CN101135659A - Beta -Ga2O3nano lines and gas sensors preparing method, and gas sensing method for realizing quick-speed response - Google Patents
Beta -Ga2O3nano lines and gas sensors preparing method, and gas sensing method for realizing quick-speed response Download PDFInfo
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- CN101135659A CN101135659A CNA2006100321690A CN200610032169A CN101135659A CN 101135659 A CN101135659 A CN 101135659A CN A2006100321690 A CNA2006100321690 A CN A2006100321690A CN 200610032169 A CN200610032169 A CN 200610032169A CN 101135659 A CN101135659 A CN 101135659A
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Abstract
The preparation method for nanometer lines comprises: coating a metal on the silicon substrate; placing the gallium powder into the boat; the substrate is placed at a location away from the boat in proper distance; heating and keeping the temperature; blowing nitrogen gas into the heating furnace; after cooling the heating furnace to the room temperature; the nanometer lines are formed in the substrate. The method for preparing the sensor comprises: depositing the golden electrode on the silicon substrate with SiO2 layer; the distance between two electrodes is 1 mu m; connecting single nanometer line to the electrode; connecting the lead; making aging process. The fast oxygen response of the sensor: at first, the free carrier concentration in the nanometer is very low; by adjusting the oxygen, its electric conductance is very week; under the illumination of the ultraviolet light, the current passing through the nanometer line is increased into a certain value, it show the oxygen concentration in short time; after closing the illumination, the photo-generated carriers are fast combined, the photo-driven oxygen sensing character disappears.
Description
Technical field
The present invention relates to β-Ga
2O
3The preparation of nano wire and gas sensor thereof, this sensor are realized the rapid-action gas sensing method to oxygen under UV-irradiation.
Background technology
Nano material is because specific surface area is big, make its electrical properties very responsive to surface adsorption, when changing, the external environment factor can cause the variation of situations such as surface, interface ion, electron transport rapidly, its resistance of appreciable impact, utilize its changes in resistance can make sensor, be characterized in highly sensitive.Present many gas sensors have adopted nanoparticle structure, and their specific areas are big, the surface-active height, very responsive to surrounding environment, but the resistance of sensor is bigger, at high temperature reunites easily, has had a strong impact on long-time stability and the sensitivity of sensor.And monodimension nanometer material not only has the big advantage of specific area, and electrical conductivity is big, at high temperature also is difficult for reuniting, and the electricity that can significantly improve sensor is led and stability.Therefore, the researchist is applied to the gas sensing field with monodimension nanometer materials such as nanotube, nano wire, nano belt, and has obtained result preferably.
The electricity of one-dimensional nano structure metal oxide semiconductor is led, and is quite sensitive as zinc paste, tin oxide, indium oxide nano thread to ambient gas.In recent years, owing to their potential application on following small gas sensor, therefore be subjected to researcher's extensive concern.The change that electricity is led is owing to absorption and desorption to gas molecule, in addition also owing to the modulating action to carrier concentration in the nano wire and mobility edge.Yet because relatively slow gas absorption and desorption process, the electricity of nano wire is led the reaction of ambient gas slower.This drawbacks limit they fast-application on the reacting gas sensor.
Realize that the rapid-action method is the carrier concentration in the quick adjustment nano wire.As everyone knows, in a semiconductor, because the fast right generation in electronics-hole and cohesive process again make carrier concentration come to regulate significantly soon by light.Studies show that the oxide nano thread that high electricity is led need to reach balance for a long time under illumination, yet the oxide nano thread that low electricity is led is under illumination, the short time can reach balance.Among the present invention, the characteristics that the oxide nano thread that we lead based on this low electricity reaches counterbalance weight realize the optical drive oxygen sensor.This way yet there are no not report.
Summary of the invention
The technical problem to be solved in the present invention is that the deficiency for prior art exists proposes a kind of β-Ga
2O
3The preparation method of nano wire and under UV-irradiation, realize fast reaction to oxygen, described method is simple, controlled, and cost is low; The preparation device stability good, the reaction time is fast, highly sensitive.
