CN103630572A - Preparation method of porous silicon/tungsten oxide nanowire composite structure for gas-sensitive material - Google Patents
Preparation method of porous silicon/tungsten oxide nanowire composite structure for gas-sensitive material Download PDFInfo
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- CN103630572A CN103630572A CN201310498459.4A CN201310498459A CN103630572A CN 103630572 A CN103630572 A CN 103630572A CN 201310498459 A CN201310498459 A CN 201310498459A CN 103630572 A CN103630572 A CN 103630572A
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Abstract
The invention discloses a preparation method of a porous silicon/tungsten oxide nanowire composite structure for a gas-sensitive material, which comprises the following steps: with p-type monocrystal silicon as a substrate, preparing a porous silicon layer on the surface of the substrate by a double-groove electrochemical process; with metal tungsten as a target material, depositing a metal tungsten film on the surface of the porous silicon by a magnetron sputtering process; finally, in a horizontal tubular furnace, preparing a gas-sensitive material with a porous silicon/tungsten oxide nanowire composite structure at 600-750 DEG C by taking argon as a working gas and oxygen as a reaction gas. By adopting the method disclosed by the invention, the growth temperature of the prepared tungsten oxide nanowire is reduced, the specific surface area of the gas-sensitive material with a composite structure is remarkably increased, and the sensitivity on the 2ppm NO2 at 150 DEG C is 4.76; the method has the advantages of simple preparation process, easiness in control, low cost, high-sensitivity detection on NO2 and the like.
Description
Technical field
The invention relates to gas sensitive, relate in particular to the preparation method of a kind of porous silicon and tungsten oxide nano composite structure gas sensitive.
Background technology
Improving constantly of the development of industrial technology and people's living standard, the toxic and harmful bringing in productive life process and inflammable gas are (as NO
2, NH
3, CO and H
2deng) roll up, in contaminated environment, also the mankind's health and safety in serious threat.For this reason, along with scientific and technical progress, in the raising and environmental consciousness enhancing of people's living standard, requirement to the detection of toxic and harmful and inflammable gas, monitoring, warning is more and more higher, this just has higher requirement to detecting the gas sensitive rely on, for the research and development of the gas sensitive of novel high-performance provide wide space.
In recent years, tungsten oxide is considered to the semi-conductor gas sensitive material that the utmost point has research and application prospect.Tungsten oxide belongs to N-shaped wide bandgap semiconductor, in fields such as gas sensor, photoelectric device and photocatalysis, is all widely used, and especially as a kind of high-performance gas sensitive, can the various poisonous and dangerous gas of high sensitivity detection, as NO
2, H
2s, Cl
2, NH
3deng.Yet tungsten oxide working temperature makes need to consider heating arrangement based on tungsten oxide gas-sensitive sensor structure far above this feature of room temperature (200 ℃～300 ℃), this has increased the power consumption of sensor greatly.There are some researches show, one dimension tungsten oxide nanometer structure is compared with traditional tungsten oxide material, it is comparable that it has larger specific surface area and the size on specific direction and Debye length, thereby show higher adsorption ability, accelerate with gas between react, and then show higher sensitivity, response and lower working temperature faster.
Porous silicon is the adjustable poriness open structure material of a kind of aperture size being formed by etching at silicon chip surface, the duct degree of depth and porosity, it has unique pore passage structure, excellent electrology characteristic, high surfactivity, at room temperature can detect NO2, NH3, H2S and multiple organic gas, and manufacture craft is easy and microelectronic process engineering is compatible.But porous silicon also exists the relatively low defect of sensitivity, restricted to a certain extent it in the practical application of gas sensing field.
Adopt the compound tungsten oxide nano that supports of porous silicon to form composite structure gas sensitive, in whiles of the advantage on air-sensitive performance in conjunction with both, make to form heterojunction between two kinds of semiconductor materials of porous silicon and tungsten oxide, because whole nanometer cooperative effect obtains the not available gas-sensitive property of homogenous material, yet the research at home and abroad of the composite air-sensitive material based on porous silicon and tungsten oxide nanometer material is less.Tungsten powder has been usingd as tungsten source in this seminar, adopt the method for chemical vapor deposition to prepare porous silicon/tungsten oxide nanometer rod (line) composite structure gas sensitive, but the growth temperature too high (being greater than 1100 ℃) of preparing tungsten oxide nanometer rod (line) has restricted the practical application of porous silicon/tungsten oxide nanometer rod (line) composite structure gas sensitive.The present invention is in conjunction with the features of porous silicon and tungsten oxide nano, under the condition of 700 ℃ and blanket gas, adopt the method for thermal annealing W film that tungsten oxide nano and porous silicon assembling is compound, prepare a kind of novel porous silicon/tungsten oxide nano sandwich, greatly reduce the growth temperature of tungsten oxide nano; Meanwhile, this compound structure for new residence gas sensitive, because having huge specific surface area and large surfactivity, is expected to reduce working temperature, develops low temperature and surveys gas sensitive.
