CN101799443A - Method for preparing multiaperture silicon substrate tungsten oxide nanometer thin film gas sensitive transducer - Google Patents
Method for preparing multiaperture silicon substrate tungsten oxide nanometer thin film gas sensitive transducer Download PDFInfo
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- CN101799443A CN101799443A CN201010125134A CN201010125134A CN101799443A CN 101799443 A CN101799443 A CN 101799443A CN 201010125134 A CN201010125134 A CN 201010125134A CN 201010125134 A CN201010125134 A CN 201010125134A CN 101799443 A CN101799443 A CN 101799443A
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Abstract
The invention discloses a method for preparing a multiaperture silicon substrate WO3 nanometer thin film gas sensitive transducer. The step comprises that: (1) a multiaperture silicon layer substrate is prepared, (2) a multiaperture silicon substrate WO3 nanometer thin film is prepared, (3) the prepared multiaperture silicon substrate WO3 nanometer thin film is placed in a 400 to 600 degrees centigrade high temperature heating furnace, (4) the prepared WO3 nanometer thin film is placed in the vacuum chamber of a UHV target magnetic control sputtering device to plate an electrode and the multiaperture silicon substrate WO3 nanometer thin film gas sensitive transducer is obtained. The invention provides the method for preparing the multiaperture silicon substrate tungsten oxide nanometer thin film gas sensitive transducer which has easy control, simple technology, low work temperature (room temperature) and high sensitivity.
Description
Technical field
The invention relates to preparation tungsten oxide (WO
3) nanometer thin film gas sensitive transducer, relating in particular to the porous silicon is substrate preparation WO
3The method of nanometer thin film gas sensitive transducer.
Background technology
WO
3Gas sensitive is because to NO
x, NH
3Short Deng gas sensitivity height, response time and release time, be easy to measure and be considered to one of tool application prospect and gas sensitive of development prospect with control, advantage such as cheap, become new concern of scientific and technical personnel and research focus.Yet WO
3This shortcoming of gas sensor working temperature height (about 250 ℃) is that the integrated microminaturization of sensor-based system has increased complicacy and instability, becomes the obstacle that the preparation low-power dissipation system must be gone beyond.Scientific and technical personnel are being devoted to reduce the research of its working temperature always for this reason, and simultaneously (porous silicon PS) also causes scientific research personnel's concern to novel room temperature gas sensitive porous silicon.Porous silicon is a kind of material of the poriness open structure with bigger serface that is formed by etching at silicon chip surface, has very high chemical activity, and its electric property has sensitivity characteristic to ammonia, is a kind of very potential novel room temperature gas sensitive.But there are shortcomings such as sensitivity is lower slightly, reaction velocity is slow, release time is long in the porous silicon gas sensor.
Enhancing along with environmental consciousness, people have higher requirement to gas sensor, and some experts and scholars proposes that the two combines the gas sensor of the low working temperature of research and development, high sensitivity, fast-response with metal oxide semiconductor material and porous silicon gas sensitive in recent years.The founder V.M.Arakelyan of this method, V.E.Galstyan etc. have delivered in " Physica E " 38 phases in 2007 and have been entitled as " Hydrogen sensitive gas sensor based on porous silicon/TiO
2-xStructure " paper, adopt electron-beam vapor deposition method with TiO in the literary composition
2-xBe deposited on the porous silicon layer surface and form PS/TiO
2-xStructure has been studied it to H
2Sensitivity characteristic, find that this method has improved the porous silicon gas sensor at room temperature to H
2Sensitivity, but the improvement degree is little.Based on above analysis, basic to the existing research of understanding and applicant place seminar of key issue in the novel sensor research and development of being touched upon to domestic and international present Research, the present invention adopts the double flute electrochemical erosion method to prepare porous silicon layer, utilizes the facing-target magnetron sputtering system legal system to be equipped with WO
3Nano thin-film, proposing with the porous silicon is the tungsten oxide (WO of substrate
3) research of nanometer thin film gas sensitive transducer, develop a kind of novel room temperature gas sensor with higher sensitivity.
