CN110499497B - Preparation method of titanium dioxide nano film and titanium dioxide nano film - Google Patents
Preparation method of titanium dioxide nano film and titanium dioxide nano film Download PDFInfo
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- CN110499497B CN110499497B CN201910790001.3A CN201910790001A CN110499497B CN 110499497 B CN110499497 B CN 110499497B CN 201910790001 A CN201910790001 A CN 201910790001A CN 110499497 B CN110499497 B CN 110499497B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 46
- 239000002120 nanofilm Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 100
- 239000011261 inert gas Substances 0.000 claims abstract description 44
- 239000012495 reaction gas Substances 0.000 claims abstract description 29
- 238000010168 coupling process Methods 0.000 claims abstract description 15
- 230000008878 coupling Effects 0.000 claims abstract description 14
- 238000005859 coupling reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 22
- 239000000919 ceramic Substances 0.000 claims description 7
- 230000005684 electric field Effects 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 230000001939 inductive effect Effects 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 10
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000006872 improvement Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000010892 electric spark Methods 0.000 description 4
- 239000002073 nanorod Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002127 nanobelt Substances 0.000 description 3
- 239000002057 nanoflower Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000005348 self-cleaning glass Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a titanium dioxide nano film and the titanium dioxide nano film, and belongs to the field of titanium dioxide nano film processing. The preparation method of the titanium dioxide nano film comprises the following steps: s1, providing inert gas; s2, coupling the inert gas, and igniting the inert gas to generate a plasma torch of the inert gas; s3, introducing reaction gas into the inert gas plasma torch to generate a plasma torch containing the reaction gas; s4, applying a plasma torch containing a reactive gas to the sample surface. The preparation method of the titanium dioxide nano film has the advantages of simple and feasible preparation process and no secondary pollution.
Description
Technical Field
The invention relates to the field of titanium dioxide nano film processing, in particular to a preparation method of a titanium dioxide nano film and the titanium dioxide nano film.
Background
Titanium dioxide (TiO)2) The crystal structure of the wide-bandgap transparent metal oxide semiconductor is three types: rutile, anatase and brookite, which are common in nature are anatase phase and rutile phase, optical band gaps are more than 3.0eV, and the rutile, anatase and brookite composite material has excellent properties of photoinduced super-hydrophilicity, photocatalysis, photo-corrosion resistance and the like, and is widely concerned by people. Nano TiO 22The material has the characteristics of high chemical stability, high thermal stability, no toxicity, no harm, super hydrophilicity, non-migration and the like, and is widely applied to the fields of ultraviolet-resistant materials, photocatalytic catalysts, self-cleaning glass, sun cream, coatings, printing ink, food packaging materials, paper industry and the like.
So far, there have been numerous reports in the literature for the preparation of TiO2Various approaches to nanostructures such as sol-gel methods, anodic oxidation methods, electrophoresis methods, Chemical Vapor Deposition (CVD), magnetron sputtering methods, and the like. In order to obtain a unique pore structure and a high specific surface area, TiO with various morphologies and structures have been researched2Including nanoparticles, nanorods, nanoflowers, nanowires, nanotubes, and the like.The existing research shows that the nano structure can effectively improve TiO2Optical properties, photocatalytic activity and optical storage properties. In particular ordered TiO2The nanorod array has the characteristics of obvious quantum confinement effect, highly ordered oriented structure, high specific surface area and the like, and can effectively improve electrons－The interface separation capability of the hole pair and the directional transmission efficiency of the current carrier enable the hole pair to have important application prospects in the technical fields of dye-sensitized cells, photoelectrochemical cells, photo (electro) catalytic degradation pollutants, sensors and the like.
However, against the existing TiO2The preparation method of the nano structure generally has some disadvantages, such as: wet chemical methods such as Chemical Vapor Deposition (CVD) require the use of a large number of metallic titanium sheets for preparing the precursor solution, which is costly; the requirements of high-temperature oxidation and a part of wet chemical methods for a long-time high-temperature or vacuum condition on equipment are high, and potential safety hazards may exist; the strong acid consumed in the acid washing process of the titanium alloy or the titanium sheet is easy to cause secondary environmental pollution in the recovery treatment process, and is not beneficial to the industrialized utilization of the titanium alloy or the titanium sheet.
Therefore, the TiO is simple, convenient and feasible, and has no secondary pollution2The film preparation process becomes a problem of great research attention.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a preparation method of a titanium dioxide nano film
The embodiment of the invention adopts the following technical scheme for solving the technical problems: the preparation method of the titanium dioxide nano film comprises the following steps: s1, providing inert gas; s2, providing a plasma torch of inert gas; s3, introducing reaction gas into the inert gas plasma torch to generate a plasma torch containing the reaction gas; s4, applying a plasma torch containing a reactive gas to the sample surface.
