CN110499497A - 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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- CN110499497A CN110499497A CN201910790001.3A CN201910790001A CN110499497A CN 110499497 A CN110499497 A CN 110499497A CN 201910790001 A CN201910790001 A CN 201910790001A CN 110499497 A CN110499497 A CN 110499497A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000002120 nanofilm Substances 0.000 title claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 96
- 239000011261 inert gas Substances 0.000 claims abstract description 42
- 239000012495 reaction gas Substances 0.000 claims abstract description 42
- 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 12
- 239000000919 ceramic Substances 0.000 claims description 7
- 230000005684 electric field Effects 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000001939 inductive effect Effects 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000002073 nanorod Substances 0.000 description 9
- 230000006872 improvement Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 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
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002127 nanobelt Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002057 nanoflower Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- -1 after mixing Substances 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000005516 engineering process 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
- 239000010408 film Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass 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
- 239000000976 ink Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 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
- 239000007788 liquid Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001617 migratory effect Effects 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
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011084 recovery Methods 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
- 239000000126 substance Substances 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000007704 wet chemistry method 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
Classifications
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Inorganic Chemistry (AREA)
- 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 present invention relates to a kind of titanium dioxide nano-film manufacture fields, more particularly, to a kind of titanium dioxide nano-film
Preparation method and titanium dioxide nano-film.
Background technique
Titanium dioxide (TiO2) it is a kind of broad stopband transparent metal oxide semiconductor, there are three types of common crystal structures:
Rutile, anatase and brockite, relatively conventional in nature is Anatase and Rutile Type, and optical band gap exists
3.0eV or more has the performances such as excellent photic Superhydrophilic, photocatalytic, anti-light corrosivity, and is closed extensively by people
Note.Nano-TiO2Material is because it is with the spies such as high chemical stability, high thermal stability, nontoxic, Superhydrophilic, non-migratory
Point, be widely used in anti-ultraviolet material, photocatalysis catalyst, glass with clean, suncream, coating, ink, packaging material for food,
The fields such as paper industry.
Up to the present, have numerous document reports and be used to prepare TiO2The various approach of nanostructure, such as colloidal sol
Gel method, anodizing, electrophoresis, chemical vapour deposition technique (CVD), magnetron sputtering method etc..Unique hole in order to obtain
Gap structure and high-specific surface area, it has been developed that the TiO of various different-shape structures2, including nano particle, nanometer rods, receive
Popped rice, nano wire, nanotube etc..Existing research surface, nanostructure can effectively improve TiO2Optical property, light urges
Change activity and optical storage performance.Especially arrange orderly TiO2Nanometer stick array possesses apparent quantum confined effect, height
The features such as degree is orderly aligned structure and high-specific surface area, can effectively improve electronicsThe interfacial separation ability and current-carrying in hole pair
The orientation transfer efficiency of son, makes it in dye-sensitized cell, photoelectrochemical cell, light (electricity) catalyzing and degrading pollutant, sensor etc.
Technical field has important application prospect.
But for existing TiO2The generally existing some drawbacks of the preparation method of nanostructure, such as: chemical vapor deposition
(CVD) etc. wet chemistries method needs to be used to prepare precursor liquid, higher cost using a large amount of metal titanium sheets；High-temperature oxydation and part are wet
High temperature or vacuum condition in forensic chemistry method for a long time is to the more demanding of equipment, it is also possible to which there are security risks；
Secondary environmental pollution is also easily caused during recovery processing to the strong acid of the acid cleaning process consumption of titanium alloy or titanium sheet, no
Conducive to its industrialization utilization.
Therefore, a kind of simple and easy to do, without secondary pollution TiO2Thin film preparation process becomes the problem of research is paid close attention to emphatically.