Summary of the invention
The objective of the invention is to overcome existing WO
3Gas sensor working temperature height (about 200 ℃), there is the low shortcoming of sensitivity in the porous silicon gas sensor, provides that a kind of preparation is easy to control, technology is simple, working temperature is low (room temperature), WO at the bottom of the highly sensitive porous silicon-base
3The method of nanometer thin film gas sensitive transducer.
WO at the bottom of the preparation porous silicon-base of the present invention
3The method of nanometer thin film gas sensitive transducer has following steps:
(1) preparation porous silicon layer substrate:
Adopt the p of double flute electrochemical erosion method at single-sided polishing
+Monocrystalline silicon sheet surface prepares porous silicon layer, used corrosive liquid is the mixed liquor of 1: 1 hydrofluorite of volume ratio (40%) and absolute ethyl alcohol, apply the size of corrosion electric current density and porosity, the thickness that etching time changes porous silicon layer by control, the corrosion electric current density that applies is 20～80mA/cm
2, etching time is 5～30min;
(2) preparation WO
3Nano thin-film:
The porous silicon layer substrate that step (1) is made places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree (2～4) * 10
-4Pa, operating air pressure 1.0～2.0Pa, working gas (argon gas, purity 99.9%) is 9: 1～1: 9 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 60～100W, sputtering time 2～30min, substrate temperature are the chamber;
(3) annealing in process
WO at the bottom of the porous silicon-base that step (2) is made
3Nano thin-film places in the high-temperature heater, and the annealing in process environment is an atmospheric environment, and the annealing in process temperature is 400～600 ℃, and the annealing in process time is 2～4h, then with the stove natural cooling;
(4) plated electrode
The WO that step (3) is made
3Nano thin-film places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, base vacuum degree (2.0～7.0) * 10
-4Pa, sputter operating air pressure 2Pa, sputtering time 8min, Ar gas flow 24ml/min is at WO
3The nano thin-film surface deposition forms two square Pt electrodes, makes WO at the bottom of the porous silicon-base
3Nanometer thin film gas sensitive transducer.
The porous silicon layer aperture size of described step (1) is about 10～20nm, and the degree of depth is 20～80 μ m, and porosity is 50～76.80%.
The vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (2), step (4) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
The minitype digital temperature controller is adopted in the annealing temperature control of described step (3).
The invention has the beneficial effects as follows, provide a kind of and be easy to control, technology simply prepares WO at the bottom of the porous silicon-base
3The method of nanometer thin film gas sensitive transducer, the gas sensor working temperature low (room temperature) of this method preparation, highly sensitive.
Description of drawings
Fig. 1 is that embodiment 1 is at room temperature to 50ppmNH
3The sensitivity characteristic curve map;
Fig. 2 is that embodiment 2 is at room temperature to 50ppmNH
3The sensitivity characteristic curve map.
Embodiment
The raw materials used commercially available chemical pure raw material that adopts routine of the present invention.
Embodiment 1
(1) preparation porous silicon-base bottom technique condition: with the p of single-sided polishing
+(100) monocrystalline silicon piece (380 ± 10 μ m, 0.009～0.12 Ω cm) cuts into the rectangle substrate that is of a size of 2.4cm * 0.9cm, adopts the double flute electrochemical erosion method at its surface preparation porous silicon layer.Used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, the corrosion electric current density that applies is 80mA/cm
2, etching time is 30min.Wherein porous silicon layer area size is 1.6cm * 0.4cm, in order to being coated with WO
3Nano thin-film.
(2) place the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment at the bottom of the porous silicon-base that step (1) is made, adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree 4.0 * 10
-4Pa, operating air pressure 1.0Pa, working gas (argon gas, purity 99.9%) is 1: 1 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 80W, sputtering time 5min, substrate temperature is a room temperature, prepares WO
3Nano thin-film.
(3) WO that step (2) is made
3Nano thin-film places in the annealing furnace, and anneal environment is an atmospheric environment, and the capping of annealing furnace can be enclosed in print in the metastable annealing atmosphere preferably, but owing to be not complete airtight container, also inevitably is subjected to the influence of external environment.The minitype digital temperature controller is adopted in temperature control.Annealing temperature is set at 400 ℃, and the annealing heat treatment time is 4h.
