CN1847837A - Prepn process of ITO nanometer line and its gas sensor - Google Patents
Prepn process of ITO nanometer line and its gas sensor Download PDFInfo
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- CN1847837A CN1847837A CN 200610031534 CN200610031534A CN1847837A CN 1847837 A CN1847837 A CN 1847837A CN 200610031534 CN200610031534 CN 200610031534 CN 200610031534 A CN200610031534 A CN 200610031534A CN 1847837 A CN1847837 A CN 1847837A
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Abstract
The present invention discloses the preparation process of ITO nanometer line and its gas sensor. The preparation process of ITO nanometer line includes the steps of: depositing one layer of gold film on substrate; setting the mixture of indium oxide, stannous oxide and graphite in certain weight proportion in a boat, setting the substrate on the boat, and heating and maintaining inside quartz tube in a furnace; maintaining the pressure at 300 Pa while introducing mixed gas containing small amount of oxygen; and cooling to room temperature to form yellowish product on the substrate. The preparation process of the gas sensor includes the steps of ultrasonically dispersing the nanometer lines in solution, stoving, coating the slurry on and between two electrodes on ceramic tube, stoving and sintering, and connecting leads. The ITO nanometer line has excellent gas sensing characteristic and the gas sensor has short response time, short restoring time, high sensitivity and other advantages.
Description
Technical field
The present invention relates to the preparation method of a kind of ITO nano wire and gas sensor thereof.
Background technology
Nanometer technology is applied to sensory field, is expected to improve sensitivity, make the element microminiaturization, improve integrated level.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 that response speed is fast, highly sensitive, selectivity is good.Present many gas sensors have adopted nanoparticle structure, and their specific surface areas are big, the surfactivity height, very responsive to surrounding environment, but the resistance of sensor is bigger, at high temperature reunites easily, has had a strong impact on the long-time stability and the sensitivity of sensor.And monodimension nanometer material not only has the big advantage of specific surface area, and 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 one-dimensional nano structure metal oxide semiconductor, because its superior optics, chemistry, electricity and gas sensing characteristics are subjected to paying close attention to widely, especially tin oxide and indium oxide one-dimensional nano structure since they at electronics, the potential using value of optoelectronics and gas sensor aspect has obtained more concern.Now, use, thereby the compound monodimension nanometer material of research preparation indium-Xi-oxygen is very attractive because indium-Xi-oxygen complex material has in industry widely.In the recent period, the ito thin film material is widely used in preparing gas sensor and they have very high gas-sensitive property to ethanol.Usually monodimension nanometer material is because their high specific surface areas have higher sensitivity than blocks material.But, also do not report so far with the gas sensor of the ITO nano wire preparation that has more application prospect.
Present and the immediate work of the present invention has: the field emission of (1) ITO nanometer rods, material wall bulletin (Materials Letters 59 (2005) 1526-1529; (2) the gas sensor characteristic of ito thin film, sensor and tuner periodical (Sensors and Actuators B, 94 (2003) 216-221), solid film (Thin Solid Films 487 (2005) 277-282) (Thin Solid Films490 (2005) 94-100).
Summary of the invention
The technical problem to be solved in the present invention is, at the deficiency that prior art exists, proposes the preparation method of a kind of ITO nano wire and gas sensor thereof, and described method is simple, controlled, and cost is low; The device stability of preparation is good, highly sensitive.
One of technical scheme of the present invention is the preparation method of described ITO nano wire:
(1) the golden film with 1 nanometer-1 micron thickness is deposited on the base substrate;
(2) powder of indium oxide, stannous oxide and graphite is 1 with mass ratio: after 3.8-4.2: 0.8-1.2 fully mixes, mixed-powder is put into an alumina boat, base substrate is placed on the alumina boat;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, then tubular furnace is heated to 600 ℃-1200 ℃, kept 1 minute-10 hours;
(4) behind the tubular furnace cool to room temperature, little yellow product-ITO nano wire generates on base substrate;
In above-mentioned preparation process, the air pressure in the quartz ampoule is the 250-350 handkerchief, feeds argon gas and oxygen with the speed of 10-30sccm (ml/min) simultaneously with it, or the mixed gas of nitrogen and oxygen, the volume ratio 5%-20% of oxygen in the mixed gas.
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 in 1 nanometer-1 micron thickness.
Described heating process can also be to heat in certain vacuum or heat in atmosphere.But, heating system inside needs the oxygen existence of certain content.
Two of technical scheme of the present invention is the preparation method of described ITO nano wire gas sensor:
(1) the ITO nano wire is uniformly dispersed in solution or makes slurry;
(2) solution or slurry are dropped in or are coated on the substrate of two conductive electrodes or on the ceramic pipe and cover on the conductive electrode;
(3) oven dry or sintering promptly are heated to 50 ℃-960 ℃, 10 minutes-10 hours heat time heating time;
(4) lead-in wire connects.
