CN103063707A - Preparation method for gas-sensitive material with composite structure - Google Patents
Preparation method for gas-sensitive material with composite structure Download PDFInfo
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Abstract
The invention discloses a preparation method for a gas-sensitive material with a composite structure. The preparation method comprises the following steps: (1) successively placing an n-type single-side polished monocrystalline silicon chip into an acetone solvent, absolute ethyl alcohol and deionized water for ultrasonic cleaning, then soaking the monocrystalline silicon chip in 5% of an aqueous hydrofluoric acid solution, flushing the monocrystalline silicon chip with ionized water and standing the monocrystalline silicon chip for subsequent usage; (2) preparing a porous silicon layer on the polished surface of the cleaned silicon chip by using a double-tank electrochemical corrosion process, wherein corrosion current density is 115 to 135 mA/cm<2> and corrosion time is 20 to 25 min; and (3) with metal tungsten as a target material, sputtering and depositing a nanometer tungsten oxide film on the surface of silicon-based porous silicon and carrying out heat treatment at a temperature of 450 to 500 DEG C for 3 to 4 h so as to prepare the gas-sensitive material with the composite structure. The invention provides a method for preparing the nanometer tungsten oxide film with a loose porous surface and containing considerable oxygen vacancies, the method has the advantages of simple equipment, convenient operation, easily controllable technological parameters and low cost, and the nanometer tungsten oxide film is fairly applicable to the gas-sensitive material.
Description
Technical field
The invention relates to the composite structure gas sensitive, relate in particular to a kind of preparation method of porous silicon-base tungsten oxide composite structure gas sensitive.
Background technology
The develop rapidly of modern industrial technology has produced tremendous influence to the mankind's civilization and progress and ecologic environment, and a large amount of toxic and harmfuls and inflammable gas are (such as NO
2, NH
3, CO and H
2Deng) also human health and safety in serious threat in contaminated environment.Along with the raising of living standards of the people and the enhancing of environmental consciousness, also more and more higher to the requirement of ecologic environment.The detection technique of toxic and harmful more and more extensively is subject to worldwide concern and attention, numerous and confused policy and the examination criteria of being correlated with of formulating in various countries, and this just provides wide application prospect and important development meaning for novel air-sensitive developing material and research.
In recent years, tungsten oxide and porous silicon are considered to the semi-conductor gas sensitive material that the utmost point has research and application prospect.Tungsten oxide belongs to the N-shaped wide bandgap semiconductor, all is widely used in fields such as gas sensor, photoelectric device and photocatalysis, and especially as a kind of high-performance gas sensitive, but the various poisonous and dangerous gases of high sensitivity detection, such as NO
2, H
2S, Cl
2, NH
3Deng.Yet the tungsten oxide working temperature causes power consumption higher far above this shortcoming of room temperature (150 ℃ ~ 250 ℃), and makes the gas-sensitive sensor structure design need to consider heating arrangement.There are some researches show, the gas sensitization mechanism of tungsten oxide belongs to the surface resistance control type, based on oxygen and the tested gas modulated process at tungsten oxide grain surface generation chemical reaction effects on surface resistance, its sensitive property is directly related with factors such as its surface structure pattern, particle crystallinity, crystallite dimension and rete poriness to the detection of gas.
Porous silicon is a kind of adjustable poriness open structure material of aperture size, the duct degree of depth and porosity that is formed by etching at silicon chip surface, namely has very high surfactivity under the room temperature, can detect NO
2, NH
3, H
2S and multiple organic gas, and manufacture craft is easy and microelectronic process engineering is compatible.But also there is the relatively low shortcoming of sensitivity in porous silicon, has restricted to a certain extent practical application.
The composite structure gas sensitive forms heterojunction by two kinds of different Semiconductor gas sensors Material claddings of energy gap, because whole nanometer cooperative effect obtains the not available gas-sensitive property of homogenous material.Recent study personnel propose porous silicon carrying metal oxide is formed nano ordered compound substance, to have higher specific surface area, can significantly improve the sensitivity of gas sensitive, reduce response/release time, reduce working temperature, be expected to develop the high-performance gas sensitive that room temperature is surveyed.