As a further improvement of the above technical solution, a first gas layer, a second gas layer and a third gas layer are sequentially arranged from inside to outside, and the ends of the first gas layer, the second gas layer and the third gas layer are communicated; and the inert gas is introduced through the second gas layer and the third gas layer, and the reaction gas is introduced through the first gas layer.
As a further improvement of the above technical solution, a gas flow rate of the second gas layer is greater than a gas flow rate of the third gas layer, and the gas flow rate of the third gas layer is greater than the gas flow rate of the first gas layer.
As a further improvement of the above technical means, in S2, the inert gas is acted on by inductive coupling or capacitive coupling.
As a further improvement of the technical proposal, an electric field is arranged above the sample, and the plasma generated by coupling moves towards the sample direction under the action of the electric field.
As a further improvement of the above technical solution, before S4, a sample is pretreated, and the pretreatment process includes: firstly, polishing the surface of a sample until the surface of the sample is smooth, then ultrasonically cleaning the sample by using absolute ethyl alcohol, and finally air-drying the sample in an inert atmosphere.
As a further improvement of the above technical solution, in S4, a moving device is provided, and the sample and the plasma torch containing the reactive gas are driven by the moving device to move relatively, so that the plasma torch containing the reactive gas scans the surface of the sample.
As a further improvement of the above technical solution, the moving device is a three-axis numerical control platform.
As a further improvement of the above technical means, in S4, the sample is mounted on a ceramic backing layer.
The invention also provides a titanium dioxide nano film, which is prepared by the preparation method of the titanium dioxide nano film.
The invention has the beneficial effects that:
the preparation method of the titanium dioxide nano film comprises the steps of generating inert gas plasma by coupling inert gas, igniting the inert gas plasma to generate an inert gas plasma torch, introducing reaction gas to form the reaction gas-containing plasma torch, and acting the reaction gas-containing plasma torch on the surface of a sample to prepare the titanium dioxide nano film.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic flow chart of one embodiment of a rapid preparation method of titanium dioxide nanorods;
FIG. 2 is a schematic view of the surface structure characterization of a scanning electron microscope of the titanium dioxide nanorods prepared by the rapid preparation method of titanium dioxide nanorods according to one embodiment of the invention;
FIG. 3 is a schematic view showing the X-ray diffraction crystal structure characterization of the titanium dioxide nanorods prepared by the rapid preparation method of titanium dioxide nanorods according to an embodiment of the present invention;
FIG. 4 is a diagram illustrating an apparatus for preparing titanium dioxide nanorods using a rapid preparation method of titanium dioxide nanorods, according to an embodiment of the present invention.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be clearly and completely described in conjunction with the embodiments and the accompanying drawings to fully understand the objects, the schemes and the effects of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
It should be noted that, unless otherwise specified, when a feature is referred to as being "fixed" or "connected" to another feature, it may be directly fixed or connected to the other feature or indirectly fixed or connected to the other feature. Furthermore, the descriptions of up, down, left, right, front, rear, etc. used in the present invention are only relative to the positional relationship of the respective components of the present invention with respect to each other in the drawings.
Furthermore, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used in the description herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any combination of one or more of the associated listed items.
Referring to fig. 1, a flow chart of one embodiment of the method for rapidly preparing titanium dioxide nanorods of the invention is shown. The detailed process is as follows:
and S1, providing an inert gas, wherein the inert gas is a gas which does not react with other gases under the conventional conditions, and is preferably a rare gas, such as helium, neon, argon, krypton and xenon. Among them, in the present embodiment, argon gas is preferable.
And S2, coupling the inert gas to generate an inert gas plasma, igniting the inert gas plasma, and igniting the inert gas plasma to generate an inert gas plasma torch.
In S2, the coupling process of the inert gas may employ inductive coupling or capacitive coupling.
S3, introducing reaction gas into the plasma torch generating the inert gas to generate the plasma torch containing the reaction gas. The reaction gas may be a gas such as oxygen or nitrogen or a mixture of a plurality of gases, and in the present embodiment, oxygen is preferred.
And S4, acting the generated plasma torch containing the reaction gas on the surface of the sample (wafer), and processing the sample to form the titanium dioxide nano film under the action of the plasma torch.
In S2 and S3, the inert gas and the reactive gas are supplied in a layered manner. Specifically, a first gas layer, a second gas layer and a third gas layer are arranged, the tail ends of the first gas layer, the second gas layer and the third gas layer are communicated, the first gas layer, the second gas layer and the third gas layer are sequentially arranged from inside to outside, inert gas is introduced through the second gas layer and the third gas layer, and reaction gas is introduced through the first gas layer. The inert gases in the second gas layer and the third gas layer can be provided by the same device or different devices, so that the flow rate of the reaction gases in the first gas layer is smaller than that of the inert gases in the second gas layer, and the flow rate of the inert gases in the second gas layer is smaller than that of the inert gases in the third gas layer.