Described solution can be alcohol, water
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 a metal electrode, as gold, resistant to elevated temperatures platinum electrode etc., can also be electrodes such as graphite.
Described oven dry or sintering 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.
Below the present invention made further specify.
The present invention has synthesized the ITO nano wire in a large number by the mixed-powder of thermal evaporation indium oxide, stannous oxide and graphite.The lateral dimension of these nano wires can be in the 70-150 nanometer range, and length can reach tens microns.Indium, tin, three kinds of elements of oxygen are evenly distributed in the whole nano wire, and the atomic concentration of indium is about 5%.Because the ITO nano wire is very responsive to alcohol gas, therefore can be made into gas sensor.When temperature was 400 ℃, the sensitivity in 200ppm alcohol was 40, and response and release time are about 2 seconds.These results show that preparing gas sensor with the ITO nano wire is good selection.
And the present invention has synthesized the Zn-Sn-O nano wire with this straightforward procedure, and same synthetic method can be used for synthetic various metal-doped tin oxide monodimension nanometer materials.
The ITO nano wire is carried out corresponding experimental analysis characterize its appearance, size, structure and measure its component.In air at room temperature, photoluminescence spectra is presented at very strong, a very wide peak about 617 nanometers, and the peak of this VISIBLE LIGHT EMISSION may derive from surface state.Gas sensor with the preparation of ITO nano wire has very high sensitivity to alcohol gas.Sensitivity is 40 in 200ppm alcohol.Response and release time are about 2 seconds.This sensitivity characteristic to ethanol is because due to the oxonium ion on absorption and desorption surface.Production in enormous quantities, high sensitivity and rapid reaction show that the ITO nano wire can be used for the industrialization production of gas sensor.
With scanning electron microscope (SEM; JEOL-JSM-6700F), X-ray diffractometer (XRD; D/max2550V, Cu Ka radiation) and the transmission electron microscope (TEM, Tecnai F20) that has an energy spectrometer respectively its pattern, crystal structure and component are analyzed.
Fig. 1 (a) is the SEM figure of a sample of growing on silicon substrate, can see the whole pattern of sample, major part be lateral dimension in the 70-150 nanometer range, length reaches tens microns nano wire.Survey the crystal structure of these nano wires with XRD, Fig. 1 (b) is an XRD figure, three main diffraction peaks are arranged, be respectively (110), (101), (211) crystal face of rutile structure tin oxide, other peaks are also consistent with the peak of this tin oxide rutile structure, see information paper (JCPPS FILE NO.41-1445), other significantly peak consistent do not occur with indium oxide.
In order to verify whether indium is incorporated in these yellowish nano wires, the subsidiary EDS of TEM is used to detect the component of single nano-wire, Fig. 2 (a) is the energy spectrogram of single nano-wire, shows and contain tin, indium, oxygen in the nano wire that their atomic ratio is 5.5: 31.6: 62.9.The peak of Cu and C derives from copper grid and the carbon film substrate in the TEM observation.We have also measured the power spectrum of 7 nano wires, the result shows that all nano wires all contain tin, indium, oxygen, and the atom content of indium is 4%-6%, what the illustration of Fig. 2 (a) showed is the element distribution of single nano-wire, tin, indium, three kinds of elements of oxygen are evenly distributed in the whole piece nano wire, and amount lacking than tin of indium as can be seen.Fig. 2 (b) is the high power TEM image of nano wire, has observed mono-crystalline structures, and corresponding diffraction result is in the illustration of Fig. 2 (b).
VLS or VS mechanism are followed in the growth of most of metal oxide one-dimensional nano structure, in VLS mechanism, at the end of nano wire an alloy particle are arranged usually, as the catalyzer of gas phase to solid state growth.The growth of ITO nano wire to the end of every nano wire this particulate arranged all by tem observation, so may be followed VLS mechanism.
The wavelength of having measured in air at room temperature with the emission of He-Cd lamp is the photoluminescence spectra of the laser of 325 nanometers as excitaton source, and as Fig. 3, very strong, a very wide peak is observed in 617 nanometers.Usually the VISIBLE LIGHT EMISSION of metal oxide one-dimensional nano structure as indium oxide nano thread, tin oxide nano band etc., all be to derive from surface state and oxygen vacancy, and VISIBLE LIGHT EMISSION does not observe in the ito thin film material, although also there is the oxygen vacancy in it.Therefore the ITO nano wire may be to derive from surface state in the strong VISIBLE LIGHT EMISSION of 617 nanometers.The ITO nano wire fact more much bigger that this result is also can be well corresponding than the specific surface area of ito thin film.
