CN103245696A - Method for preparing porous silicon-based one-dimensional nanowire gas sensitive element - Google Patents
Method for preparing porous silicon-based one-dimensional nanowire gas sensitive element Download PDFInfo
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Abstract
The invention discloses a method for a preparing porous silicon-based one-dimensional nanowire gas sensitive element, wherein a silicon-based porous silicon composite one-dimensional tungsten oxide nano-structure which has the bore diameter in the range from 1 to 2 microns and also has highly orderly arranged ducts is taken as a gas sensitive element for the first time; due to huge specific surface area and high surface activity, lots of gas absorption positions and gas dispersion channels can be provided so that the gas sensitive element is easy to react with gas. The gas sensitive sensor element provided by the invention has high response value and good sensitivity and selectivity for low-concentration oxynitride gas at a low temperature (100 DEG C), and further is small in size, simple in structure, mature in fabrication process, convenient to use and low in price; as a result, the gas sensitive sensor element is expected to be popularized and applied to the field of the gas sensitive sensor.
Description
Technical field
The invention relates to gas sensor, relate in particular to a kind of can be in preparation method lower temperature work and that be applicable to the micron-scale duct porous silicon-base one dimension tungsten oxide nanometer structure gas sensor that detects oxides of nitrogen gas.
Background technology
Along with the develop rapidly of industrial technology and improving constantly of people's living standard, all gases pollutant that brings in the productive life process rolls up.Oxides of nitrogen (NO
x) as a kind of strong poisonous gas, be the main source of acid rain and photo-chemical smog, human beings'health and safety are constituted a serious threat.Therefore the detection to oxides of nitrogen gas becomes hot research in recent years.In recent years, continuous development along with nanometer technology, the nanostructured gas-sensitive sensor device has obtained significant progress, and especially in order to satisfy pressing for of commercial production and environment measuring, utilizing the metal-oxide semiconductor (MOS) nanostructured to prepare gas sensor becomes research emphasis.Tungsten oxide is a kind of N-type semiconductor material of broad stopband, has a wide range of applications at gas sensor and broadcasting and TV devices field, especially as a kind of high performance gas sensitive, can be widely used in various toxicity and dangerous gas such as NOx, SO
2, H
2Detections such as S.
For gas sensitive, tungsten oxide working temperature higher (being generally 200 ℃～300 ℃), this has seriously restricted the research and development of the integrated microminaturization air-sensitive of low-power consumption sensor-based system, and scientific and technical personnel are being devoted to reduce the research of sensitive material working temperature always for this reason.There are some researches show, one dimension tungsten oxide nanometer structure is compared with traditional tungsten oxide material, it has bigger specific surface area, bigger surfactivity and stronger gas absorption ability, thereby can accelerate and gas between reaction, when further improving sensitivity, working temperature is significant for reducing.
Silica-based porous silicon is a kind of at silicon chip surface formation aperture size, the duct degree of depth and the adjustable novel gas sensitive that has potentiality of porosity, have very high chemical mobility of the surface under the room temperature, and manufacture craft is because being easy to and compatible one of the most attractive research field that becomes of microelectronic process engineering.Its special micromechanism obtains huge specific surface area, and can provide effective passage for the gas diffusion, significantly reduces response/release time, has good air-sensitive performance.
In recent years, some scholar is devoted to the research of one-dimensional metal oxide gas sensitive, develops some gas sensors, because its working temperature higher (being higher than 150 ℃) has seriously restricted its application in the actual production life.The present invention adopts the method for chemical vapor deposition to utilize horizontal pipe furnace that ordered porous silicon and one dimension tungsten oxide nanometer structure are compounded to form new composite structure gas sensitive, it has huge specific surface area and big surfactivity, a large amount of gas absorption position and diffusion admittances is provided, overcome currently based on the higher defective of one dimension tungsten oxide nanometer structure gas sensitive working temperature, developed and a kind ofly have higher sensitivity and than the silica-based one dimension tungsten oxide nanometer structure gas sensor element of fast-response/regeneration rate at lower temperature (100 ℃).