Preferably, in one embodiment, the inert gas is argon, the reactant gas is oxygen, the flow rate of oxygen in the first gas layer is 20sccm, the flow rate of argon in the second gas layer is 1.5slm, and the flow rate of argon in the third gas layer is 13 slm.
In order to process the surface of the sample, preferably, the plasma torch containing the reaction gas is uniformly scanned over the entire surface of the sample to ensure the uniformity of the processing. In one embodiment, the moving device is connected with the sample, and the sample is driven to move by the moving device, so that the sample and the plasma torch generate uniform relative motion.
In a preferred embodiment, the moving means is a three-axis numerically controlled platform. The required motion program can be written in the triaxial numerical control platform in advance, so that the triaxial numerical control platform can enable a plasma torch containing reaction gas to uniformly scan the surface of the whole sample when in work. In addition, a repeated scanning program can be set through the three-axis numerical control platform, so that the whole scanning process is completed within a set time, and then the three-axis numerical control platform repeatedly executes scanning actions to continuously process different wafers, thereby obviously improving the processing efficiency. In one embodiment, the time for one program is set to 330 seconds.
In this embodiment, the control program of the three-axis numerical control platform belongs to the existing technical means for those skilled in the art, and is not described herein again.
In one embodiment, the sample is mounted on a ceramic backing layer prior to processing the sample using a plasma torch containing a reactive gas. The ceramic cushion layer has good heat resistance, and the sample is installed on the ceramic cushion layer, so that the sample can be effectively prevented from being processed, and the material of the bottom layer of the sample is prevented from being etched during sample processing.
Preferably, when preparing the sample (wafer), i.e., before S4, the sample is polished and cleaned until the surface of the sample is smooth and clean and the smooth and clean side of the sample faces upward, then the sample is ultrasonically cleaned with absolute ethyl alcohol, and after the cleaning is completed, the sample is air-dried in an inert atmosphere.
In one embodiment, an electric field is further arranged, the electric field area covers the surface of the sample and the plasma torch containing the reaction gas, and the generated plasma moves directionally towards the surface of the sample under the action of the electric field, so that the etching efficiency of the plasma torch containing the reaction gas on the sample is improved.
Fig. 2 is a schematic view showing the surface structure characterization of the titanium dioxide nanorods prepared by the method for preparing titanium dioxide nano-films according to the present invention by using a scanning electron microscope. Referring to fig. 2, under the condition of power of 800w (power of radio frequency power supply for providing power for the inductive coupling device), a uniform and dense oxide thin film is formed on the surface of the sample, and at the power of 800w, the length of the formed nano-rod is as long as about 500nm, the diameter is not equal to 20-60 nm, and in addition, the structure of the nano-rod becomes more and more obvious with the increase of the power.
As shown in FIG. 3, a schematic diagram showing the characterization of the X-ray diffraction crystal structure of the titanium dioxide nanorods prepared by the preparation method of the titanium dioxide nano-films of the present invention is shown. As shown in FIG. 3, at this time, the power is 800w, and all the prepared titanium dioxide nanorods are rutile phase titanium dioxide, because at 800w, the temperature of the inductively coupled plasma is higher, which is favorable for the generation of rutile phase, and the preparation of the titanium dioxide nanorods is also confirmed to be successful.
Based on the principle of the titanium dioxide nano-film preparation method, the method can also be used for preparing titanium dioxide nano-films such as titanium dioxide nanowires, titanium dioxide nano-flowers, titanium dioxide nano-belts and the like. If the processing condition is low power and can prepare the titanium dioxide nano-wire and the titanium dioxide nano-belt structure for a long time, and if the processing condition is high power, the titanium dioxide nano-belt and the titanium dioxide nano-flower and other structures can be prepared according to different processing time.
Based on the preparation method of the titanium dioxide nano film, the embodiment of the invention also provides the titanium dioxide nano film, which is prepared by the preparation method of the titanium dioxide nano film.
Fig. 4 is a schematic structural diagram of an embodiment of a titanium dioxide nano-film manufacturing apparatus according to an embodiment of the present invention. Referring to fig. 4, the apparatus for preparing a titanium dioxide nano-film according to the embodiment of the present invention includes a rectangular tube 1, an inert gas supply device 2, a reaction gas supply device 3, an electric spark igniter 4, an inductive coupling device 5, a sample stage 6, and a moving device 7.