The gas sensitization characteristic of prepared sensor is measured in bottle type gas tank.Identical in humidity and the air in the cabin, alcohol gas does not contain water, so the influence of humidity can be ignored.Usually, sensitivity S is defined as Ra/Rg, and Ra is a resistance in the air, and Rg is the resistance in ethanol and air gas mixture.
Fig. 4 provide ITO nano wire gas sensor 10,30,50,200,500 and 1000ppm ethanol in response and release time, heating voltage is 6V, working temperature is 400 ℃, sensor has very high sensitivity to alcohol gas.Response and release time are about 2 seconds, and when 200ppm ethanol, sensitivity reaches 40, with the ito thin film material same level and high is slightly arranged.High and fast reaction makes it that good prospect be arranged in commercial production.
Usually, the high sensitivity of one-dimensional nano structure material is because due to the absorption and desorption of surperficial oxonium ion.Only consider single ITO nano wire, its sensing process is reflected in the illustration of Fig. 4.When sensor is in air, some oxygen molecules will be adsorbed on the surface of ITO nano wire, and the oxygen molecule of absorption is caught free electron from the conduction band of nano wire, form oxonium ion (O
-, O
2-, O
2 -), this has increased depletion width and has reduced conductivity, and when sensor is placed in the gas tank that contains a certain amount of ethanol, ethanol molecule will generate acetaldehyde with the oxonium ion reaction, the electronics of catching is released to be got back in the nano wire, and this process has reduced depletion width and increased conductivity.Therefore, the adsorption/desorption of this oxonium ion and big specific surface area make the ITO nanowire sensor have high sensitivity.In addition, the network-like structure of device nano wire may increase the oxygen adsorption rate, reduce release time.
As known from the above, the present invention is the preparation method of ITO nano wire and gas sensor thereof, thereby the preparation of ITO nano wire is because indium content seldom greatly reduces the cost of raw material, and material has good gas-sensitive property; Utilize the gas sensor of the material preparation of nanoscale that very high sensitivity is arranged, response and release time are very fast, stable performance, and noise is low, is suitable for the commercial production of scale.
Description of drawings
Fig. 1 (a) is the SEM figure of the sample of growing on silicon substrate;
Fig. 1 (b) is an XRD figure;
Fig. 2 (a) is the energy spectrogram and the distribution diagram of element of single nano-wire;
Fig. 2 (b) is the high power TEM image of nano wire;
Fig. 3 is ITO nano wire photoluminescence spectra figure;
Fig. 4 is response and the release time of ITO nano wire gas sensor in different content ethanol, and sensing process synoptic diagram.
Embodiment
Embodiment 1:ITO nano wire preparation method:
(1) the golden film with 5 nanometer thickness is deposited on the base substrate;
(2) after the powder of indium oxide, stannous oxide and graphite is 1: 3.8: 0.8 abundant mixing with mass ratio, mixed-powder is put into an alumina boat, base substrate is placed on the alumina boat;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, tubular furnace is heated to 600 ℃ then, kept 1 minute;
(4) behind the tubular furnace cool to room temperature, little yellow product-ITO nano wire generates on base substrate;
In above-mentioned preparation process, the air pressure in the quartz ampoule is 250 handkerchiefs, feeds the mixed gas of argon gas and oxygen, the volume ratio 5% of oxygen in the mixed gas simultaneously with the speed of 10sccm with it.
Described base substrate is a N type silicon substrate, and described golden film deposits by thermal evaporation.
Embodiment 2:ITO nano wire preparation method:
(1) the golden film with 1 micron thickness is sprayed on the base substrate;
(2) after the powder of indium oxide, stannous oxide and graphite is 1: 4.2: 1.2 abundant mixing with mass ratio, mixed-powder is placed in the alumina boat, base substrate is placed on the alumina boat;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, tubular furnace is heated to 1200 ℃ then, kept 10 hours;
(4) behind the tubular furnace cool to room temperature, little yellow product-ITO nano wire generates on base substrate;
In above-mentioned preparation process, the air pressure in the quartz ampoule is the 250-350 handkerchief, feeds the mixed gas of nitrogen and oxygen, the volume ratio 20% of oxygen in the mixed gas simultaneously with the speed of 30sccm with it.
Described base substrate is a P type silicon substrate, and golden film is by the method deposition of sputter or electron beam evaporation.
The preparation of embodiment 3:ITO nano wire gas sensor:
(1) the ITO nano wire is uniformly dispersed in ethanolic solution makes slurry;
(2) slurry is coated on the ceramic pipe of two gold electrodes and covers on the described electrode;
(3) oven dry or sintering promptly are heated to 50 ℃, 10 hours heat time heating times;
(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.