Summary of the invention
Purpose of the present invention, it is the deficiency that overcomes existing one dimension tungsten oxide nanometer structure gas sensor working temperature higher (more than 150 ℃), the advantage of can room temperature surveying and effective passage can being provided for gas in conjunction with orderly porous silicon, the preparation method of a kind of novel structure, the simple novel porous silica-based one dimension tungsten oxide nanometer structure gas sensor of manufacture craft is provided, high sensitivity and good response recovery characteristics are organically combined, can have toxicity and dangerous gas such as NOx, a SO to low concentration at low temperature (100 ℃)
2, H
2S, especially NOx detects.
The present invention is achieved by following technical solution.
The preparation method of porous silicon-base one dimension tungsten oxide nano gas sensor has following steps:
(1) cleans the silicon chip substrate
Be the p-type monocrystalline silicon substrate single-sided polishing of 10～15 Ω cm with resistivity, cleaned 10～15 minutes through the concentrated sulphuric acid and mixed solution of hydrogen peroxide immersion 30-40 minute, hydrofluoric acid aqueous solution immersion 15-20 minute, acetone solvent ultrasonic cleaning 10-15 minute, absolute ethyl alcohol ultrasonic cleaning 10-15 minute, deionized water for ultrasonic respectively, to remove surface and oil contaminant, organic impurities and surface oxide layer;
(2) the ordered porous silicon in preparation silica-based micron-scale duct
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 mass concentration are that 40% dimethyl formamide is formed by mass concentration, its volume ratio is 1:2, do not add surfactant and additional optical photograph, the corrosion electric current density that applies is 50～120mA/cm
2, etching time is 5～20min;
(3) preparation porous silicon-base one dimension tungsten oxide nano
The silica-based porous silicon of step (2) preparation is placed horizontal pipe furnace, utilize the method for chemical vapor deposition, tungsten powder is as the tungsten source, and as working gas, oxygen is as reacting gas with argon gas, gas flow is controlled to be 5～10sccm and 0.5～5sccm respectively, source temperature is 900～1100 degree, and temperature retention time is 60～100min, and body vacuum tightness is 1～5Pa, operating pressure is 50～80Pa, and the distance between substrate and the tungsten source is 15～20 centimetres;
(4) preparation porous silicon-base tungsten oxide nano gas sensor element:
The porous silicon-base one dimension tungsten oxide nano that makes in the step (3) is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment; Adopt metal platinum as target, as working gas, gas flow is 23～25sccm with argon gas, the sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～12min, substrate temperature is room temperature, at tungsten oxide nano surface deposition platinum point electrode, makes the gas sensor element.
The silicon chip substrate of described step (1) is of a size of 2.4cm * 0.9cm.
Ordered porous silicon average pore size 1～2 μ m in silica-based micron-scale duct of described step (2) preparation, thickness is 8～15 μ m.
Described step (3) tungsten powder quality purity is 99.99%, and the one dimension tungsten oxide nanometer linear diameter of preparation is 40-100nm, and length is 20-40 μ m.
The horizontal pipe furnace of the employing of described step (3) is the GSL-1400X tubular furnace.
The preparation condition of described step (4) is: the metal platinum target of employing is quality purity 99.95%, with quality purity be 99.999% argon gas as working gas, base vacuum degree 4～6 * 10
-4Pa, the platinum film thickness 80～120nm 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 (4) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
The preparation method of porous silicon-base one dimension tungsten oxide nanometer line structure gas sensor element of the present invention, initiative has adopted the aperture at 1-2 μ m, the compound one dimension tungsten oxide nanometer of the silica-based porous silicon structure that has duct high-sequential arrangement concurrently is gas sensitive, because huge specific surface area and surfactivity can provide a large amount of gas absorption position, gas diffusion paths, make it comparatively be easy to react with gas.Gas sensor element of the present invention can have higher response and well sensitivity, selectivity to low-concentration nitrogen oxide gas down at low temperature (100 ℃), response/release time is short, and volume is small and exquisite, simple in structure, manufacture craft is ripe, easy to use, cheap, be expected to put it in the gas sensor field and use.