One of technical scheme of the present invention is described β-Ga
2O
3The preparation method's of nano wire step is:
(1) the golden film with 1 nanometer-1 micron thickness is deposited on the base substrate;
(2) the gallium metal particle is put into the alumina boat, substrate is placed on apart from 0.8 centimetre-1.2 centimeters of boat, makes it together to heat, be incubated by following condition;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, then tubular furnace is heated to 970 ℃-990 ℃, kept 0.9-1.1 hour;
(4) nitrogen of feeding 380sccm-420sccm (ml/min) in the heating furnace;
(5) behind the tube furnace cool to room temperature, product-β-Ga
2O
3Nano wire generates in base substrate;
Described base substrate can be N type silicon substrate or P type silicon substrate, Silicon-On-Insulator substrate, also can be other exotic material.
Described golden film, method deposition that can be by thermal evaporation, sputter or electron beam evaporation, golden film thickness is in 1 nanometer-1 micron thickness, is one of preferred with 10 nanometer thickness.
Described heating process can also be to heat in certain vacuum or heat in atmosphere.But, heating system inside need to have the oxygen of certain content to exist.
Two of technical scheme of the present invention is described β-Ga
2O
3The preparation method of nano wire gas sensor:
(1) thickness is that the gold electrode of 40nm-60nm deposits to thickness by means of electron beam deposition and is
400nm-600nm, following with Si0
2On the silicon substrate of layer.
(2) two electrode distances 0.8 μ m-1.2 μ m;
(3) with single β-Ga
2O
3Nano wire is put on the described electrode, makes it to connect this two electrode;
(4) lead-in wire connects, and namely gets product sensor, become product again through 24 hours burin-in process.
The substrate of described two electrodes is to realize by photoetching on potsherd.
The substrate of described two conductive electrodes can be at insulating trips such as silicon chip or potteries.Its electrode can be realized by methods such as photoetching or printings.Described conductive electrode can be metal electrode, such as gold, resistant to elevated temperatures platinum electrode etc., can also be the electrodes such as graphite.And surface that it should be noted that nano wire is very smooth.
Described oven dry or sintering (burin-in process) mainly are in order to improve the caking ability of ITO nano wire on substrate or ceramic pipe, to prevent to come off, improving device stability.
Three of technical scheme of the present invention is that the described realization fast gas sensing method of response is by using the sensor of the present invention that is made by said method, to realize quick oxygen reaction; During beginning, the free carrier concentration in nano wire is very low, a little less than regulating its electricity and lead very by oxygen, under UV Light, is increased to certain value by the electric current in the nano wire, has reflected at short notice the pressure of oxygen; After illumination was closed, photo-generated carrier is again combination rapidly, and optical drive oxygen sensor characteristic disappears.
Below the present invention made further specify.
The present invention has synthesized β-Ga in a large number by thermal evaporation gallium powder
2O
3Nano wire.The diameter of these nano wires can be in tens nanometer range, and length can reach tens microns.
Respectively its pattern, crystal structure and optical property are analyzed with scanning electron microscope (SEM), X-ray diffractometer (XRD) and the x-ray spectrometer that can loose, Raman scattering instrument.
Fig. 1 (a) is the TEM figure of a sample of growing on silicon substrate, can see the whole pattern of sample, major part be diameter in tens nanometer range, length can reach tens microns nano wire.Fig. 1 (b) and Fig. 1 (c) are the high power TEM images of nano wire, have observed mono-crystalline structures, and corresponding diffraction result is in Fig. 1 (d).
β-Ga
2O
3The electrons transport property of nano wire characterizes with the model device that single nano-wire connects two gold electrodes.Depress by the oxygen of dry oxygen (99.99%) adjusting in vacuum chamber neutralization and to measure.