Summary of the invention
In order to solve the deficiencies in the prior art, the embodiment of the present invention provides a kind of titanium dioxide nano-film preparation method
The embodiment of the present invention solves the technical solution that above-mentioned technical problem is taken are as follows: it is thin to provide a kind of nano titania
Membrane preparation method includes the following steps: S1, provides inert gas；S2, the plasma flare of inert gas is provided；S3, to lazy
Property gas the inside of plasma flare be passed through reaction gas, generate the plasma flare containing reaction gas；S4, pass through
Plasma flare containing reaction gas acts on sample surfaces.
As a further improvement of the above technical scheme, first gas layer, second gas layer, are set gradually from the inside to the outside
The end of three gas blankets, the first gas layer, the second gas layer and the third gas layer three is connected；Its
In, the inert gas is passed through by the second gas layer and the third gas layer, and the reaction gas passes through described the
One gas blanket is passed through.
As a further improvement of the above technical scheme, the gas flow rate of the second gas layer is greater than the third gas
The gas flow rate of layer, the gas flow rate of the third gas layer are greater than the gas flow rate of the first gas layer.
As a further improvement of the above technical scheme, in S2, by inductive coupling or capacitive coupling to inert gas into
Row effect.
As a further improvement of the above technical scheme, electric field is set in the top of sample, the plasma for generating coupling
Body moves under the action of electric field to sample direction.
As a further improvement of the above technical scheme, before S4, sample is pre-processed, preprocessing process are as follows:
Then sample surfaces of first polishing are cleaned by ultrasonic until sample surfaces are smooth with dehydrated alcohol, finally under an inert atmosphere by sample wind
It is dry.
As a further improvement of the above technical scheme, in S4, mobile device is set, sample is driven by mobile device
Relative movement is generated with the plasma torch containing reaction gas, so that the plasma flare containing reaction gas scans sample
Surface.
As a further improvement of the above technical scheme, the mobile device is three-axis numerical control platform.
As a further improvement of the above technical scheme, in S4, sample is mounted on ceramic bed course.
The present invention also provides a kind of titanium dioxide nano-films, pass through titanium dioxide nano-film preparation side as described above
Method is made.
Beneficial effects of the present invention:
Titanium dioxide nano-film preparation method of the invention, by inert gas is coupled generate inert gas it is equal from
Daughter, the plasma of inert gas is ignited the plasma torch for generating inert gas, then accesses reaction gas, is allowed to be formed
Plasma flare containing reaction gas acts on sample surfaces by the plasma flare containing reaction gas,
Titanium dioxide nano-film is prepared, whole preparation process is simple, easy, without secondary pollution.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the flow diagram of titanium dioxide nano-rod fast preparation method one embodiment of the present invention；
Fig. 2 receives for titanium dioxide made from the titanium dioxide nano-rod fast preparation method of one embodiment through the invention
The schematic diagram of the scanning electron microscope surface texture characterization of rice stick；
Fig. 3 receives for titanium dioxide made from the titanium dioxide nano-rod fast preparation method of one embodiment through the invention
The schematic diagram of the X ray diffractive crystal structural characterization of rice stick；
Fig. 4 is to prepare nano titania using titanium dioxide nano-rod fast preparation method in one embodiment of the invention
The device of stick.
Specific embodiment
It is carried out below with reference to technical effect of the embodiment and attached drawing to design of the invention, specific structure and generation clear
Chu, complete description, to be completely understood by the purpose of the present invention, scheme and effect.It should be noted that the case where not conflicting
Under, the features in the embodiments and the embodiments of the present application can be combined with each other.
It should be noted that unless otherwise specified, when a certain feature referred to as " fixation ", " connection " are in another feature,
It can directly fix, be connected to another feature, and can also fix, be connected to another feature indirectly.In addition, this
The descriptions such as up, down, left, right, before and after used in invention are only relative to the mutual of each component part of the invention in attached drawing
For positional relationship.
In addition, unless otherwise defined, the technology of all technical and scientific terms used herein and the art
The normally understood meaning of personnel is identical.Term used in the description is intended merely to description specific embodiment herein, without
It is to limit the present invention.Term " and or " used herein includes the arbitrary of one or more relevant listed items
Combination.