The rectangular tube 1 is internally provided with a first gas layer, a second gas layer and a third gas layer (not shown in the figure) from inside to outside in sequence, the first gas layer, the second gas layer and the third gas layer are separated in sequence, the tail ends of the first gas layer, the second gas layer and the third gas layer are communicated, an inert gas supply device 2 is communicated with the second gas layer and the third gas layer and used for supplying inert gas to the second gas layer and the third gas layer, and a reaction gas supply device 3 is communicated with the first gas layer and used for supplying reaction gas to the first gas layer.
The ignition wire 40 of the electric spark igniter 4 extends into the second gas layer or the third gas layer, and the electric spark igniter 4 works to enable the ignition wire 40 to generate sparks, so that the gas in the second gas layer or the third gas layer is ignited to generate flame; the inductive coupling device 5 comprises a radio frequency power supply 50, a matcher 51 and an inductance coil 52, wherein the inductance coil 52 is wound at the outlet end of the rectangular tube 1, the radio frequency power supply 50, the matcher 51 and the inductance coil 52 are sequentially connected, under the condition of electrifying, the inductance coil 52 generates inductance and acts on the gas in the rectangular tube 1 to generate gas plasma, in the embodiment, the inert gas in the second gas layer and the inert gas in the third gas layer are inductively coupled by the inductance coil 52 to generate the inert gas plasma, and the inert gas plasma is ignited under the action of the electric spark igniter 4 to form an inert gas plasma torch. The reaction gas is supplied to the first gas layer by the reaction gas supply device 3, and the reaction gas flows out along with the first gas layer and is mixed with the plasma of the inert gas flowing out of the second gas layer and the third gas layer to form a plasma torch containing the reaction gas.
The sample table 6 is used for containing a sample 60 to be processed, and preferably, a ceramic cushion layer 61 is arranged on the sample table 6, and the sample 60 to be processed is installed through the ceramic cushion layer 61. The moving device 7 is connected with the sample stage 6 to drive the sample stage 6 to move, so that relative motion is generated between the sample 60 and the generated plasma torch containing the reaction gas, and the relative motion is preferably used for uniformly scanning the surface of the sample by the plasma torch containing the reaction gas. In one embodiment, the moving means 7 is preferably a three-axis numerically controlled platform.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a titanium dioxide nano film is characterized by comprising the following steps:
s1, providing inert gas;
s2, providing a plasma torch of inert gas;
s3, introducing reaction gas containing oxygen into the inert gas plasma torch to generate the plasma torch containing the reaction gas;
s4, applying a plasma torch containing a reactive gas to the sample surface.
2. The method for preparing the titanium dioxide nano-film according to claim 1, wherein a first gas layer, a second gas layer and a third gas layer are sequentially arranged from inside to outside, and the ends of the first gas layer, the second gas layer and the third gas layer are communicated; and the inert gas is introduced through the second gas layer and the third gas layer, and the reaction gas is introduced through the first gas layer.
3. The method for preparing a titanium dioxide nano-film according to claim 2, wherein the gas flow rate of the second gas layer is greater than the gas flow rate of the third gas layer, and the gas flow rate of the third gas layer is greater than the gas flow rate of the first gas layer.
4. The method for preparing a titanium dioxide nano-film according to any one of claims 1 to 3, wherein in S2, the inert gas is acted by inductive coupling or capacitive coupling.
5. The method for preparing titanium dioxide nano-film according to claim 4, characterized in that an electric field is arranged above the sample, and the plasma generated by coupling moves towards the sample under the action of the electric field.
6. The method for preparing a titanium dioxide nano-film according to any one of claims 1 to 3, wherein before S4, a sample is pretreated by the following steps: firstly, polishing the surface of a sample until the surface of the sample is smooth, then ultrasonically cleaning the sample by using absolute ethyl alcohol, and finally air-drying the sample in an inert atmosphere.
7. The method of producing a titanium dioxide nanofilm according to any one of claims 1 to 3, wherein in S4, a moving device is provided, and the sample and the plasma torch containing the reactive gas are moved relatively by the moving device, so that the plasma torch containing the reactive gas scans the surface of the sample.
8. The method for preparing titanium dioxide nano-film according to claim 7, wherein the moving device is a three-axis numerical control platform.
9. The method of preparing a titanium dioxide nanofilm according to any one of claims 1 to 3, wherein in S4, the sample is mounted on a ceramic cushion layer.
10. A titanium dioxide nano-film produced by the method for producing a titanium dioxide nano-film according to any one of claims 1 to 9.
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| CN201910790001.3A CN110499497B (en) | 2019-08-26 | 2019-08-26 | Preparation method of titanium dioxide nano film and titanium dioxide nano film |
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| CN110499497B true CN110499497B (en) | 2021-09-21 |
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