In the dark, or under indoor incandescence, or when under green glow, measuring, very little by the electric current of nano wire, and the change of pressing with oxygen has faint variation.On the contrary, under the illumination of 254nm wavelength, electric current increases considerably.This is consistent with the light reflection spectrum of nano wire among Fig. 2.Luminous reflectivity spectrum is that the reflectance spectrum of tens microns nano wire film obtains by direct detect thickness.Suddenly the explanation nano wire that descends has absorbed the radiation of wavelength less than 270nm very doughtily.With these results of physical interpretation, only has photon energy greater than β-Ga
2O
3The forbidden band of nano wire can light (be the light of 254nm such as wavelength) just can cause the rapid increase of carrier in the nano wire and the obvious increase of electric current.
The present invention depresses at different oxygen, is not having and the electric current of measuring under the UV-irradiation of 254nm wavelength of bias voltage 20V by nano wire is arranged, and Fig. 3 provides the result.Fig. 3 (a) shows not to be had under the illumination condition, and electric current is 26pA, and in that depress fluctuation at different oxygen very little.On the contrary, under illumination condition, electric current rapidly increases to certain value, reflect the value that oxygen is pressed in the chamber, electric current is respectively 0.56,0.23, and 0.15 and 0.095nA, oxygen is pressed and is respectively 22 in the chamber, 540,5000 and 20000Pa, under the illumination, depress current reduction in higher oxygen, further prove above-mentioned conclusion [Fig. 3 (b) by measuring current value under the condition of constantly falling low oxygen pressure.More as can be known, nano wire only just has sensitivity to oxygen under irradiation in Fig. 3 (b), and the optical drive oxygen sensor is different from the gas sensor of introducing in the past under the room temperature, and it is the reason that causes the quick oxygen reaction of our devices.
Do not having under the 254nm length ultraviolet irradiation condition, the carrier concentration in the nano wire is very low.Fig. 3 (a) shows its low-down electric current.As everyone knows, the chemical potential of oxygen is lower than β-Ga
2O
3The conduction band energy.In the time of in being exposed to oxygen, oxygen molecule meeting chemisorbed causes the transmission of electronics from nano wire to oxygen molecule on the surface, forms oxonium ion on the surface, such as O
2 -, because low-down carrier concentration, although depress at a very low oxygen, most free electrons also can be caught by the oxygen molecule that is adsorbed on the surface, shown in Fig. 4 (a).Leading by the electricity of the nano wire after the oxygen modulation will be very little, so our device does not have sensitiveness to oxygen.
Yet when under the 254nm wavelength light irradiation, because the quick generation of electron-hole pair, the carrier concentration in the nano wire increases sharply, shown in Fig. 4 (b).In this case, more Surface Oxygen ion will produce, and the increase of Surface Oxygen ion directly is pressed with the pass with oxygen, reflects the size of oxygen pressure in the chamber by the electric current in the nano wire.Because the light sensitivity that oxidation absorption produces also has discovery in bulk or thin-film metallic oxide, oxide nano thread is because its big specific area, research this rule be a kind of ideal system, nano wire is owing to high carrier concentration has oxygen sensor in the report before, arranged, this and β-Ga the long reaction time under illumination
2O
3The nano wire difference.β-Ga
2O
3Nano wire has low carrier concentration, only just can have the oxygen sensor characteristic under UV-irradiation, and our device rapid-action reason is because this special optical drive oxygen sensor characteristic.
Generally, the oxygen of adsorption affects two approach that conducted of single nano-wire, at first, oxonium ion can with again combination of photohole, discharge an oxygen molecule; Another oxygen molecule of absorption forms oxonium ion with trapped electrons, and in this process, the concentration in electronics and hole all can reduce, and depresses in higher oxygen, and more Surface Oxygen ion forms, and therefore, carrier concentration can be lower.Secondly, the Surface Oxygen ion forms scattering center, thereby reduces the mobility of carrier, so the electric current in the nano wire is pressed to increase with oxygen and descended, such as Fig. 3.