(4) WO at the bottom of the porous silicon-base that step (3) is made
3Nano thin-film places the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, the base vacuum degree is 5.0 * 10
-4Pa, sputter operating air pressure are 2Pa, and sputtering time is 8min, and the Ar gas flow is 24ml/min, at WO
3The nanometer particle film surface deposition forms two square Pt electrodes.
WO at the bottom of the porous silicon-base that embodiment 1 makes
3Nano thin-film is at room temperature to 50ppmNH
3Sensitivity be 18.7, be 15/27min response/release time.
Embodiment 1 is at room temperature to 50ppmNH
3The sensitivity characteristic curve as shown in Figure 1.
Embodiment 2
(1) preparation porous silicon-base bottom technique condition: with the p of single-sided polishing
+(100) monocrystalline silicon piece (380 ± 10 μ m, 0.009～0.12 Ω cm) cuts into the rectangle substrate that is of a size of 2.4cm * 0.9cm, adopts the double flute electrochemical erosion method at its surface preparation porous silicon layer.Used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, the corrosion electric current density that applies is 80mA/cm
2, etching time is 30min.Wherein porous silicon layer area size is 1.6cm * 0.4cm, in order to being coated with WO
3Nano thin-film;
(2) place the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment at the bottom of the porous silicon-base that step (1) is made, adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree 2.0 * 10
-4Pa, operating air pressure 1.0Pa, working gas (argon gas, purity 99.9%) is 1: 1 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 80W, sputtering time 30min, substrate temperature is a room temperature, prepares WO
3Nano thin-film.
(3) WO that step (2) is made
3Nano thin-film places in the annealing furnace, and anneal environment is an atmospheric environment, and the capping of annealing furnace can be enclosed in print in the metastable annealing atmosphere preferably, but owing to be not complete airtight container, also inevitably is subjected to the influence of external environment.The minitype digital temperature controller is adopted in temperature control.Annealing temperature is set at 450 ℃, and the annealing heat treatment time is 4h.
(4) WO at the bottom of the porous silicon-base that step (3) is made
3Nano thin-film places the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, the base vacuum degree is 4.0 * 10
-4Pa, sputter operating air pressure are 2Pa, and sputtering time is 8min, and the Ar gas flow is 24ml/min, at WO
3The nanometer particle film surface deposition forms two square Pt electrodes.
WO at the bottom of the porous silicon-base that embodiment 2 makes
3Nano thin-film is at room temperature to 50ppmNH
3Sensitivity be 17.2, be 7/29min. response/release time
Embodiment 2 is at room temperature to 50ppmNH
3The sensitivity characteristic curve as shown in Figure 2.
Embodiment 3
(1) preparation porous silicon-base bottom technique condition: with the p of single-sided polishing
+(100) monocrystalline silicon piece (380 ± 10 μ m, 0.009～0.12 Ω cm) cuts into the rectangle substrate that is of a size of 2.4cm * 0.9cm, adopts the double flute electrochemical erosion method at its surface preparation porous silicon layer.Used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, the corrosion electric current density that applies is 80mA/cm
2, etching time is 20min.Wherein porous silicon layer area size is 1.6cm * 0.4cm, in order to being coated with WO
3Nano thin-film;
(2) place the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment at the bottom of the porous silicon-base that step (1) is made,
Adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree 3.0 * 10
-4Pa, operating air pressure 1.5Pa, working gas (argon gas, purity 99.9%) is 7: 3 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 100W, sputtering time 2min, substrate temperature is a room temperature, prepares WO
3Nano thin-film.
(3) WO that step (2) is made
3Nano thin-film places in the annealing furnace, and anneal environment is an atmospheric environment, and the capping of annealing furnace can be enclosed in print in the metastable annealing atmosphere preferably, but owing to be not complete airtight container, also inevitably is subjected to the influence of external environment.The minitype digital temperature controller is adopted in temperature control.Annealing temperature is set at 500 ℃, and the annealing heat treatment time is 2h.