The preparation of embodiment 4:ITO nano wire gas sensor:
(1) the ITO nano wire is disperseed in water;
(2) with drips of solution on the ceramic pipe that two graphite electrodes are arranged and cover on the described electrode;
(3) oven dry or sintering promptly are heated to 660 ℃, 10 minutes heat time heating times;
(4) lead-in wire connects.
Claims (4)
1, a kind of preparation method of ITO 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) powder of indium oxide, stannous oxide and graphite is 1 with mass ratio: after 3.8-4.2: 0.8-1.2 fully mixes, mixed-powder is put into an alumina boat, base substrate is placed on the alumina boat;
(3) the alumina boat is put into quartz ampoule, again quartz ampoule is put into tubular furnace, then tubular furnace is heated to 600 ℃-1200 ℃, kept 1 minute-10 hours;
(4) behind the tubular furnace cool to room temperature, little yellow product-ITO nano wire generates on base substrate;
In above-mentioned preparation process, the air pressure in the quartz ampoule is the 250-350 handkerchief, feeds argon gas and oxygen with the speed of 10-30sccm simultaneously with it, or the mixed gas of nitrogen and oxygen, the volume ratio 5%-20% of oxygen in the mixed gas.
According to the preparation method of the described ITO nano wire of claim 1, it is characterized in that 2, described base substrate is N type silicon substrate or P type silicon substrate, Silicon-On-Insulator substrate.
3, a kind of preparation method of ITO nano wire gas sensor is characterized in that, this method is:
(1) the ITO nano wire is uniformly dispersed in solution or makes slurry;
(2) solution or slurry are dropped in or are coated on the substrate of two conductive electrodes or on the ceramic pipe and cover on the conductive electrode;
(3) oven dry or sintering promptly are heated to 50 ℃-960 ℃, 10 minutes-10 hours heat time heating time;
(4) lead-in wire connects;
Described solution is alcohol or water.
According to the preparation method of the described ITO nano wire of claim 3 gas sensor, it is characterized in that 4, described conductive electrode is metal electrode or graphite electrode.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101109687B (en) * | 2007-07-20 | 2010-06-02 | 北京工业大学 | Testing device for force-electricity property under nanowire original position stretching in transmission electron microscope |
| CN108112263A (en) * | 2015-08-28 | 2018-06-01 | 松下知识产权经营株式会社 | Gas sensor and fuel cell car |
| CN108588657A (en) * | 2018-04-17 | 2018-09-28 | 西安交通大学 | A method of it is sputtered using high RF power and prepares ITO nano wires and its gas sensor |
| CN111965324A (en) * | 2020-08-24 | 2020-11-20 | 深圳市美克森电子有限公司 | Preparation method of silicon-resistant gas-sensitive detection body of methane gas sensor |
| CN112557458A (en) * | 2020-12-04 | 2021-03-26 | 江南大学 | Preparation method of indium oxide nanowire and NO containing indium oxide nanowire2Method for manufacturing sensor and sensor |
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| JP2000275200A (en) * | 1999-03-24 | 2000-10-06 | Matsushita Electric Ind Co Ltd | Nox sensor and production thereof |
| JP2001264237A (en) * | 2000-03-21 | 2001-09-26 | Sony Corp | Permeability evaluation method of thin film and permeability evaluation device |
| US7153401B2 (en) * | 2002-05-13 | 2006-12-26 | The Regents Of The University Of California | Current-biased potentiometric NOx sensor for vehicle emissions |
| CN1237006C (en) * | 2003-10-10 | 2006-01-18 | 桂林电子工业学院 | In2O3 and ITO monodisperse nano powder hydrothermal preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101109687B (en) * | 2007-07-20 | 2010-06-02 | 北京工业大学 | Testing device for force-electricity property under nanowire original position stretching in transmission electron microscope |
| CN108112263A (en) * | 2015-08-28 | 2018-06-01 | 松下知识产权经营株式会社 | Gas sensor and fuel cell car |
| CN108588657A (en) * | 2018-04-17 | 2018-09-28 | 西安交通大学 | A method of it is sputtered using high RF power and prepares ITO nano wires and its gas sensor |
| CN111965324A (en) * | 2020-08-24 | 2020-11-20 | 深圳市美克森电子有限公司 | Preparation method of silicon-resistant gas-sensitive detection body of methane gas sensor |
| CN112557458A (en) * | 2020-12-04 | 2021-03-26 | 江南大学 | Preparation method of indium oxide nanowire and NO containing indium oxide nanowire2Method for manufacturing sensor and sensor |
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