Such as Fig. 1, the flow diagram of titanium dioxide nano-rod fast preparation method one embodiment of the invention is shown.
Its detailed process is as follows:
S1, inert gas is provided, inert gas is the gas not reacted with other gases under normal condition, preferably
Rare gas, such as helium, neon, argon gas, Krypton, xenon.Wherein, in the present embodiment, preferably argon gas.
S2, coupling generation inert gas plasma is carried out to inert gas, meanwhile, it lights a fire, makes the inertia generated
Gaseous plasma is ignited, and generates the plasma flare of inert gas, during being somebody's turn to do, persistently provides inert gas, is guaranteed
The flow speed stability of inert gas, so as to generate the plasma flare of stable inert gas.
In S2, the coupling process of inert gas can use inductive coupling or capacitive coupling.
S3, it is passed through reaction gas to the inside for the plasma flare for generating inert gas, is allowed to generate and contains reaction gas
The plasma flare of body.Wherein, reaction gas can be the mixed gas of the gases such as oxygen, nitrogen or multiple gases, this
In embodiment, preferably oxygen.
S4, sample (wafer) surface is acted on using the plasma flare containing reaction gas of generation, is being waited
Under the action of gas ions torch, sample is processed to form titanium dioxide nano-film.
In S2 and S3, inert gas and reaction gas are provided by way of layering.Specifically, setting first gas
Layer, second gas layer and third gas layer, first gas layer, second gas layer, third gas layer three end be connected, and
First gas layer, second gas layer and third gas layer are set gradually from the inside to the outside, wherein pass through second gas layer, third gas
Body layer is passed through inert gas, is passed through reaction gas by first gas layer.Wherein, second gas layer with it is lazy in third gas layer
Property gas can be provided by the same device, can also be provided by different devices, generally, guarantee first gas layer in
Reaction gas flow velocity be less than second gas layer inert gas flow velocity, the flow velocity of the inert gas in second gas layer is small
In the flow velocity of the inert gas in third gas layer.
Preferably, in one embodiment, inert gas is argon gas, and reaction gas is oxygen, oxygen in first gas layer
Flow velocity be 20sccm, the flow velocity of argon gas is 1.5slm in second gas layer, and the flow velocity of argon gas is 13slm in third gas layer.
When processing to sample surfaces, the plasma flare containing reaction gas is preferably made equably to scan sample
Whole surface for this purpose, in one embodiment, mobile device is set, in the band of mobile device to guarantee the uniformity of processing
Under dynamic, sample is made to generate uniform relative motion with the plasma flare containing reaction gas.In one embodiment, mobile
Device is connected with sample, and it is mobile to drive sample by mobile device, so that sample be made to generate uniform phase with plasma flare
To movement, in another embodiment, the generation of mobile device Yu the plasma flare containing reaction gas also can be set
Device is connected, and drives the generation device of the plasma flare containing reaction gas mobile by mobile device, to make sample
Uniform relative motion is generated with plasma flare.
In a preferred embodiment, mobile device is three-axis numerical control platform.It can shift to an earlier date in three-axis numerical control platform
Motor program needed for write-in, enabling three-axis numerical control platform at work keeps the plasma flare containing reaction gas uniform
Scan the surface of entire sample in ground.In addition, the program of multiple scanning can be set by three-axis numerical control platform, make entire scanned
It is completed in the time that journey is set at one, then three-axis numerical control platform repeats scanning motion, continuously to different wafers
It is processed, the efficiency of processing can be improved significantly in this way.In one embodiment, the time of a program is set as 330
Second.
In the present embodiment, the control program of three-axis numerical control platform belongs to existing skill to those skilled in the art
Art means, just repeat no more here.