Summary of the invention
Object of the present invention, to overcome the shortcoming that single gas sensitive exists, provide a kind of novel method with thermal annealing W film that tungsten oxide nano and porous silicon assembling is compound, to prepare a kind of novel porous silicon/tungsten oxide nano composite structure gas sensitive, when tungsten oxide nano growth temperature is prepared in reduction, can significantly improve the specific surface area of composite structure sensitive material, and utilize the heterojunction that electric charge transfer formation occurs between two kinds of semiconductor materials, thereby further improve the response to probe gas.Preparation condition is easy to control, and technique is simple, and the composite structure gas sensitive making has important value and Research Significance.
The present invention is achieved by following technical solution.
A preparation method for porous silicon/tungsten oxide nano composite structure of gas sensitive, has following steps:
(1) clean silicon chip substrate
It by resistivity, is the p-type monocrystalline silicon substrate of the single-sided polishing of 10～15 Ω cm, prior to soaking in the concentrated sulphuric acid and mixed solution of hydrogen peroxide 30～50 minutes, through hydrofluoric acid aqueous solution immersion 20～40 minutes, acetone solvent ultrasonic cleaning 5～15 minutes, absolute ethyl alcohol ultrasonic cleaning 5～15 minutes, deionized water for ultrasonic, clean 5～15 minutes again, to remove surface and oil contaminant, organic impurities and surface oxide layer;
(2) at the bottom of preparing porous silicon-base
The silicon chip polished surface that adopts double flute electrochemical erosion method to clean in step (1) is prepared porous silicon layer, corrosion electrolytic solution used is that 1:2 forms by the hydrofluorite of massfraction 40% and the dimethyl formamide of massfraction 40% according to volume ratio, not adding surfactant and additional optical shines, the corrosion electric current density applying is 50～120mA/cm2, and etching time is 5～20min;
(3) prepare porous silicon and W film sandwich
At the bottom of the porous silicon-base that step (2) is made, be placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment.Adopt tungsten as target, using argon gas as working gas, argon gas flow is 30～50sccm, sputter operating pressure is 2.0Pa, sputtering power 80～100W, sputtering time 15～30min, substrate temperature is room temperature, at porous silicon surface plated metal W film, prepare W film and porous silicon sandwich;
(4) prepare porous silicon and tungsten oxide nano composite structure gas sensitive
W film and porous silicon sandwich prepared by step (3) are placed in horizontal pipe furnace, utilize the method for thermal annealing, using argon gas as working gas, oxygen is as reacting gas, it is 30～40sccm and 0.05～0.1sccm that gas flow is controlled respectively, and annealing temperature is 600～750 degree, and temperature retention time is 50～80min, body vacuum tightness is 1～5Pa, and operating pressure is 120～200Pa.
Ordered porous silicon average pore size 1～2 μ m in silica-based micron-scale duct prepared by described step (2), thickness is 8～15 μ m, porosity is 35～45%.
The preparation condition of described step (3) is: the tungsten target of employing is quality purity 99.95%, and the argon gas that the quality purity of usining is 99.999% is as working gas, base vacuum degree 4～6 * 10
-4pa, the W film thickness 100～200nm that adopts radio-frequency magnetron sputter method to prepare.
The vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (3) is the vacuum chamber institute of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment
Tungsten oxide nanometer linear diameter prepared by described step (4) is 20～40nm, and length is 1～2 μ m.
The horizontal pipe furnace that described step (4) adopts is GSL-1400X tubular furnace.
Compared with the prior art, beneficial effect is as follows in the present invention:
(1) provide a kind of under cryogenic conditions (700 ℃) prepare one dimension tungsten oxide nanometer line method, the porous silicon with large specific surface area and gas diffusion paths of formation and the composite structure of tungsten oxide nano, be highly suitable for as gas sensitive.
(2) advantages such as to have equipment simple, easy to operate for preparation method, and technological parameter is easy to control, with low cost.
