CN103063706A - Preparation method for porous silicon based tungsten oxide nanocomposite structure gas sensor - Google Patents
Preparation method for porous silicon based tungsten oxide nanocomposite structure gas sensor Download PDFInfo
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- CN103063706A CN103063706A CN2012105762479A CN201210576247A CN103063706A CN 103063706 A CN103063706 A CN 103063706A CN 2012105762479 A CN2012105762479 A CN 2012105762479A CN 201210576247 A CN201210576247 A CN 201210576247A CN 103063706 A CN103063706 A CN 103063706A
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Abstract
The invention discloses a preparation method for a porous silicon based tungsten oxide nanocomposite gas sensor. The method comprises the steps of preparing a porous silicon layer on a polished surface of a single crystal silicon substrate by using n-type single side polished single crystal silicon substrate as a substrate for the silicon substrate, wherein a corrosion electrolyte is composed of 40% hydrofluoric acid and deionized water; sputtering depositing a tungsten oxide nanometer film on the surface of the silicon-based porous silicon surface by using high pure metal tungsten as a target, argon gas as a working gas and oxygen gas as a reaction gas; heat-treating the film for 3-4 hours at a temperature of 450 DEG C-500 DEG C under an air atmosphere; depositing a platinum electrode on the surface of the tungsten oxide film by using metal platinum as a target and the argon gas as a working gas to prepare the composite structure gas sensor at a room temperature. The preparation method has the advantages of high sensitivity, high selectivity, fast response/recovery characteristics and good repeatability, and can maintain long-term stability.
Description
Technical field
The invention relates to a kind of gas sensor, relate in particular to a kind of working and room temperature and be applicable to detect the preparation method of the nano-scale duct ordered porous silica-based tungsten oxide film nano composite structure gas sensor of oxides of nitrogen gas.
Background technology
Since 20th century, along with the develop rapidly of industrial technology, the various gas pollutants that bring in the production run roll up.Especially oxides of nitrogen (NO
x) as a kind of strong poisonous gas, be the main source of acid rain and photo-chemical smog, the mankind's health and safety constituted a serious threat.Therefore the detection of oxides of nitrogen gas is become in recent years study hotspot.Up to now, in studied metal oxide semiconductor gas sensitive, tungsten oxide is to NO
xGas has very high sensitivity and selectivity, is the sensitive material that a kind of utmost point has research and application prospect.Yet the tungsten oxide material working temperature is higher, is generally 150 ° of C ~ 250 ° C.The long-time microstructure that can make tungsten oxide film of at high temperature working is tending towards fine and close gradually, causes gas to spread in sensitive material and becomes very difficult, causes the bad stability of sensor.Scientific and technical personnel are being devoted to reduce the research of the working temperature of sensitive material always for this reason.
According to studies show that in the past, mixing or forming compound gas sensitive is a kind of effective way that reduces the tungsten oxide material working temperature, and can further improve NO
xSensitivity and selectivity.Yet realize at present room temperature detection low concentration of NO
xOr one is rich in challenging problem.
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 of easy and compatible one of the most attractive research field that becomes of microelectronic process engineering.Especially for aperture size at 150 ~ 200nm, have the porous silicon of the uniform sequential arrangement of high porosity and duct concurrently, its unique micromechanism obtains huge specific surface area, and can provide effective passage for the gas diffusion, significantly reduce response/release time, at room temperature have good air-sensitive performance.
In recent years, some scholar develops the porous silicon-base tungsten oxide film gas sensor that can at room temperature work.But because the porous silicon duct presents the too fine and close smooth effective gas diffusion paths that lacks in tungsten oxide film surface of disorder distribution or sputter, have a strong impact on response/release time, restricted its further practical application.The present invention adopts the double flute electrochemical erosion method to prepare the ordered porous silicon layer in silicon-based nano size duct, utilizes the standby surface porosity porous of facing-target magnetron sputtering system legal system and contains the tungsten oxide nanometer thin film (WO in a large amount of oxygen room
3-x, x represents oxygen vacancy concentration).Loose porous surface and a large amount of oxygen room be because having huge specific activity surface area and high density surface attitude, and a large amount of gas absorption positions and direct diffusion admittance are provided, and then develops a kind of room temperature that can realize and survey NO
xGas and have high sensitivity and the quick nano composite structure gas sensor element of response/regeneration rate.