In one embodiment, before being processed using the plasma flare containing reaction gas to sample, by sample
Product are mounted on ceramic bed course.Ceramic bed course has good heat resistance, and sample is mounted on ceramic bed course, can be effective
When preventing sample from processing, the material of sample bottom is etched when sample being avoided to process.
Preferably, when preparing sample (wafer), i.e., before S4, sample is first subjected to polishing cleaning, until sample
Surface smooth pieces, and make the one of sample smooth pieces to face upward, then sample is cleaned by ultrasonic with dehydrated alcohol, clear
Sample is carried out under an inert atmosphere after the completion of washing air-dried.
In one embodiment, be additionally provided with electric field, electric field region cover sample surfaces with containing reaction gas it is equal from
Daughter torch, the plasma of generation is under the action of electric field, the movement oriented to sample surfaces, thus improve containing
Etching efficiency of the plasma flare of reaction gas to sample.
Such as Fig. 2, shows and utilize titanium dioxide nano-rod made from titanium dioxide nano-film preparation method of the invention
Scanning electron microscope surface texture characterization schematic diagram.Such as Fig. 2, (filled under conditions of power is 800w for inductive coupling
Set and the power of the radio-frequency power supply of power supply be provided), sample surfaces form the sull of even compact, when power is 800w,
The length of the nanometer rods of formation is up to 500nm or so, diameter 20 to 60nm etc., in addition, with the increase of power, nanometer rods
Structure can be more and more obvious.
Such as Fig. 3, shows and utilize titanium dioxide nano-rod made from titanium dioxide nano-film preparation method of the invention
X ray diffractive crystal structural characterization schematic diagram.Such as Fig. 3, power is 800w at this time, and the titanium dioxide nano-rod of preparation is
Rutile phase titanium dioxide is conducive to the life of Rutile Type this is because inductively coupled plasma temperature is higher under 800w
At also demonstrating that the preparation of titanium dioxide nano-rod is successful.
Based on the principle of titanium dioxide nano-film preparation method of the invention, can be also used for titanium dioxide nano thread,
The preparation of the titanium dioxide nano-films such as titanium oxide nanoflower, titanium dioxide nano-belts.When as long for low-power such as processing conditions
Between when can prepare titanium dioxide nano thread and titanium dioxide nano-belts structure, and when processing conditions is high power, when according to processing
Between difference, the structures such as titanium dioxide nano-belts and titanium oxide nanoflower can be prepared.
Based on above-mentioned titanium dioxide nano-film preparation method, it is thin that the embodiment of the present invention also provides a kind of nano titania
Film is made by titanium dioxide nano-film preparation method as described above.
Such as Fig. 4, the knot of titanium dioxide nano-film preparation facilities one embodiment of one embodiment of the invention is shown
Structure schematic diagram.Such as Fig. 4, the titanium dioxide nano-film preparation facilities of the embodiment of the present invention includes quarter bend 1, inert gas offer dress
It sets 2, reaction gas and device 3, electric spark fire maker 4, inductance coupling device 5, sample stage 6, mobile device 7 is provided.
First gas layer, second gas layer, third gas layer are disposed in quarter bend 1 from the inside to the outside (not show in figure
Out), first gas layer, second gas layer, third gas layer successively separate, and the end of three is connected, and inert gas provides
Device 2 is connected to second gas layer, third gas layer, for providing inert gas, reaction to second gas layer, third gas layer
Gas provides device 3 and is connected to first gas layer, for providing reaction gas to first gas layer.