Summary of the invention
Purpose of the present invention, to overcome the shortcoming that single gas sensitive exists, provide a kind of loose porous and contain the method for the tungsten oxide nanometer thin film in a large amount of oxygen room as substrate prepares take porous silicon, can significantly improve the specific surface area of sensitive material, and utilize the redox-potential that electric charge shifts the heterojunction change tungsten oxide film surface that forms occurs between two kinds of semiconductor materials, thereby further improve the response to probe gas.
The present invention is achieved by following technical solution.
A kind of preparation method of composite structure gas sensitive has following steps:
(1) cleans the silicon chip substrate
Monocrystalline silicon piece with the N-shaped single-sided polishing, cut into the rectangular silicon substrate that is of a size of 2.0 ~ 2.4cm * 0.8 ~ 0.9cm, again the silicon chip substrate is put into successively the respectively ultrasonic cleaning 10 ~ 20 minutes of acetone solvent, absolute ethyl alcohol, deionized water, removed surface and oil contaminant and organic impurities; Put into subsequently mass percent and be 5% hydrofluoric acid aqueous solution and soaked 15 ~ 30 minutes, remove the oxide layer on surface; Only for subsequent use with deionized water rinsing again;
(2) preparation porous silicon
Adopt the double flute electrochemical erosion method to prepare porous silicon layer at the silicon chip polished surface that cleaned, used corrosion electrolytic solution is that 40% hydrofluorite and deionized water form by mass percent, and volume ratio is 1:5, and the corrosion electric current density that applies is 115 ~ 135mA/cm
2, etching time is 20 ~ 25min;
(3) preparation composite structure gas sensitive
The silica-based porous silicon of step (2) preparation is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopting quality purity is that 99.95% tungsten is as target, take quality purity as 99.999% argon gas and oxygen as working gas and reacting gas, gas flow is controlled to be respectively 44.5 ~ 45.5sccm and 4.5 ~ 5.5sccm, sputtering power 90 ~ 100W, the sputter operating pressure is 1.0 ~ 2.0Pa, sputtering time is 5 ~ 15min, and body vacuum tightness is 2 ~ 4 * 10
-4Pa is at silica-based porous silicon surface sputtering sedimentation tungsten oxide nanometer thin film; The porous silicon-base tungsten oxide film that makes is placed the program sintering furnace, and in 450 ℃ ~ 500 ℃ air atmosphere thermal treatment 3 ~ 4h, the control heating rate is 2.5 ℃/min, makes the composite structure gas sensitive.
The monocrystalline silicon substrate substrate that described step (1) adopts, resistivity is 0.01 ~ 0.015 Ω cm, silicon chip thickness is 350 ~ 500 μ m.
The porous silicon average pore size 150 ~ 170nm of described step (2) preparation, porous silicon layer thickness is 65 ~ 70 μ m.
The vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (3) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
Compared with the prior art, beneficial effect of the present invention is:
(1) provide a kind of surface for preparing loose porous and contain the method for the tungsten oxide nanometer thin film in a large amount of oxygen room, the heterojunction composite structure that forms has huge specific surface area and gas diffusion paths, be highly suitable for gas sensitive, have important using value and Research Significance.
The advantages such as (2) to have equipment simple, easy to operate for the preparation method, and technological parameter is easy to control, and is with low cost.
Description of drawings
Fig. 1 is the prepared porous silicon-base tungsten oxide film electron scanning micrograph of embodiment 1;
Fig. 2 is the prepared porous silicon-base tungsten oxide film electron scanning micrograph of embodiment 2;
Fig. 3 is the prepared porous silicon-base tungsten oxide film electron scanning micrograph of embodiment 3;
Fig. 4 is the prepared porous silicon-base tungsten oxide film electron scanning micrograph of embodiment 4;
Fig. 5 is the prepared porous silicon-base tungsten oxide film electron scanning micrograph of embodiment 5;
Fig. 6 is the X-ray diffraction spectrogram of the prepared porous silicon-base tungsten oxide film of embodiment 1;
Fig. 7 is the Raman spectrogram of the prepared porous silicon-base tungsten oxide film of embodiment 1;
Fig. 8 is the prepared porous silicon-base tungsten oxide film W of embodiment 1
4fX-ray photoelectron can spectrogram;
Embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment.