Contacting also of nano wire and gold electrode can change with the variation that oxygen is pressed, and once has report, oxygen molecule to be adsorbed on the gold electrode, and concurrent charge transport will produce an interface dipole, sets up an outside electric field.This electric field makes electronics be difficult to discharge from gold electrode, causes the small increase of work function on the gold electrode.Therefore, depress in higher oxygen, reduce in the potential barrier of nano wire/gold electrode contact position, this may cause not having under the illumination condition, and also can observe the increase that electric current presses with oxygen in some devices increases.Therefore, this increase can not explain that by considering nano wire self do not lead because oxygen affects electricity, this contact is exposed at nano wire plays small effect under the 254nm wavelength light.
In sum, the present invention is β-Ga
2O
3The preparation of nano wire and gas sensor thereof and realization be the gas sensing method of response fast, and it passes through a kind of quick method to oxygen reaction of design, and uses β-Ga
2O
3Nano wire is achieved.When under ultraviolet light illumination, be increased to certain value by the electric current in the nano wire, reflected the pressure of oxygen at short notice, provide the method for preparing the quick oxygen sensor of room temperature thus; Described method is simple, controlled, and cost is low; The device stability of preparation is good, the reaction time is fast, release time is short, stable performance, and noise is low, and is highly sensitive, is suitable for the commercial production of scale.
Description of drawings
Fig. 1 (a) is the TEM figure of a sample of growing on silicon substrate;
Fig. 1 (b) is β-Ga
2O
3The high power TEM image of nano wire;
Fig. 1 (c) is β-Ga
2O
3The high power TEM image of nano wire;
β-Ga among Fig. 1 (d)
2O
3The high power TEM diffraction pattern of nano wire;
Fig. 2 is β-Ga
2O
3The reverberation spectrogram of nano wire
Fig. 3 (a) is β-Ga
2O
3The nano wire gas sensor is not having under the illumination condition, the situation of change that electric current is pressed with oxygen;
Fig. 3 (b) is β-Ga
2O
3The nano wire gas sensor is not having under the illumination condition, the situation of change that electric current is pressed with oxygen;
Fig. 4 is β-Ga
2O
3The sensing process schematic diagram of nano wire gas sensor.
Embodiment
Embodiment 1: β-Ga
2O
3The fabricate of nanowires method:
(1) the golden film with 10 nanometer thickness is deposited on the base substrate;
(2) the gallium powder is put into boat, substrate is placed on apart from boat 1 centimeters, together heats, is incubated;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, tubular furnace is heated to 980 ℃ then, kept 1 hour;
(4) nitrogen of feeding 400sccm (ml/min) in the heating furnace;
(5) behind the tube furnace cool to room temperature, product-β-Ga
2O
3Nano wire generates in base substrate;
Described base substrate can be N type silicon substrate, P type silicon substrate, Silicon-On-Insulator substrate, also can be other exotic material.
Described golden film can be by the method deposition of thermal evaporation, sputter or electron beam evaporation, and golden film thickness is 10 nanometer thickness.
Described heating process can also be to heat in certain vacuum or heat in atmosphere.But, heating system inside need to have the oxygen of certain content to exist.
Embodiment 2: β-Ga
2O
3The preparation of nano wire gas sensor:
(1) thickness is that to deposit to thickness by means of electron beam deposition be 500nm, following with SiO for the gold electrode of 50nm
2On the silicon substrate of layer.
(2) two electrode distances 1 μ m.；
(3) single nano-wire is put on the electrode;
(4) lead-in wire connects.Become product through 24 hours burin-in process.
The substrate of described two electrodes is to realize by photoetching on potsherd.And surface that it should be noted that nano wire is very smooth.
Embodiment 3: the present invention depresses at different oxygen, is not having and the electric current of measuring under the UV-irradiation of 254nm wavelength of bias voltage 20V by nano wire is arranged, and Fig. 3 provides the result.Fig. 3 (a) shows not to be had under the illumination condition, and electric current is 26pA, and in that depress fluctuation at different oxygen very little.On the contrary, under illumination condition, electric current rapidly increases to certain value, reflect the value that oxygen is pressed in the chamber, electric current is respectively 0.56,0.23, and 0.15 and 0.095nA, oxygen is pressed and is respectively 22 in the chamber, 540,5000 and 20000Pa, under the illumination, depress current reduction in higher oxygen, further prove above-mentioned conclusion [Fig. 3 (b)] by measuring current value under the condition of constantly falling low oxygen pressure.More as can be known, nano wire only just has sensitivity to oxygen under irradiation in Fig. 3 (b), and the optical drive oxygen sensor is different from the gas sensor of introducing in the past under the room temperature, and it is the reason that causes the quick oxygen reaction of our devices.