Accompanying drawing explanation
Fig. 1 is the prepared porous silicon of embodiment 1 and tungsten film composite structure surface scan electron micrograph;
Fig. 2 is the prepared porous silicon of embodiment 1 and tungsten oxide nano composite structure surface electron scanning micrograph;
Fig. 3 is the prepared porous silicon of embodiment 1 and tungsten oxide nano composite structure profile scanning electron micrograph;
Fig. 4 is that the prepared porous silicon/tungsten oxide nano sandwich of embodiment 1 is 150 ℃ of air-sensitive test results to gas with various.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
1) clean silicon chip substrate
By resistivity, be 10 Ω cm, thickness is 400 μ m, (100) monocrystalline silicon piece of 2 of crystal orientation cun of p-type single-sided polishings, cut into the rectangular silicon substrate that is of a size of 2.4cm * 0.9cm, through the concentrated sulphuric acid and mixed solution of hydrogen peroxide immersion 30 minutes, hydrofluoric acid aqueous solution immersion 20 minutes, acetone solvent ultrasonic cleaning 15 minutes, absolute ethyl alcohol ultrasonic cleaning 15 minutes, deionized water for ultrasonic, clean 15 minutes successively.
2) prepare porous silicon
Utilize double flute electrochemical process to prepare porous silicon layer at the polished surface of silicon chip.Corrosion electrolytic solution used is comprised of the hydrofluorite of massfraction 40% and the dimethyl formamide of massfraction 40%, and its volume ratio is 1:2, does not add surfactant and additional optical photograph, and the corrosion electric current density applying is 60mA/cm
2, etching time is 10min.
3) prepare porous silicon/tungsten film composite structure material
The porous silicon making in step (2) is placed in to the vacuum chamber of DPS-III ultrahigh vacuum facing-target magnetron sputtering system equipment.Base vacuum degree 4.5 * 10
-4pa, adopt the tungsten of quality purity 99.95% as target, the argon gas that the quality purity of usining is 99.999% is as working gas, argon gas flow is 45sccm, and sputter operating pressure is 2.0Pa, sputtering power 90W, sputtering time 25min, substrate temperature is room temperature, the tungsten film that is 200nm at porous silicon surface sputter thickness, and its microscopic appearance is as shown in Figure 1.
4) prepare porous silicon/tungsten oxide nano composite structure gas sensitive
W film prepared by step (3) and porous silicon composite structure are placed in center, horizontal pipe furnace flat-temperature zone, pass into after argon gas cleans boiler tube 20min and be evacuated to the interior vacuum of stove at 2Pa, pass into quality purity and be the mixed gas of the oxygen that 99.999% argon gas and quality purity are 99.999%, gas flow is respectively 40sccm and 0.1sccm, and adjustments of gas valve makes pressure in stove remain on 150Pa; The speed of 10 ℃/min of take is heated to growth temperature as 700 ℃, after constant temperature 60min, at mixed-gas atmosphere, drops to room temperature, make the composite structure of tungsten oxide nano and porous silicon, its result is as shown in Fig. 2～3, and the diameter of tungsten oxide nano is 20～40nm, and length is 1-～2 μ m.
The air-sensitive method of testing of the quick material of porous silicon/tungsten oxide nano composite structure:
The porous silicon making in step (4) and tungsten oxide nano composite structure are placed in to the vacuum chamber of DPS-III ultrahigh vacuum facing-target magnetron sputtering system equipment.Base vacuum degree 4.5 * 10
-4pa, adopt the metal platinum of quality purity 99.95% as target, the argon gas that the quality purity of usining is 99.999% is as working gas, argon gas flow is 24sccm, and sputter operating pressure is 2.0Pa, sputtering power 90W, sputtering time 8min, substrate temperature is room temperature, and at a pair of square platinum electrode that is of a size of 0.2cm * 0.2cm of tungsten oxide film surface sputtering, electrode separation is 0.8cm.Adopt static gas distributing system under the condition of 150 ℃ to gas (NO to be measured
2, NH
3, ethanol and methyl alcohol) detect, its air-sensitive test result is as shown in Figure 4.
Embodiment 2
The present embodiment is similar to embodiment 1, and difference is: in step 3), the growth temperature of tungsten oxide nano is 650 ℃, makes porous silicon/tungsten oxide nano composite structure gas sensitive, and it is to 2ppm NO
2sensitivity be 1.26.
