shown in Figure 2
2The sensor of film 3.
4, the selection of synthetic dyestuff sensitized material is an example with the methylene blue, selects methylene blue to be dissolved into the pigment solution that forms 0.5mol/L in the water as dye-sensitized material and with it.
5, dye-sensitized material is fixing: will process nanocrystalline TiO
2Film is put into the 0.5mol/L methylene blue solution and is soaked taking-up after 48 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 5h in 80 ℃ of baking ovens and promptly obtains required sensor as shown in Figure 3.In the present embodiment, if selection is other in the step 4
SyntheticThe formed solution of dye-sensitized material, this step method is constant.
Embodiment 6
Present embodiment is to use natural colouring matter dye material and nanocrystalline TiO
2The film making gas sensor that combines, making step is following:
4, the extraction of the quick material of natural color and preparation: with the purple potato pigment is example, gets the purple potato of 20g and cleans, and is cut into the fourth shape and puts into tissue refiner and smash to pieces; Obtain slurries shape solution; Measure 20 milliliters of purple potatos with graduated cylinder and smash liquid to pieces, pour in the triangular flask, add 200 milliliter 5% citric acid again; Shake up, place 60 ℃ of thermostat water bath lixiviates 2 hours.After treating that raw material obviously fades, filter out extract with the qualitative filter paper of diameter 15cm, with the extract evaporation and concentration, being concentrated into water percentage is 80% with Rotary Evaporators, obtains required concentrated purple potato pigment solution.
5, look quick material is fixing: the nanocrystalline TiO that will process
2Film is put into concentrated purple potato pigment solution and is soaked taking-up after 48 hours, with absolute ethyl alcohol impurity is rinsed well, in dry air, dries back oven dry 5h in 80 ℃ of baking ovens and promptly obtains required sensor as shown in Figure 3.In the present embodiment, if what extract in the step 4 is the formed solution of the quick material of other natural colors, this step method is constant.
Claims (4)
1. one kind based on dye-sensitized TiO
2The gas sensor method for making of film is characterized in that may further comprise the steps:
(1) selection is suitable for the substrate of follow-up plated film, on substrate, makes electrode through film plating process, and the substrate that is coated with electrode is prepared nanocrystalline TiO through magnetron sputtering method
2Film;
(2) select suitable dye-sensitized material to the gas of required detection and with dye-sensitized material dissolves in compatible with it solvent, process pigment solution;
(3) with said nanocrystalline TiO
2Film is put into said pigment solution and is soaked taking-up after 12 ~ 48 hours, with absolute ethyl alcohol impurity is rinsed well, in 30 ~ 80 ℃ of baking ovens, dries by the fire 1 ~ 5h after drying and gets final product.
2. gas sensor method for making according to claim 1 is characterized in that: said magnetron sputtering method prepares nanocrystalline TiO
2The method of film is following: the substrate that will be coated with electrode is put into the base material objective table; With Titanium or titanium dioxide as the target platform; The distance of regulating between titanium target and the base material objective table is 20 ~ 30cm, and the speed of rotation of objective table is 4 ~ 8rp, and magnetron sputtering reaction chamber vacuum tightness is extracted into 10 at least
-3Pa, temperature is heated to 20 ~ 250 ℃, and inert gas flow is 60 ~ 100sccm, and magnetron sputtering power is 80 ~ 120w, sputter 15 ~ 60min under 0.5 ~ 2.0Pa pressure.
3. gas sensor method for making according to claim 1; It is characterized in that: said dye-sensitized material comprises synthetic dyestuff sensitized material and natural colouring matter sensitized material; When adopting the synthetic dyestuff sensitized material; The concentration of the pigment solution of processing is 0.1mol/L ~ 0.5mol/L, and when adopting the natural colouring matter sensitized material, the pigment solution water percentage is 60% ~ 80%.
4. gas sensor method for making according to claim 1 is characterized in that: substrate is silicon chip, glass sheet, electro-conductive glass sheet or teflon plate, and electrode is gold or platinum electrode.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210188675.4A CN102768227B (en) | 2012-06-11 | 2012-06-11 | Production method of dye-sensitized TiO2 film based gas sensor |
| GB1421877.0A GB2518308B8 (en) | 2012-06-11 | 2012-11-28 | Method for manufacturing gas sensors based on dye-sensitized TIO2 film |
| PCT/CN2012/085448 WO2013185440A1 (en) | 2012-06-11 | 2012-11-28 | Method for manufacturing gas sensor based on dye-sensitized tio2 film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210188675.4A CN102768227B (en) | 2012-06-11 | 2012-06-11 | Production method of dye-sensitized TiO2 film based gas sensor |
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| CN102768227A true CN102768227A (en) | 2012-11-07 |
| CN102768227B CN102768227B (en) | 2015-04-22 |
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| CN201210188675.4A Active CN102768227B (en) | 2012-06-11 | 2012-06-11 | Production method of dye-sensitized TiO2 film based gas sensor |
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| Country | Link |
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| CN (1) | CN102768227B (en) |
| GB (1) | GB2518308B8 (en) |
| WO (1) | WO2013185440A1 (en) |
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| WO2013185440A1 (en) * | 2012-06-11 | 2013-12-19 | 江苏大学 | Method for manufacturing gas sensor based on dye-sensitized tio2 film |
| CN103575771A (en) * | 2013-11-20 | 2014-02-12 | 江苏大学 | Gas sensor and fabrication method thereof |
| CN104237325A (en) * | 2014-10-09 | 2014-12-24 | 扬州大学 | Preparation method of nitrogen dioxide sensing membrane based on dye-sensitized semiconductor |
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| CN104237325A (en) * | 2014-10-09 | 2014-12-24 | 扬州大学 | Preparation method of nitrogen dioxide sensing membrane based on dye-sensitized semiconductor |
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| Publication number | Publication date |
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| GB2518308A (en) | 2015-03-18 |
| GB201421877D0 (en) | 2015-01-21 |
| WO2013185440A1 (en) | 2013-12-19 |
| CN102768227B (en) | 2015-04-22 |
| GB2518308B8 (en) | 2021-02-10 |
| GB2518308A9 (en) | 2020-09-23 |
| GB2518308B (en) | 2020-12-09 |
| GB2518308A8 (en) | 2021-02-10 |
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