(4) WO at the bottom of the porous silicon-base that step (3) is made
3Nano thin-film places the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, the base vacuum degree is 3.0 * 10
-4Pa, sputter operating air pressure are 2Pa, and sputtering time is 8min, and the Ar gas flow is 24ml/min, at WO
3The nanometer particle film surface deposition forms two square Pt electrodes.
WO at the bottom of the porous silicon-base that embodiment 3 makes
3Nano thin-film is at room temperature to 50ppmNH
3Sensitivity be 9.67.
Embodiment 4
(1) preparation porous silicon-base bottom technique condition: with the p of single-sided polishing
+(100) monocrystalline silicon piece (380 ± 10 μ m, 0.009～0.12 Ω cm) cuts into the rectangle substrate that is of a size of 2.4cm * 0.9cm, adopts the double flute electrochemical erosion method at its surface preparation porous silicon layer.Used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, the corrosion electric current density that applies is 40mA/cm
2, etching time is 10min.Wherein porous silicon layer area size is 1.6cm * 0.4cm, in order to being coated with WO
3Nano thin-film;
(2) place the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment at the bottom of the porous silicon-base that step (1) is made,
Adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree 4.0 * 10
-4Pa, operating air pressure 2.0Pa, working gas (argon gas, purity 99.9%) is 9: 1 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 60W, sputtering time 20min, substrate temperature is a room temperature, prepares WO
3Nano thin-film.
(3) WO that step (2) is made
3Nano thin-film places in the annealing furnace, and anneal environment is an atmospheric environment, and the capping of annealing furnace can be enclosed in print in the metastable annealing atmosphere preferably, but owing to be not complete airtight container, also inevitably is subjected to the influence of external environment.The minitype digital temperature controller is adopted in temperature control.Annealing temperature is set at 600 ℃, and the annealing heat treatment time is 3h.
(4) WO at the bottom of the porous silicon-base that step (3) is made
3Nano thin-film places the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, the base vacuum degree is 2.0 * 10
-4Pa, sputter operating air pressure are 2Pa, and sputtering time is 8min, and the Ar gas flow is 24ml/min, at WO
3The nanometer particle film surface deposition forms two square Pt electrodes.
WO at the bottom of the porous silicon-base that embodiment 4 makes
3Nano thin-film is at room temperature to 50ppmNH
3Sensitivity be 7.0.
Embodiment 5
(1) preparation porous silicon-base bottom technique condition: with the p of single-sided polishing
+(100) monocrystalline silicon piece (380 ± 10 μ m, 0.009～0.12 Ω cm) cuts into the rectangle substrate that is of a size of 2.4cm * 0.9cm, adopts the double flute electrochemical erosion method at its surface preparation porous silicon layer.Used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, the corrosion electric current density that applies is 20mA/cm
2, etching time is 5min.Wherein porous silicon layer area size is 1.6cm * 0.4cm, in order to being coated with WO
3Nano thin-film;
(2) place the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment at the bottom of the porous silicon-base that step (1) is made,
Adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree 2.0 * 10
-4Pa, operating air pressure 1.0Pa, working gas (argon gas, purity 99.9%) is 1: 9 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 90W, sputtering time 10min, substrate temperature is a room temperature, prepares WO
3Nano thin-film.
(3) WO that step (2) is made
3Nano thin-film places in the annealing furnace, and anneal environment is an atmospheric environment, and the capping of annealing furnace can be enclosed in print in the metastable annealing atmosphere preferably, but owing to be not complete airtight container, also inevitably is subjected to the influence of external environment.The minitype digital temperature controller is adopted in temperature control.Annealing temperature is set at 600 ℃, and the annealing heat treatment time is 4h.
(4) WO at the bottom of the porous silicon-base that step (3) is made
3Nano thin-film places the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, the base vacuum degree is 7.0 * 10
-4Pa, sputter operating air pressure are 2Pa, and sputtering time is 8min, and the Ar gas flow is 24ml/min, at WO
3The nanometer particle film surface deposition forms two square Pt electrodes.
