CN103864460A - Preparation method of sequenced tungsten oxide nanowire array structure - Google Patents
Preparation method of sequenced tungsten oxide nanowire array structure Download PDFInfo
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- CN103864460A CN103864460A CN201410083125.5A CN201410083125A CN103864460A CN 103864460 A CN103864460 A CN 103864460A CN 201410083125 A CN201410083125 A CN 201410083125A CN 103864460 A CN103864460 A CN 103864460A
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Abstract
The invention discloses a preparation method of a sequenced tungsten oxide nanowire array structure. The preparation method comprises the following steps: carrying out direct in-situ assembling on a multistage tungsten oxide nano-structure on the surface of a substrate in a seed-layer induced growth manner; preplating a tungsten film source material layer on the substrate, transferring the substrate into a tube furnace, and carrying out recrystallization and annealing treatment, so as to obtain a tungsten oxide nanowire with a good appearance. The preparation method has the characteristics of simple experiment method, low experiment cost, flexible experiment condition and easiness in control. According to the preparation method, tungsten oxide nanowire arrays having the characteristics of large specific surface area, accuracy in positioning and large density grow on monocrystalline silicon, porous silicon and aluminum oxide substrates without using a catalyst at the lower temperature; and the sequenced tungsten oxide nanowire array structure is an ideal material for preparing gas sensitive sensors, electrochromic films, electronic field emission devices and light-catalyzed electrolysis water electrodes.
Description
Technical field
The invention relates to nano material, relate in particular to a kind of preparation method of orderly tungsten oxide nanometer linear array structure.
Background technology
The nano material of the main nulling dimension of nano material, a peacekeeping two dimension.Nano particle all at nanoscale, is zero-dimension nano material in three dimensions of solid space.Nano wire, nanometer rod, nanotube at nanoscale, are monodimension nanometer materials in two dimensions of solid space.The film of nano thickness only has a dimension at nanoscale in solid space, is two-dimensional nano material.
In tungstic oxide, there is some lattice defect, lattice oxygen atom vacancy, causing tungstic oxide is a kind of N-shaped semi-conductor, its energy gap arrives 2.9ev at 2.5ev.It is widely used, the especially nano material of tungstic oxide in electrochomeric films, gas sensor, ultracapacitor, smart window, photocatalysis to degrade organic matter, a transmitting field.
The widespread use of tungsten trioxide nanowires, need to study a kind of method that technique is simple, stable, can big area prepare tungsten trioxide nanowires.A lot of tungsten trioxide nanowires preparation methods in document, are reported.Prepare tungsten trioxide nanowires comprising thermal evaporation, hydrothermal method, sol-gel method.Hydrothermal method and sol-gel method preparation process are simple, and the material obtaining is pure, and favorable repeatability also can be grown on a large scale, and change experiment condition, can also obtain special nanostructure, as nano flower, and nanometer ball structure, these have report in the literature.But the great majority that obtain are in this way nano wire powder, the report of directly growing on base material is little, even if be grown in substrate, the direction of growth is also unordered.With with thermal evaporation compared with the substrate surface direct growth nano wire, chemical process a little less than the nano wire of substrate surface growth and the sticking power of substrate, thereby limited its application.
About thermal evaporation growth tungsten oxide nano, in bibliographical information, conventionally adopt the method for thermal evaporation tungsten powder or tungsten trioxide powder to obtain tungsten trioxide nanowires or nano-wire array.But this method needs extra high temperature.Because the fusing point of tungsten powder and tungstic oxide is high, thermal evaporation process needs the high temperature of 900-1100 ℃, and growth technique condition harshness, high to experimental installation requirement, repeatable poor, is not easy to realize scale operation.Thermal evaporation method advantage is that the sticking power of the nano wire that obtains in substrate and substrate is good, can obtain orderly nano-wire array, and be easy to realize heterojunction structure, enriches its Application Areas.
Summary of the invention
Object of the present invention, for avoiding hydrothermal method and thermal evaporation to prepare the shortcoming of nano wire, adopts W film recrystallization method to be low to moderate in temperature to grow under the condition of 600 ℃ orderly tungsten oxide nanometer linear array.Utilize the method growth tungsten oxide nano experiment condition gentleness, experimental installation is simple, and preparation process is easy, is easy to realize scale production.The present invention can prepare the orderly tungsten oxide nanometer linear array that pattern is good in the multiple substrates such as silicon single crystal, porous silicon or alumina-ceramic.
The present invention is achieved by following technical solution
A preparation method for orderly tungsten oxide nanometer linear array structure, has following steps:
(1) clean substrate
Silicon single crystal, porous silicon or alumina-ceramic substrate are put into beaker, in beaker, add dehydrated alcohol, put into ultrasonic cleaning device ultrasonic cleaning 20 minutes; Take out substrate, with after deionized water rinsing, then in hydrofluoric acid solution, continue ultrasonic cleaning 5-10 minute, with thorough clean surface impurity; Then, continue ultrasonic cleaning 20 minutes with deionized water; Again that substrate is dry, for subsequent use under air atmosphere;
(2) deposits tungsten Thin-film Sources material layer
Utilize silicon single crystal, porous silicon or the alumina-ceramic substrate surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean; Using tungsten as target, using argon gas as sputter gas, argon flow amount is 35-40sccm, and sputter operating air pressure is 2.0Pa, and sputtering power is 80-100W, and sputtering time is 10-20min;
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment, the orderly tungsten oxide nano of growing; Ambiance is the mixed gas of oxygen and argon gas, in process of growth, controls oxygen and argon flow amount and is respectively 0.1-0.3sccm and 30-40sccm, and controlling growth pressure in stove is 150-160Pa;
The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be raised to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃; At 600 ℃ of insulation 1-2 hour, insulation finishes, and naturally cools to room temperature.