Summary of the invention
Purpose of the present invention, to overcome the higher shortcoming of conventional oxidation tungsten gas sensor working temperature, improvement is because of the disorder distribution of porous silicon duct structure and the too fine and close smooth adverse effect to traditional porous silicon-base tungsten oxide material air-sensitive performance in tungsten oxide film surface of sputter, the preparation method of a kind of novel structure, the ordered porous silica-based tungsten oxide film nano composite structure gas sensor in the simple novel nano size of preparation technology duct is provided, high sensitivity and good response/recovery characteristics are combined, can be at room temperature to the NO of super low concentration
xGas is realized well surveying, and has good long-time stability.
The present invention is achieved by following technical solution.
Be used for the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor of room temperature, have following steps:
(1) cleans the silicon chip substrate
Be the monocrystalline silicon substrate of the N-shaped single-sided polishing of 0.01 ~ 0.015 Ω cm with resistivity, put into successively the respectively ultrasonic cleaning 10 ~ 20 minutes of acetone solvent, absolute ethyl alcohol, deionized water, remove 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; Clean with deionized water rinsing again;
(2) the ordered porous silicon in preparation silicon-based nano size duct
The monocrystalline silicon substrate polished surface that adopts the double flute electrochemical erosion method to clean in step (1) prepares porous silicon layer, used corrosion electrolytic solution is that 40% hydrofluorite and deionized water form by mass percent, volume ratio is 1:5, do not add surfactant and additional optical photograph, the corrosion electric current density that applies is 115 ~ 135mA/cm
2, etching time is 20 ~ 25min;
(3) preparation porous silicon-base tungsten oxide nanometer composite structure
The silica-based porous silicon of step (2) preparation is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the tungsten of quality purity 99.95% as target, the sputter operating pressure is 1.0 ~ 2.0Pa, take the argon gas of quality purity as 99.999% as working gas, oxygen is as reacting gas, and gas flow is controlled to be respectively 44.5 ~ 45.5sccm and 4.5 ~ 5.5sccm, sputtering power 90 ~ 100W, sputtering time is 5 ~ 15min, and body vacuum tightness is 2 ~ 4 * 10
-4Pa, substrate temperature are room temperature, 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, thermal treatment 3 ~ 4h in ° C air atmosphere of 450 ° of C ~ 500, the control heating rate is 2.5 ° of C/min;
(4) preparation porous silicon-base tungsten oxide nanometer composite structure gas sensor element
The porous silicon-base tungsten oxide nanometer composite structure that step (3) is made places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.95% as target, take the argon gas of quality purity as 99.999% as working gas, the argon gas flow is 20 ~ 25sccm, the sputter operating pressure is 2.0Pa, sputtering power 80 ~ 90W, sputtering time 8 ~ 12min, body vacuum tightness is 4 ~ 6 * 10
-4Pa, substrate temperature are room temperature, at tungsten oxide film surface deposition platinum electrode, make the porous silicon-base tungsten oxide nanometer composite structure gas sensor for room temperature.
The cut lengths of the monocrystalline silicon substrate substrate of described step (1) are 2.2 ~ 2.4cm * 0.8 ~ 0.9cm.
The silicon-based nano size duct ordered porous silicon average pore size 150 ~ 170nm of described step (2) preparation, thickness is 65 ~ 70 μ m.
It is 25 ~ 70nm that described step (3) adopts the tungsten oxide film thickness of dc reactive magnetron sputtering technique preparation.
Described step (4) adopts the Platinum Electrode Thickness 80 ~ 120nm of radio-frequency magnetron sputter method preparation.
The vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (3) and (4) is DPS-III type ultrahigh vacuum pair
The vacuum chamber of target magnetic control sputtering equipment.
Beneficial effect of the present invention is: a kind of working and room temperature is provided and the super low concentration oxides of nitrogen gas is had high sensitivity, high selectivity, the quick preparation method of response/recovery characteristics, good reproducibility and porous silicon-base tungsten oxide nanometer composite structure gas sensor that can maintaining a long-term stability property.