Embodiment 3
The present embodiment is similar to embodiment 1, and difference is: in step 3), the growth temperature of tungsten oxide nano is 750 ℃, makes porous silicon/tungsten oxide nano composite structure gas sensitive, and it is to 2ppm NO
2sensitivity be 2.46.
Claims (6)
1. for a preparation method for porous silicon/tungsten oxide nano composite structure of gas sensitive, there are following steps:
(1) clean silicon chip substrate
It by resistivity, is the p-type monocrystalline silicon substrate of the single-sided polishing of 10～15 Ω cm, prior to soaking in the concentrated sulphuric acid and mixed solution of hydrogen peroxide 30～50 minutes, through hydrofluoric acid aqueous solution immersion 20～40 minutes, acetone solvent ultrasonic cleaning 5～15 minutes, absolute ethyl alcohol ultrasonic cleaning 5～15 minutes, deionized water for ultrasonic, clean 5～15 minutes again, to remove surface and oil contaminant, organic impurities and surface oxide layer;
(2) at the bottom of preparing porous silicon-base
The silicon chip polished surface that adopts double flute electrochemical erosion method to clean in step (1) is prepared porous silicon layer, corrosion electrolytic solution used is that 1:2 forms by the hydrofluorite of massfraction 40% and the dimethyl formamide of massfraction 40% according to volume ratio, not adding surfactant and additional optical shines, the corrosion electric current density applying is 50～120mA/cm2, and etching time is 5～20min;
(3) prepare porous silicon and W film sandwich
At the bottom of the porous silicon-base that step (2) is made, be placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment.Adopt tungsten as target, using argon gas as working gas, argon gas flow is 30～50sccm, sputter operating pressure is 2.0Pa, sputtering power 80～100W, sputtering time 15～30min, substrate temperature is room temperature, at porous silicon surface plated metal W film, prepare W film and porous silicon sandwich;
(4) prepare porous silicon and tungsten oxide nano composite structure gas sensitive
W film and porous silicon sandwich prepared by step (3) are placed in horizontal pipe furnace, utilize the method for thermal annealing, using argon gas as working gas, oxygen is as reacting gas, it is 30～40sccm and 0.05～0.1sccm that gas flow is controlled respectively, and annealing temperature is 600～750 degree, and temperature retention time is 50～80min, body vacuum tightness is 1～5Pa, and operating pressure is 120～200Pa.
2. according to the preparation method of the porous silicon/tungsten oxide nano composite structure for gas sensitive of claim 1, it is characterized in that, ordered porous silicon average pore size 1～2 μ m in silica-based micron-scale duct prepared by described step (2), thickness is 8～15 μ m, porosity is 35～45%.
3. according to the preparation method of the porous silicon/tungsten oxide nano composite structure for gas sensitive of claim 1, it is characterized in that, the preparation condition of described step (3) is: the tungsten target of employing is quality purity 99.95%, the argon gas that the quality purity of usining is 99.999% is as working gas, base vacuum degree 4～6 * 10
-4pa, the W film thickness 100～200nm that adopts radio-frequency magnetron sputter method to prepare.
4. according to the preparation method of the porous silicon/tungsten oxide nano composite structure for gas sensitive of claim 1, it 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 institute of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
5. according to the preparation method of the porous silicon/tungsten oxide nano composite structure for gas sensitive of claim 1, it is characterized in that, tungsten oxide nanometer linear diameter prepared by described step (4) is 20～40nm, and length is 1～2 μ m.
6. according to the preparation method of the porous silicon/tungsten oxide nano composite structure for gas sensitive of claim 1, it is characterized in that, the horizontal pipe furnace that described step (4) adopts is GSL-1400X tubular furnace.
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| CN103903664A (en) * | 2014-04-17 | 2014-07-02 | 武汉大学 | Irradiation resistance nano-porous membrane |
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| CN104445047A (en) * | 2014-11-05 | 2015-03-25 | 天津大学 | Tungsten oxide/vanadium oxide heterojunction nanowire array and manufacturing method thereof |
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| CN108376641A (en) * | 2018-02-05 | 2018-08-07 | 天津理工大学 | A method of Cu doped indium oxide nano wires are prepared based on controllable porous substrate |
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| CN108931560A (en) * | 2018-05-23 | 2018-12-04 | 西安交通大学 | A kind of preparation method based on monodimension nanometer material sensor |
| CN114441599A (en) * | 2020-10-30 | 2022-05-06 | 天津大学 | Porous silicon-based VO2Preparation method of gas-sensitive sensing element with nano particle composite structure |
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Application publication date: 20140312 |