The quality purity of the target tungsten of described step (2) is 99.999%.
The quality purity of the sputter gas argon gas of described step (2) is 99.999%.
The thickness of the W film of described step (2) sputtering sedimentation is 50-100nm.
The invention provides the preparation method of the orderly tungsten oxide nanometer linear array of a kind of low temperature large area deposition high-density, by the source material layer as tungsten oxide nano growth at substrate surface pre-deposition W film, and then in vacuum tube furnace, making W film recrystallize, nano wire is from upwards accurate oriented growth and obtained orderly nano-wire array of the tungsten thin film layer of electrode surface.Method of the present invention is prepared tungsten oxide nanometer linear array and is not used catalyzer, and experimental technique is simple, cost is low, experiment condition is flexible, be easy to control.
Accompanying drawing explanation
Fig. 1 is the low power inclined surface SEM picture of embodiment 1 processing condition lower mono-crystalline silicon substrate surface gained ordered nano line;
Fig. 2 is the high power inclined surface SEM picture of embodiment 1 processing condition lower mono-crystalline silicon substrate surface gained ordered nano line;
Fig. 3 is SEM picture in the high power of gained ordered nano line surface in alumina substrate under embodiment 2 processing condition;
Fig. 4 be under embodiment 3 processing condition at the bottom of porous silicon-base on the inclined surface SEM picture of gained ordered nano line;
Fig. 5 is the XRD spectra of gained nano wire in alumina substrate under embodiment 1 processing condition;
Fig. 6 is the TEM of gained nano wire figure in alumina substrate under embodiment 1 processing condition.
Embodiment
The present invention is raw materials used all adopts commercially available chemically pure reagent, below in conjunction with specific embodiment, the present invention is described in more detail.
Embodiment 1
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.
The product obtaining under the processing condition of the present embodiment is analyzed: Fig. 1, Fig. 2 are low power and the high power inclined surface SEM picture of monocrystal silicon substrate surface gained ordered nano line.As seen from the figure, silicon chip surface grows evenly intensive nano wire of diameter, and nanowire diameter is in 10nm left and right, and length is in 2 μ m left and right, and nanowire surface is smooth does not have bending, upwards grows along substrate, and directional property is good.Fig. 5 be Tc at 600 ℃, argon gas and oxygen flow are respectively under 35sccm and 0.1sccm condition the XRD spectra of gained nano wire in alumina substrate.As seen from the figure, nano wire is monocline WO
3structure, the diffraction peak that crystal face (002) is corresponding is the strongest, and WO is described
3nano wire is along the growth of [002] direction.Fig. 6 be Tc at 600 ℃, argon gas and oxygen flow are respectively the TEM of gained nano wire figure in alumina substrate under 35sccm and 0.1sccm condition.As seen from the figure, nano wire, along the growth of [002] direction, coincide with the result that XRD spectra obtains, and single nanowire diameter, in 15nm left and right, obtains nanowire diameter result with SEM picture and coincide.
Embodiment 2
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first alumina substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the alumina surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 90W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃ from 500 ℃ of room temperatures, 10 ℃/min of temperature rise rate.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.
The product obtaining under the processing condition of the present embodiment is analyzed: Fig. 3 is the high power surface SEM picture of gained ordered nano line in alumina substrate.As seen from Figure 3, Tc is in the time of 600 ℃, and alumina substrate surface growth goes out in a large number certainly to nano wire, nanowire diameter is between 10nm～20nm, and diameter is even, and length is in 2 μ m left and right, be column, nanowire surface is smooth, and every line is grown separately.
Embodiment 3
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first, by putting into beaker at the bottom of porous silicon-base, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the porous silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 25min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 700 ℃ from 500 ℃ of room temperatures, 10 ℃/min of temperature rise rate.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.
The product obtaining under the processing condition of the present embodiment is analyzed: Fig. 4 be at the bottom of porous silicon-base on the inclined surface SEM picture of gained ordered nano line, as seen from Figure 4, Tc is in the time of 600 ℃, alumina substrate surface growth goes out in a large number certainly to nano wire, and nanowire diameter is between 10nm～20nm, and diameter is even, length is in 2 μ m left and right, be column, nanowire surface is smooth, and every line is grown separately.
Embodiment 4
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 10 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.Product analysis is observed: nanowire growth is good, smooth surface does not have bending, upwards grows along substrate, and directional property is good, similar to embodiment 1 resulting product.