Description of drawings
Fig. 1 is the electron scanning micrograph of the ordered porous silicon in embodiment 1 silicon-based nano size duct;
Fig. 2 is embodiment 1 porous silicon-base tungsten oxide nanometer composite structure electron scanning micrograph;
Fig. 3 is the sensitivity to gas under the different operating temperature of embodiment 1 porous silicon-base tungsten oxide nanometer composite structure gas sensor;
Fig. 4 is that embodiment 1 porous silicon-base tungsten oxide nanometer composite structure gas sensor is at room temperature to 30 ~ 1000ppb NO
2The dynamic continuous response curve of gas;
Fig. 5 is that embodiment 1 porous silicon-base tungsten oxide nanometer composite structure gas sensor is at room temperature to 500ppb NO
2The repeated curve of gas;
Fig. 6 is that embodiment 1 porous silicon-base tungsten oxide nanometer composite structure gas sensor is at room temperature to the selectivity synoptic diagram of gas with various;
Fig. 7 is that embodiment 1 porous silicon-base tungsten oxide nanometer composite structure gas sensor is placed in air behind the different time at room temperature to 1ppmNO
2Sensitivity.
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 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 with deionized water again;
2) the ordered porous silicon in preparation silicon-based nano size 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 deionized water form by massfraction, and volume ratio is 1:5, does not add surfactant and illumination, 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.The embodiment 1 prepared ordered porous silicon average pore size in silicon-based nano size duct is 170.28nm, thickness is 68.78 μ m, surface topography is the cellular structure that polygonal hole forms, Cross Section Morphology is that straight columniform duct high-sequential is arranged, and the scanning electron microscope analysis result of its surface topography and cross-section structure as shown in Figure 1;
3) preparation porous silicon-base tungsten oxide nanometer composite structure:
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, the sputter operating pressure is 1.0Pa, and sputtering power 90 ~ 100W, sputtering time are 9min, at silica-based porous silicon surface sputtering sedimentation tungsten oxide nanometer thin film, substrate temperature is room temperature.Subsequently the porous silicon-base tungsten oxide film that makes is placed the program sintering furnace, in 450 ° of C air atmosphere thermal treatment 4h, the control heating rate is 2.5 ° of C/min.The prepared tungsten oxide film of embodiment 1 is coarse and discontinuous, there is a large amount of channel-like structures, surface structure is extremely loose, specific surface area is very high and provide a large amount of passages for gas diffusion, and having formed the heterojunction nano composite structure with porous silicon layer, the scanning electron microscope analysis result of its surface topography is as shown in Figure 2;
4) preparation porous silicon-base tungsten oxide nanometer composite structure gas sensor element:
The porous silicon-base tungsten oxide nanometer composite structure that makes in the step (3) is placed the vacuum chamber of DPS-III ultrahigh vacuum facing-target magnetron sputtering system equipment.Body vacuum tightness 4.5 * 10
-4Pa, adopt the metal platinum of quality purity 99.95% as target, as working gas, the argon gas flow is 24sccm take the argon gas of quality purity as 99.999%, and 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 film surface sputtering, thickness of electrode is 80nm, and electrode separation is 0.8cm.
The porous silicon-base tungsten oxide nanometer composite structure gas sensor that embodiment 1 makes under the different operating temperature to 1ppm NO
2The sensitivity of gas as shown in Figure 3, the sensitivity under 25 ° of C of room temperature, 50 ° of C, 75 ° of C, 100 ° of C is respectively 6.478,3.86,2.762 and 1.467, sensitivity significantly descends with the rising of temperature, this shows that its optimum working temperature is room temperature.This gas sensor is to super low concentration NO
2Gas has obvious gas response, at room temperature to variable concentrations NO
2The dynamic response curve of gas as shown in Figure 4, to 30,60,125,250,500,750,1000ppb NO
2Sensitivity be respectively 2.406,2.910,3.784,4.892,5.994,6.597,6.992, sensitivity is with NO
2The rising of concentration and increasing gradually; This gas sensor repeatedly is exposed to 500ppb NO
2, average response and release time are respectively 76s and 144s, show good repeatability and gas response/recovery characteristics faster, and four times loop test the results are shown in Fig. 5.
By embodiment 1 prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor element at room temperature to 1ppmNO
2, 20ppm NH
3, SO
2, H
2S, the sensitivity of 100ppm ethanol, acetone, methyl alcohol, IPA vapor is respectively 6.478,1.183,1.053,2.133,1.024,1.052,1.062,1.087.The gas sensor that shows this invention when room temperature to NO
2Gas has certain selectivity, and the result as shown in Figure 6.
By embodiment 1 prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor element within 35 days standing time to NO
2Can keep certain sensitive property, under atmospheric environment, place a week, two weeks, three weeks, all around and after five weeks to 1ppmNO
2Sensitivity be respectively 6.898,5.449,4.871,4.278,3.066, show that the gas sensor of this invention has good long-time stability, the result as shown in Figure 7.