Description of drawings
Fig. 1 is the electron scanning micrograph of the ordered porous silicon face in embodiment 1 silica-based micron-scale duct;
Fig. 2 is the electron scanning micrograph of the ordered porous silicon section in embodiment 1 silica-based micron-scale duct;
Fig. 3 is embodiment 1 porous silicon-base one dimension tungsten oxide nano electron scanning micrograph;
Fig. 4 be embodiment 1 porous silicon-base one dimension tungsten oxide nano gas sensor under the different operating temperature to 1.5ppm NO
2Sensitivity;
Fig. 5 be embodiment 1 porous silicon-base one dimension tungsten oxide nano gas sensor under 100 ℃ to 1.5～0.5ppm NO
2The dynamic continuous response curve of gas;
Fig. 6 is embodiment 1 porous silicon-base one dimension tungsten oxide nano gas sensor selectivity diagram to gas with various under 100 ℃;
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.
1) clean the silicon chip substrate:
Be 10 Ω cm with resistivity, thickness is 400 μ m, (100) monocrystalline silicon piece of 2 of the crystal orientation cun p-type single-sided polishings, cut into the rectangle silicon base that is of a size of 2.4cm * 0.9cm, cleaned 10 minutes 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 successively;
2) the ordered porous silicon in preparation silica-based micron-scale duct:
Utilize the double flute electrochemical process to prepare porous silicon layer at the polished surface of silicon chip.Used corrosion electrolytic solution is that 40% hydrofluorite and mass concentration are that 40% dimethyl formamide is formed by mass concentration, and volume ratio is 1:2, does not add surfactant and additional optical photograph, and the corrosion electric current density that applies is 60mA/cm
2, etching time is 10min; Wherein porous silicon forms the regional 1.6cm * 0.4cm that is.The ordered porous silicon face pattern in silica-based micron-scale duct of preparation and scanning electron microscope analysis result such as Fig. 1 of cross-section structure, shown in 2, and to record average pore size be 1.5 μ m, thickness is 10 μ m;
3) preparation porous silicon-base one dimension tungsten oxide nano:
The 5g tungsten powder is contained in the aluminium oxide porcelain boat, be placed on center, horizontal pipe furnace flat-temperature zone; The porous silicon that step (2) is made is placed on tubular furnace gas outlet direction apart from aluminium oxide porcelain boat 16cm place; Feed and be evacuated to the interior vacuum of stove at 5Pa after argon gas cleans boiler tube 20min, feed quality purity and be 99.999% argon gas and quality purity and be the mixed gas of 99.999% oxygen, gas flow is respectively 5sccm and 0.5sccm, and the adjustments of gas valve makes the interior pressure of stove remain on 57Pa; Speed with 30 ℃/min is heated to 1100 ℃ of temperature of reaction, behind the constant temperature 90min, drops to room temperature at mixed-gas atmosphere, makes porous silicon-base one dimension tungsten oxide nano.Its result as shown in Figure 3, one dimension tungsten oxide nanometer linear diameter is 40-60nm, length is 20-30 μ m.
4) preparation porous silicon-base one dimension tungsten oxide nano gas sensor element:
The porous silicon-base one dimension tungsten oxide nano that makes in the step (3) is placed 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, with quality purity be 99.999% argon gas as working gas, the argon gas flow is 24sccm, the sputter operating pressure is 2.0Pa, sputtering power 90W, sputtering time 8min, substrate temperature are room temperature, at a pair of square platinum electrode that is of a size of 0.2cm * 0.2cm of tungsten oxide nano surface sputtering, electrode separation is 0.8cm, makes the gas sensor element.