WO at the bottom of the porous silicon-base that embodiment 5 makes
3Nano thin-film is at room temperature to 50ppmNH
3Sensitivity be 4.0.
The related process parameter of the embodiment of the invention sees following table for details.
The present invention adopts static distribution method at room temperature to measure WO at the bottom of the porous silicon-base
3Nanometer thin film gas sensitive transducer is to NH
3Deng the sensitivity characteristic of gas, the sensitivity S of definition gas sensor is S=(R
Gas-R
Air)/R
Air, R wherein
a, R
gBe respectively element in air and detected gas in resistance value.
According to WO at the bottom of the porous silicon-base of technical solution of the present invention preparation
3Nanometer thin film gas sensitive transducer compared with prior art, its sensitivity improves nearly 10 times.
WO at the bottom of the preparation porous silicon-base of the present invention
3The method of nanometer thin film gas sensitive transducer is except being applicable to WO
3Outside the nano thin-film, also applicable to SnO
2Nano thin-film, ZnO nano thin-film etc.; WO at the bottom of the porous silicon-base of the present invention
3Nanometer thin film gas sensitive transducer is the ideal material that is used for making low working temperature gas sensor at present.
Claims (4)
1. one kind prepares WO at the bottom of the porous silicon-base
3The method of nanometer thin film gas sensitive transducer has following steps:
(1) preparation porous silicon layer substrate:
Adopt the p of double flute electrochemical erosion method at single-sided polishing
+Monocrystalline silicon sheet surface prepares porous silicon layer, used corrosive liquid be volume ratio 1: 1 the mixed liquor of hydrofluorite (40%) and absolute ethyl alcohol, apply the size of corrosion electric current density and porosity, the thickness that etching time changes porous silicon layer by control, the corrosion electric current density that applies is 20～80mA/cm
2, etching time is 5～30min;
(2) preparation WO
3Nano thin-film:
The porous silicon layer substrate that step (1) is made places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% tungsten as target, concrete process conditions are: base vacuum degree (2～4) * 10
-4Pa, operating air pressure 1.0～2.0Pa, working gas (argon gas, purity 99.9%) is 9: 1～1: 9 with the ratio of reacting gas (oxygen, purity 99.9%) flow, sputtering power 60～100W, sputtering time 2～30min, substrate temperature are the chamber;
(3) annealing in process
WO at the bottom of the porous silicon-base that step (2) is made
3Nano thin-film places in the high-temperature heater, and the annealing in process environment is an atmospheric environment, and the annealing in process temperature is 400～600 ℃, and the annealing in process time is 2～4h, then with the stove natural cooling;
(4) plated electrode
The WO that step (3) is made
3Nano thin-film places the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt quality purity be 99.995% metal platinum as target, with quality purity be 99.999% argon gas as working gas, base vacuum degree (2.0～7.0) * 10
-4Pa, sputter operating air pressure 2Pa, sputtering time 8min, Ar gas flow 24ml/min is at WO
3The nano thin-film surface deposition forms two square Pt electrodes, makes WO at the bottom of the porous silicon-base
3Nanometer thin film gas sensitive transducer.
2. according to WO at the bottom of the preparation porous silicon-base of claim 1
3The method of nanometer thin film gas sensitive transducer is characterized in that, the porous silicon layer aperture size of described step (1) is about 10～20nm, and the degree of depth is 20～80 μ m, and porosity is 50～76.80%.
3. according to WO at the bottom of the preparation porous silicon-base of claim 1
3The method of nanometer thin film gas sensitive transducer is characterized in that, the vacuum chamber of the ultrahigh vacuum facing-target magnetron sputtering system equipment of described step (2), step (4) is the vacuum chamber of DPS-III type ultrahigh vacuum facing-target magnetron sputtering system equipment.
4. according to WO at the bottom of the preparation porous silicon-base of claim 1
3The method of nanometer thin film gas sensitive transducer is characterized in that, the minitype digital temperature controller is adopted in the annealing temperature control of described step (3).
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