The ignition lead 40 of electric spark fire maker 4 protrudes into second gas layer or third gas layer, 4 work of electric spark fire maker
Make, ignition lead 40 is made to generate spark, so that the gas ignition in second gas layer or third gas layer is generated flame；Inductance
Coupling device 5 includes radio-frequency power supply 50, adaptation 51 and inductance coil 52, and inductance coil 52 is set around the outlet end of quarter bend 1,
Radio-frequency power supply 50, adaptation 51 and inductance coil 52 are sequentially connected, and in the case where energization, inductance coil 52 generates inductance, and
To the gas effect in quarter bend 1, the plasma of gas is generated, in the present embodiment, in second gas layer and third gas layer
The inductive coupling that inert gas is generated by inductance coil 52 generates the plasma of inert gas, and in electric spark fire maker 4
Under effect, the plasma of inert gas is ignited, and forms the plasma flare of inert gas.Dress is provided by reaction gas
Set 3 and provide reaction gas to first gas layer, reaction gas goes out with first gas laminar flow, and with second gas layer and third
The plasma mixing of the inert gas of gas blanket outflow, forms the plasma flare containing reaction gas, after mixing, reaction
Gas is located at the inside of the torch formed.
Sample stage 6 is used to hold the sample 60 for needing to process, it is preferred that is equipped with ceramic bed course 61 on sample stage 6, passes through
The sample 60 that the ceramic installation of bed course 61 needs to process.Mobile device 7 is connect with sample stage 6, to drive sample stage 6 to generate movement,
And then make to generate relative motion between sample 60 and the plasma flare containing reaction gas generated, the relative motion is preferred
The surface of sample is equably scanned for the plasma flare containing reaction gas.In one embodiment, mobile device 7 is preferred
For three-axis numerical control platform.
It is to be illustrated to what preferable implementation of the invention carried out, but the invention is not limited to the implementation above
Example, those skilled in the art can also make various equivalent variations on the premise of without prejudice to spirit of the invention or replace
It changes, these equivalent deformations or replacement are all included in the scope defined by the claims of the present application.
Claims (10)
1. a kind of titanium dioxide nano-film preparation method, which comprises the steps of:
S1, inert gas is provided；
S2, the plasma flare of inert gas is provided；
S3, it is passed through reaction gas to the inside of the plasma flare of inert gas, generates the plasma containing reaction gas
Torch；
S4, sample surfaces are acted on by the plasma flare containing reaction gas.
2. titanium dioxide nano-film preparation method according to claim 1, which is characterized in that set gradually from the inside to the outside
First gas layer, second gas layer, third gas layer, the first gas layer, the second gas layer and the third gas
The end of body layer three is connected；Wherein, the inert gas is passed through by the second gas layer and the third gas layer,
The reaction gas is passed through by the first gas layer.
3. titanium dioxide nano-film preparation method according to claim 2, which is characterized in that the second gas layer
Gas flow rate 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 first gas
The gas flow rate of layer.
4. titanium dioxide nano-film preparation method according to any one of claim 1 to 3, which is characterized in that in S2,
Inert gas is acted on by inductive coupling or capacitive coupling.
5. titanium dioxide nano-film preparation method according to claim 4, which is characterized in that be arranged in the top of sample
Electric field, the plasma for generating coupling move under the action of electric field to sample direction.
6. titanium dioxide nano-film preparation method according to any one of claim 1 to 3, which is characterized in that in S4
Before, sample is pre-processed, preprocessing process are as follows: sample surfaces of first polishing, until sample surfaces are smooth, then with anhydrous second
Alcohol ultrasonic cleaning, finally under an inert atmosphere air-dries sample.
7. titanium dioxide nano-film preparation method according to any one of claim 1 to 3, which is characterized in that in S4
In, mobile device is set, drives sample to generate relative movement with the plasma torch containing reaction gas by mobile device, with
The plasma flare containing reaction gas is set to scan the surface of sample.
8. titanium dioxide nano-film preparation method according to claim 7, which is characterized in that the mobile device is three
Shaft and NC Machining Test platform.
9. titanium dioxide nano-film preparation method according to any one of claim 1 to 3, which is characterized in that in S4,
Sample is mounted on ceramic bed course.
10. a kind of titanium dioxide nano-film, which is characterized in that pass through titanium dioxide as claimed in any one of claims 1-9 wherein
Titanium nano thin-film preparation method is made.
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