Claims (7)
1. β-Ga
2O
3The preparation method of nano wire is characterized in that, this method is:
(1) the golden film with 1 nanometer-1 micron thickness is deposited on the base substrate;
(2) the gallium metal particle is put into the alumina boat, substrate is placed on apart from 0.8 centimetre-1.2 centimeters of boat, makes it together to heat, be incubated by following condition;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, then tubular furnace is heated to 970 ℃-990 ℃, kept 0.9-1.1 hour;
(4) nitrogen of feeding 380sccm-420sccm (ml/min) in the heating furnace;
(5) behind the tube furnace cool to room temperature, product-β-Ga
2O
3Nano wire generates in base substrate;
2. according to the described β-Ga of claim 1
2O
3The preparation method of nano wire is characterized in that, described base substrate is N-type silicon substrate or P type silicon substrate, SOI substrate.
3. β-Ga
2O
3The preparation method of nano wire gas sensor is characterized in that, this method is:
(1) thickness is that to deposit to thickness by means of electron beam deposition be 400nm-600nm, following with SiO for the gold electrode of 40nm-60nm
2On the silicon substrate of layer.
(2) two electrode distances 0.8 μ m-1.2 μ m;
(3) with single β-Ga
2O
3Nano wire is put on the described electrode, makes it to connect this two electrode;
(4) lead-in wire connects, and namely gets product sensor, become product again through 24 hours burin-in process.
4. according to the described β-Ga of claim 3
2O
3Nano wire gas sensor preparation method is characterized in that, the substrate of described two electrodes is to realize by photoetching on potsherd.
5. according to the described β-Ga of claim 3
2O
3Nano wire gas sensor preparation method is characterized in that, the surface of described nano wire is smooth surface.
6. according to the described β-Ga of claim 3
2O
3The preparation method of nano wire gas sensor is characterized in that, described conductive electrode is metal electrode or graphite electrode.
7. realize the fast gas sensing method of response for one kind, it is characterized in that, by the sensor that right to use requires 3 method to make, realize quick oxygen reaction; During beginning, the free carrier concentration in nano wire is very low, a little less than regulating its electricity and lead very by oxygen, under UV Light, is increased to certain value by the electric current in the nano wire, has reflected at short notice the pressure of oxygen; After illumination was closed, photo-generated carrier is again combination rapidly, and optical drive oxygen sensor characteristic disappears.
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| CN103868951A (en) * | 2014-02-24 | 2014-06-18 | 北京大学 | Method for preparing nanowire array gas sensitive elements by dry method |
| CN103868951B (en) * | 2014-02-24 | 2016-12-07 | 北京大学 | A kind of method of dry process nano-wire array gas sensor |
| CN105481002A (en) * | 2015-11-03 | 2016-04-13 | 辽宁师范大学 | Autocatalysis growth method for large-dimension beta-Ga2O3 microwire |
| CN105481002B (en) * | 2015-11-03 | 2017-04-19 | 辽宁师范大学 | Autocatalysis growth method for large-dimension beta-Ga2O3 microwire |
| CN105932104A (en) * | 2016-05-23 | 2016-09-07 | 中国科学院长春光学精密机械与物理研究所 | Gallium oxide solar-blind UV detector and preparation method thereof |
| CN105826433A (en) * | 2016-05-23 | 2016-08-03 | 中国科学院长春光学精密机械与物理研究所 | Beta-Gallium oxide nanowire array film and preparation method thereof |
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| CN112210768A (en) * | 2019-07-12 | 2021-01-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | Epitaxial method of vertical beta gallium oxide nanowire array |
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Application publication date: 20080305 |