The present invention is raw materials used all to adopt commercially available chemically pure reagent.
Embodiment 1
(1) cleans the silicon chip substrate
Be 0.01 Ω cm with resistivity, thickness is 400 μ m, (100) monocrystalline silicon piece of 2 of the crystal orientation cun N-shaped single-sided polishings, cut into the rectangular silicon substrate that is of a size of 2.4cm * 0.9cm, put into successively acetone solvent, absolute ethyl alcohol and deionized water and distinguish ultrasonic cleaning 20 minutes, put into subsequently massfraction and be 5% hydrofluoric acid aqueous solution and soaked 15 minutes, clean for subsequent use with deionized water again;
(2) preparation porous silicon
Utilize the double flute electrochemical process to prepare porous silicon layer at the polished surface of silicon chip.Used corrosion electrolytic solution is comprised of hydrofluorite and the deionized water of massfraction 40%, and volume ratio is 1:5, does not add surfactant and additional optical photograph, and the corrosion electric current density that applies is 125mA/cm
2, etching time is 20min; Wherein porous silicon forms the regional 1.6cm * 0.4cm that is.Recording average pore size is 170.28nm, and thickness is 68.78 μ m;
(3) preparation composite structure gas sensitive
The silica-based porous silicon of step (2) preparation is placed the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the tungsten target of quality purity 99.95%, body vacuum tightness is 3.7 * 10
-4Pa, take the argon gas of quality purity as 99.999% as working gas, take the oxygen of quality purity as 99.999% as reacting gas, gas flow is respectively 45sccm and 5sccm, and the sputter operating air pressure is 1.0Pa, sputtering power 100W, sputtering time is 9min, film thickness is about 35nm, forms tungsten oxide film in silica-based porous silicon surface sputter, and substrate temperature is room temperature.Subsequently the porous silicon-base tungsten oxide film that makes is placed the program sintering furnace, in 450 ℃ of air atmosphere thermal treatment 4h, the control heating rate is 2.5 ℃/min.
The scanning electron microscope analysis result of the composite structure gas sensitive surface topography that embodiment 1 is prepared as shown in Figure 1, there is a large amount of channel-like structures in coarse and discontinuous tungsten oxide film, surface structure is extremely loose, specific surface area is very high and for gas diffusion provides a large amount of passages, and has formed the heterojunction nano composite structure with porous silicon layer.Fig. 6 is the X-ray diffractogram of the prepared composite structure gas sensitive of present embodiment, as seen from the figure, and the corresponding monocline WO in gained tungsten oxide diffractive features peak
290Standard card (010) and (403) crystal face, calculate its average grain size according to the Scherrer formula and be about 39.5nm, less crystallite dimension makes membrane structure more loose, thereby obtains to be conducive to gas absorption than bigger serface.Fig. 7 is the Raman spectrum of composite structure gas sensitive, and as seen from the figure, the frequency of five tungsten oxide peak lays respectively at 134cm
-1, 270cm
-1, 710cm
-1, 807cm
-1And 951cm
-1, show that the tungsten oxide structure that makes is monocline γ phase.Fig. 8 is the prepared composite structure gas sensitive W of present embodiment
4fX-ray photoelectron can spectrogram, as seen from the figure, a large amount of W
5+Existence show that more oxygen vacancy defect introduces, form non-stoichiometric WO
3-xStructure, it has than pure phase WO
3More surface state provides more reactivity position.
Embodiment 2
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 5min in the step (3), makes porous silicon-base tungsten oxide composite structure gas sensitive.The scanning electron microscope analysis result of surface topography as shown in Figure 2, tungsten oxide film is uniform fold not yet on the surface, has a large amount of holes.
Embodiment 3
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 8min in the step (3), makes porous silicon-base tungsten oxide composite structure gas sensitive.The scanning electron microscope analysis result of surface topography as shown in Figure 3, the film surface structure is very loose, has a large amount of darker holes.
Embodiment 4
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 10min in the step (3), makes porous silicon-base tungsten oxide composite structure gas sensitive.The scanning electron microscope analysis result of surface topography as shown in Figure 4, particle is reunited mutually, surfaceness is very high, has some holes.