Embodiment 5
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 40sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.Product analysis is observed: nanowire growth is good, smooth surface does not have bending, upwards grows along substrate, and directional property is good, similar to embodiment 1 resulting product.
Embodiment 6
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 30sccm and 0.2sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.Product analysis is observed: nanowire growth is good, smooth surface does not have bending, upwards grows along substrate, and directional property is good, similar to embodiment 1 resulting product.
Embodiment 7
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 40sccm and 0.3sccm by gas meter control flow, furnace pressure remains on 150Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.Product analysis is observed: nanowire growth is good, smooth surface does not have bending, upwards grows along substrate, and directional property is good, similar to embodiment 1 resulting product.
Embodiment 8
(1) clean substrate
Substrate must thoroughly clean before use, to remove surface impurity.Substrate cleans and uses ultrasonic cleaning device, first monocrystal silicon substrate is put into beaker, in beaker, adds dehydrated alcohol, is placed in ultrasonic cleaning device ultrasonic cleaning 20 minutes.Take out substrate, with after deionized water rinsing, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity.Then, continue ultrasonic cleaning 20 minutes with deionized water.Finally, by substrate drying for standby under air atmosphere.
(2) prepare W film
Utilize the monocrystalline silicon surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean.Using the tungsten of quality purity 99.999% as target, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, and sputtering power is 80W, argon flow amount 35sccm, sputtering time is 20min.The thickness of gained sputter W film is about 50nm.
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment.The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be warmed up to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃.In this process, pass into argon gas and oxygen, be respectively 35sccm and 0.1sccm by gas meter control flow, furnace pressure remains on 160Pa.600 ℃ of insulations 1 hour, insulation finished, and naturally cools to room temperature.Goods are mazarine.Product analysis is observed: nanowire growth is good, smooth surface does not have bending, upwards grows along substrate, and directional property is good, similar to embodiment 1 resulting product.
Claims (4)
1. a preparation method for orderly tungsten oxide nanometer linear array structure, has following steps:
(1) clean substrate
Silicon single crystal, porous silicon or alumina-ceramic substrate are put into beaker, in beaker, add dehydrated alcohol, put into ultrasonic cleaning device ultrasonic cleaning 20 minutes; Take out substrate, with after deionized water rinsing, then in hydrofluoric acid solution, continue ultrasonic cleaning 5-10 minute, with thorough clean surface impurity; Then, continue ultrasonic cleaning 20 minutes with deionized water; Again that substrate is dry, for subsequent use under air atmosphere;
(2) deposits tungsten Thin-film Sources material layer
Utilize silicon single crystal, porous silicon or the alumina-ceramic substrate surface deposits tungsten Thin-film Sources material layer of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment in dried and clean; Using tungsten as target, using argon gas as sputter gas, argon flow amount is 35-40sccm, and sputter operating air pressure is 2.0Pa, and sputtering power is 80-100W, and sputtering time is 10-20min;
(3) recrystallize of nano wire growth
In vacuum high-temperature tube furnace equipment, the W film of step (2) is carried out to recrystallize thermal treatment, the orderly tungsten oxide nano of growing; Ambiance is the mixed gas of oxygen and argon gas, in process of growth, controls oxygen and argon flow amount and is respectively 0.1-0.3sccm and 30-40sccm, and controlling growth pressure in stove is 150-160Pa;
The substrate that is coated with W film is placed on to the high-temperature zone of tube furnace, tube furnace is raised to 500 ℃ from room temperature, 5 ℃/min of temperature rise rate, then be raised to 600 ℃, 10 ℃/min of temperature rise rate from 500 ℃; At 600 ℃ of insulation 1-2 hour, insulation finishes, and naturally cools to room temperature.
2. the preparation method of a kind of orderly tungsten oxide nanometer linear array structure according to claim 1, is characterized in that, the quality purity of the target tungsten of described step (2) is 99.999%.
3. the preparation method of a kind of orderly tungsten oxide nanometer linear array structure according to claim 1, is characterized in that, the quality purity of the sputter gas argon gas of described step (2) is 99.999%.
4. the preparation method of a kind of orderly tungsten oxide nanometer linear array structure according to claim 1, is characterized in that, the thickness of the W film of described step (2) sputtering sedimentation is 50-100nm.
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| CN104655802A (en) * | 2015-01-28 | 2015-05-27 | 天津大学 | Preparation method of porous-silicon-based tungsten oxide nanowire composite structure |
| CN106145030A (en) * | 2015-04-23 | 2016-11-23 | 天津大学 | A kind of hud typed tungsten oxide cupric oxide heterojunction nano-wire array of vertical orientation and preparation method thereof |
| CN105699440A (en) * | 2016-03-02 | 2016-06-22 | 五邑大学 | Method for preparing tungsten oxide nanoflower hydrogen sensor |
| CN105699440B (en) * | 2016-03-02 | 2018-08-07 | 五邑大学 | A kind of preparation method of tungsten oxide nanometer flower hydrogen gas sensor |
| CN113003607A (en) * | 2019-12-20 | 2021-06-22 | 中国科学院理化技术研究所 | Dark blue tungsten oxide nanowire and preparation method thereof |
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