The porous silicon-base one dimension tungsten oxide nano gas sensor element of embodiment 1 preparation under the different operating temperature to 1.5ppm NO
2The sensitivity of gas as shown in Figure 4, sensitivity under room temperature (25 ℃), 50 ℃, 75 ℃, 100 ℃, 125 ℃, 150 ℃, 200 ℃, 250 ℃ is respectively 1.51,1.82,2.24,2.75,2.43,2.09,1.63 and 1.12, between 25 ℃ to 100 ℃, sensitivity raises with the rising of temperature; After surpassing 100 ℃, sensitivity descends along with the rising of temperature, and this shows that its optimum working temperature is 100 ℃, and its maximum sensitivity is 2.75.Simultaneously, this gas sensor is to low concentration of NO
2Gas has the response of tangible gas, under 100 ℃ to variable concentrations NO
2The dynamic response curve of gas as shown in Figure 5, to 1.5,1.25,1,0.75,0.5ppm NO
2Sensitivity be respectively 2.75,2.43,2.16,1.93,1.58, sensitivity is with NO
2The rising of concentration and increasing gradually; In addition, this gas sensor average response and be respectively 200s and 100s release time shows better gas response/recovery characteristics.
The porous silicon-base one dimension tungsten oxide nano gas sensor element of embodiment 1 preparation under 100 ℃ to 2ppm NO
2, 50ppm NH
3, 100ppm ethanol, 100ppm acetone steam sensitivity be respectively 3.35,1.12,1.03,1.05; Show this sensor element in the time of 100 ℃ to NO
2Gas has selectivity preferably, and the result as shown in Figure 6.
The difference of present embodiment and embodiment 1 is: preparation one dimension tungsten oxide nanometer line structure makes behind 1100 ℃ of constant temperature 60min in the step (3), prepared porous silicon-base one dimension tungsten oxide nano gas sensor 100 ℃ of conditions to 2ppmNO
2The sensitivity of gas is 3.05.
The difference of present embodiment and embodiment 1 is: preparation one dimension tungsten oxide nano makes behind 1150 ℃ of constant temperature 90min in the step (3), prepared porous silicon-base one dimension tungsten oxide nano gas sensor 100 ℃ of conditions to 2ppmNO
2The sensitivity of gas is 2.51.
Embodiment 4
The difference of present embodiment and embodiment 1 is: preparation one dimension tungsten oxide nanometer line structure makes behind 1150 ℃ of constant temperature 60min in the step (3), prepared porous silicon-base one dimension tungsten oxide nano gas sensor 100 ℃ of conditions to 2ppmNO
2The sensitivity of gas is 1.81.
Embodiment 5
The difference of present embodiment and embodiment 1 is: preparation one dimension tungsten oxide nanometer line structure makes behind 1050 ℃ of constant temperature 90min in the step (3), prepared porous silicon-base one dimension tungsten oxide nano gas sensor 100 ℃ of conditions to 2ppmNO
2The sensitivity of gas is 2.14.
Embodiment 6
The difference of present embodiment and embodiment 1 is: preparation one dimension tungsten oxide nanometer line structure makes behind 1050 ℃ of constant temperature 60min in the step (3), prepared porous silicon-base one dimension tungsten oxide nano gas sensor 100 ℃ of conditions to 2ppmNO
2The sensitivity of gas is 1.87.