Embodiment 5
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 13min in the step (3), makes porous silicon-base tungsten oxide composite structure gas sensitive.The scanning electron microscope analysis result of surface topography as shown in Figure 5, the film surface opposed flattened, the particle Contact is tight, forms continuous film.
Obviously, those skilled in the art can carry out various changes and modification to the preparation method of composite structure gas sensitive of the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these revise and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then all should be within protection scope of the present invention.
Claims (4)
1. the preparation method of a composite structure gas sensitive has following steps:
(1) cleans the silicon chip substrate
Monocrystalline silicon piece with the N-shaped single-sided polishing, cut into the rectangular silicon substrate that is of a size of 2.0 ~ 2.4cm * 0.8 ~ 0.9cm, again the silicon chip substrate is put into successively the respectively ultrasonic cleaning 10 ~ 20 minutes of acetone solvent, absolute ethyl alcohol, deionized water, removed surface and oil contaminant and organic impurities; Put into subsequently mass percent and be 5% hydrofluoric acid aqueous solution and soaked 15 ~ 30 minutes, remove the oxide layer on surface; Only for subsequent use with deionized water rinsing again;
(2) preparation porous silicon
Adopt the double flute electrochemical erosion method to prepare porous silicon layer at the silicon chip polished surface that cleaned, used corrosion electrolytic solution is that 40% hydrofluorite and deionized water form by mass percent, and volume ratio is 1:5, and the corrosion electric current density that applies is 115 ~ 135mA/cm
2, etching time is 20 ~ 25min;
(3) preparation composite structure gas sensitive
The silica-based porous silicon of step (2) preparation is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopting quality purity is that 99.95% tungsten is as target, take quality purity as 99.999% argon gas and oxygen as working gas and reacting gas, gas flow is controlled to be respectively 44.5 ~ 45.5sccm and 4.5 ~ 5.5sccm, sputtering power 90 ~ 100W, the sputter operating pressure is 1.0 ~ 2.0Pa, sputtering time is 5 ~ 15min, and body vacuum tightness is 2 ~ 4 * 10
-4Pa is at silica-based porous silicon surface sputtering sedimentation tungsten oxide nanometer thin film; The porous silicon-base tungsten oxide film that makes is placed the program sintering furnace, and in 450 ℃ ~ 500 ℃ air atmosphere thermal treatment 3 ~ 4h, the control heating rate is 2.5 ℃/min, makes the composite structure gas sensitive.
2. according to claim 1 a kind of preparation method of composite structure gas sensitive is characterized in that, the monocrystalline silicon substrate substrate that described step (1) adopts, and resistivity is 0.01 ~ 0.015 Ω cm, silicon chip thickness is 350 ~ 500 μ m.
3. according to claim 1 a kind of preparation method of composite structure gas sensitive is characterized in that, the porous silicon average pore size 150 ~ 170nm of described step (2) preparation, and porous silicon layer thickness is 65 ~ 70 μ m.