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 5min in the step (3), prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor at room temperature condition to 1ppm NO
2The sensitivity of gas is 1.09.
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 8min in the step (3), prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor at room temperature condition to 1ppm NO
2The sensitivity of gas is 2.803.
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 10min in the step (3), prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor at room temperature condition to 1ppm NO
2The sensitivity of gas is 5.167.
The difference of present embodiment and embodiment 1 is: the tungsten oxide nanometer thin film sputtering time is 13min in the step (3), prepared porous silicon-base tungsten oxide nanometer composite structure gas sensor at room temperature condition to 1ppm NO
2The sensitivity of gas is 2.091.
Obviously, those skilled in the art can carry out various changes and modification to porous silicon-base tungsten oxide nanometer composite structure gas sensor of working and room temperature of the present invention and preparation method thereof and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (6)
1. preparation method who is used for the porous silicon-base tungsten oxide nanometer composite structure gas sensor of room temperature has following steps:
(1) cleans the silicon chip substrate
Be the monocrystalline silicon substrate of the N-shaped single-sided polishing of 0.01 ~ 0.015 Ω cm with resistivity, put into successively the respectively ultrasonic cleaning 10 ~ 20 minutes of acetone solvent, absolute ethyl alcohol, deionized water, remove 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; Clean with deionized water rinsing again;
(2) the ordered porous silicon in preparation silicon-based nano size duct
The monocrystalline silicon substrate polished surface that adopts the double flute electrochemical erosion method to clean in step (1) prepares porous silicon layer, used corrosion electrolytic solution is that 40% hydrofluorite and deionized water form by mass percent, volume ratio is 1:5, do not add surfactant and additional optical photograph, the corrosion electric current density that applies is 115 ~ 135mA/cm
2, etching time is 20 ~ 25min;
(3) preparation porous silicon-base tungsten oxide nanometer composite structure
The silica-based porous silicon of step (2) preparation is placed the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the tungsten of quality purity 99.95% as target, the sputter operating pressure is 1.0 ~ 2.0Pa, take the argon gas of quality purity as 99.999% as working gas, oxygen is as reacting gas, and gas flow is controlled to be respectively 44.5 ~ 45.5sccm and 4.5 ~ 5.5sccm, sputtering power 90 ~ 100W, sputtering time is 5 ~ 15min, and body vacuum tightness is 2 ~ 4 * 10
-4Pa, substrate temperature are room temperature, 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, thermal treatment 3 ~ 4h in ° C air atmosphere of 450 ° of C ~ 500, the control heating rate is 2.5 ° of C/min;
(4) preparation porous silicon-base tungsten oxide nanometer composite structure gas sensor element
The porous silicon-base tungsten oxide nanometer composite structure that step (3) is made places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.95% as target, take the argon gas of quality purity as 99.999% as working gas, the argon gas flow is 20 ~ 25sccm, the sputter operating pressure is 2.0Pa, sputtering power 80 ~ 90W, sputtering time 8 ~ 12min, body vacuum tightness is 4 ~ 6 * 10
-4Pa, substrate temperature are room temperature, at tungsten oxide film surface deposition platinum electrode, make the porous silicon-base tungsten oxide nanometer composite structure gas sensor for room temperature.
2. according to claim 1 the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor that is used for room temperature is characterized in that the cut lengths of the monocrystalline silicon substrate substrate of described step (1) are 2.2 ~ 2.4cm * 0.8 ~ 0.9cm.
3. according to claim 1 the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor that is used for room temperature, it is characterized in that, the silicon-based nano size duct ordered porous silicon average pore size 150 ~ 170nm of described step (2) preparation, thickness is 65 ~ 70 μ m.
4. according to claim 1 the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor that is used for room temperature is characterized in that it is 25 ~ 70nm that described step (3) adopts the tungsten oxide film thickness of dc reactive magnetron sputtering technique preparation.
5. according to claim 1 the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor that is used for room temperature is characterized in that described step (4) adopts the Platinum Electrode Thickness 80 ~ 120nm of radio-frequency magnetron sputter method preparation.
6. according to claim 1 the preparation method of the porous silicon-base tungsten oxide nanometer composite structure gas sensor that is used for room temperature, it is characterized in that the vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (3) and (4) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
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