Claims (7)
1. the preparation method of a porous silicon-base one dimension tungsten oxide nano gas sensor has following steps:
(1) cleans the silicon chip substrate
Be the p-type monocrystalline silicon substrate single-sided polishing of 10～15 Ω cm with resistivity, cleaned 10～15 minutes through the concentrated sulphuric acid and mixed solution of hydrogen peroxide immersion 30-40 minute, hydrofluoric acid aqueous solution immersion 15-20 minute, acetone solvent ultrasonic cleaning 10-15 minute, absolute ethyl alcohol ultrasonic cleaning 10-15 minute, deionized water for ultrasonic respectively, to remove surface and oil contaminant, organic impurities and surface oxide layer;
(2) the ordered porous silicon in preparation silica-based micron-scale duct
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 mass concentration are that 40% dimethyl formamide is formed by mass concentration, its volume ratio is 1:2, do not add surfactant and additional optical photograph, the corrosion electric current density that applies is 50～120mA/cm
2, etching time is 5～20min;
(3) preparation porous silicon-base one dimension tungsten oxide nano
The silica-based porous silicon of step (2) preparation is placed horizontal pipe furnace, utilize the method for chemical vapor deposition, tungsten powder is as the tungsten source, and as working gas, oxygen is as reacting gas with argon gas, gas flow is controlled to be 5～10sccm and 0.5～5sccm respectively, source temperature is 900～1100 degree, and temperature retention time is 60～100min, and body vacuum tightness is 1～5Pa, operating pressure is 50～80Pa, and the distance between substrate and the tungsten source is 15～20 centimetres;
(4) preparation porous silicon-base tungsten oxide nano gas sensor element:
The porous silicon-base one dimension tungsten oxide nano that makes in the step (3) is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment; Adopt metal platinum as target, as working gas, gas flow is 23～25sccm with argon gas, the sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～12min, substrate temperature is room temperature, at tungsten oxide nano surface deposition platinum point electrode, makes the gas sensor element.
2. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that the silicon chip substrate of described step (1) is of a size of 2.4cm * 0.9cm.
3. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that, ordered porous silicon average pore size 1～2 μ m in silica-based micron-scale duct of described step (2) preparation, thickness is 8～15 μ m.
4. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that described step (3) tungsten powder quality purity is 99.99%, the one dimension tungsten oxide nanometer linear diameter of preparation is 40-100nm, and length is 20-40 μ m.
5. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that the horizontal pipe furnace of the employing of described step (3) is the GSL-1400X tubular furnace.
6. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that, the preparation condition of described step (4) is: the metal platinum target of employing is quality purity 99.95%, with quality purity be 99.999% argon gas as working gas, base vacuum degree 4～6 * 10
-4Pa, the platinum film thickness 80～120nm that adopts radio-frequency magnetron sputter method to prepare.
7. according to the preparation method of the porous silicon-base one dimension tungsten oxide nano gas sensor of claim, it is characterized in that the vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (4) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
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| CN103512924A (en) * | 2013-10-21 | 2014-01-15 | 天津大学 | Preparation method of gas sensitive element for detecting nitric oxide at low temperature |
| 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 |
| CN103626117A (en) * | 2013-10-21 | 2014-03-12 | 天津大学 | Method for preparing tungsten oxide nanowire/porous silicon composite structure material at low temperature |
| CN103630572A (en) * | 2013-10-21 | 2014-03-12 | 天津大学 | Preparation method of porous silicon/tungsten oxide nanowire composite structure for gas-sensitive material |
| CN103641061A (en) * | 2013-12-03 | 2014-03-19 | 电子科技大学 | Micro-nano gas sensor with gas-sensitive reconstruction effect and preparation method of micro-nano gas sensor |
| CN104634824A (en) * | 2015-01-28 | 2015-05-20 | 天津大学 | Preparation method of gas-sensitive sensor with porous-silicon-based tungsten-oxide nano-rod composite structure |
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| CN108459060A (en) * | 2017-02-20 | 2018-08-28 | 天津大学 | One-dimensional silicon substrate gas sensitive of polypyrrole surface modification and preparation method thereof |
| CN109298026A (en) * | 2017-07-24 | 2019-02-01 | 天津大学 | Silicon nanowires-tungsten oxide nano brush multilevel structure and preparation method thereof and the application in detection nitrogen dioxide |
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| CN104634824A (en) * | 2015-01-28 | 2015-05-20 | 天津大学 | Preparation method of gas-sensitive sensor with porous-silicon-based tungsten-oxide nano-rod composite structure |
| CN105529191A (en) * | 2016-01-13 | 2016-04-27 | 张志华 | High-conversion-efficiency solar cell based vehicle license plate recognition device of parking lot |
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| CN109298026A (en) * | 2017-07-24 | 2019-02-01 | 天津大学 | Silicon nanowires-tungsten oxide nano brush multilevel structure and preparation method thereof and the application in detection nitrogen dioxide |
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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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Application publication date: 20130814 |