4. according to claim 1 a kind of preparation method of composite structure gas sensitive is characterized in that the vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (3) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278534A (en) * | 2013-05-11 | 2013-09-04 | 天津大学 | Preparation method of ammonia-sensitive sensor component at room temperature |
| CN103278537A (en) * | 2013-06-17 | 2013-09-04 | 天津大学 | Preparation method of gas-sensitive element for room-temperature ultrafast detection of nitrogen oxide gas |
| CN103526157A (en) * | 2013-10-21 | 2014-01-22 | 天津大学 | Preparation method of composite structure material based on silicon-based porous silicon/tungsten oxide nanowires |
| CN103760309A (en) * | 2014-01-23 | 2014-04-30 | 天津大学 | Preparation method for porous-silicon-based vanadium oxide nano rod composite structure |
| CN104198532A (en) * | 2014-09-05 | 2014-12-10 | 中国石油大学(华东) | Molybdenum disulfide thin film device with ammonia sensitive effect as well as preparation method and application thereof |
| CN105486820A (en) * | 2016-01-13 | 2016-04-13 | 时建华 | Outdoor video surveillance equipment with gas detection function |
| CN105513810A (en) * | 2016-01-13 | 2016-04-20 | 肖锐 | Oil tank with high-repetitiveness detection function of refueling station |
| CN105513811A (en) * | 2016-01-13 | 2016-04-20 | 周丽娜 | Camping tent with high-repetitiveness gas detection function |
| CN105655137A (en) * | 2016-01-13 | 2016-06-08 | 潘燕 | Outdoor communication device based on self-powered detection |
| CN105673377A (en) * | 2016-01-13 | 2016-06-15 | 吴本刚 | Metering refueling pump based on high-efficiency solar cell |
| CN105674192A (en) * | 2016-01-13 | 2016-06-15 | 蔡雄 | Solar street lamp with high-sensitivity detecting function |
| CN105675662A (en) * | 2016-01-13 | 2016-06-15 | 蔡权 | Building roof decorative material based on self-power detection |
| CN105702471A (en) * | 2016-01-13 | 2016-06-22 | 杨炳 | Greenhouse based on self-energized detection |
| CN105699436A (en) * | 2016-01-13 | 2016-06-22 | 钟林超 | Exhaust gas detection device based on solar cell high in conversion rate |
| CN108982599A (en) * | 2017-06-05 | 2018-12-11 | 天津师范大学 | Porous silicon-base tungsten oxide film composite material gas sensor and its preparation method and application |
| CN109813776A (en) * | 2017-11-20 | 2019-05-28 | 天津师范大学 | Intermediate pore size porous silicon-base zinc oxide films film composite material gas sensor and its preparation method and application |
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Cited By (17)
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| CN103278534A (en) * | 2013-05-11 | 2013-09-04 | 天津大学 | Preparation method of ammonia-sensitive sensor component at room temperature |
| CN103278537A (en) * | 2013-06-17 | 2013-09-04 | 天津大学 | Preparation method of gas-sensitive element for room-temperature ultrafast detection of nitrogen oxide gas |
| CN103526157A (en) * | 2013-10-21 | 2014-01-22 | 天津大学 | Preparation method of composite structure material based on silicon-based porous silicon/tungsten oxide nanowires |
| CN103760309A (en) * | 2014-01-23 | 2014-04-30 | 天津大学 | Preparation method for porous-silicon-based vanadium oxide nano rod composite structure |
| CN104198532A (en) * | 2014-09-05 | 2014-12-10 | 中国石油大学(华东) | Molybdenum disulfide thin film device with ammonia sensitive effect as well as preparation method and application thereof |
| CN105486820A (en) * | 2016-01-13 | 2016-04-13 | 时建华 | Outdoor video surveillance equipment with gas detection function |
| CN105513810A (en) * | 2016-01-13 | 2016-04-20 | 肖锐 | Oil tank with high-repetitiveness detection function of refueling station |
| CN105513811A (en) * | 2016-01-13 | 2016-04-20 | 周丽娜 | Camping tent with high-repetitiveness gas detection function |
| CN105655137A (en) * | 2016-01-13 | 2016-06-08 | 潘燕 | Outdoor communication device based on self-powered detection |
| CN105673377A (en) * | 2016-01-13 | 2016-06-15 | 吴本刚 | Metering refueling pump based on high-efficiency solar cell |
| CN105674192A (en) * | 2016-01-13 | 2016-06-15 | 蔡雄 | Solar street lamp with high-sensitivity detecting function |
| CN105675662A (en) * | 2016-01-13 | 2016-06-15 | 蔡权 | Building roof decorative material based on self-power detection |
| CN105702471A (en) * | 2016-01-13 | 2016-06-22 | 杨炳 | Greenhouse based on self-energized detection |
| CN105699436A (en) * | 2016-01-13 | 2016-06-22 | 钟林超 | Exhaust gas detection device based on solar cell high in conversion rate |
| CN105486820B (en) * | 2016-01-13 | 2017-12-01 | 南京波瑞自动化科技有限公司 | A kind of outdoor video monitoring device with gas detection function |
| CN108982599A (en) * | 2017-06-05 | 2018-12-11 | 天津师范大学 | Porous silicon-base tungsten oxide film composite material gas sensor and its preparation method and application |
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Application publication date: 20130424 |