CN109457227A - A kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode - Google Patents
A kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 19
- 230000008569 process Effects 0.000 title claims description 15
- 238000007254 oxidation reaction Methods 0.000 title claims description 10
- 239000000758 substrate Substances 0.000 claims abstract description 61
- 238000004544 sputter deposition Methods 0.000 claims abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010936 titanium Substances 0.000 claims description 53
- 229910052719 titanium Inorganic materials 0.000 claims description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 29
- 238000000137 annealing Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 43
- 238000000151 deposition Methods 0.000 abstract description 11
- 230000008021 deposition Effects 0.000 abstract description 8
- 239000010409 thin film Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 230000033001 locomotion Effects 0.000 description 6
- 230000005684 electric field Effects 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
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- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000013077 target material Substances 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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Abstract
本发明公开了一种直流磁控溅射法制备光电催化氧化钛电极的方法，该直流磁控溅射法制备光电催化氧化钛电极的方法采用直流磁控溅射方法制备了氧化钛薄膜电极，把磁控原理与溅射相结合，既保持了溅射的优点，又克服了溅射的缺点，具有其独特的优越性；还可以大大降低基片温度，提高了沉积率，溅射速率高，也解决了薄膜被污染的问题。
The invention discloses a method for preparing a photoelectric catalytic titanium oxide electrode by a direct current magnetron sputtering method. The direct current magnetron sputtering method for preparing a photoelectric catalytic titanium oxide electrode adopts a direct current magnetron sputtering method to prepare a titanium oxide thin film electrode. The combination of magnetron principle and sputtering not only maintains the advantages of sputtering, but also overcomes the shortcomings of sputtering, and has its unique advantages; it can also greatly reduce the temperature of the substrate, improve the deposition rate, and have a high sputtering rate. , also solves the problem of film contamination.
Description
Technical field
The present invention relates to the technical fields of thin film of titanium oxide electrode process more particularly to a kind of direct current magnetron sputtering process to prepare
The method of photoelectrocatalysioxidization oxidization Ti electrode.
Background technique
Magnetron sputtering method is novel, low-temperature and high-speed the sputtering film coating method of one kind of initial stage seventies invention, belongs to and splashes
Penetrate one kind of method.The film of such method preparation has many advantages, such as high quality, high density, good associativity and intensity.It is filled
It sets performance to stablize, is convenient for operation, technique is easy to control, and production is reproducible, is suitable for deposited of large area, and convenient for continuously and partly
Continuous production.
Sputtering method be thin film physical vapor deposition (PVD) a kind of method, be associated with chemical vapor deposition (CVD) and
Completely different a kind of film deposition techniques.It has certain kinetic energy after accelerating in the electric field using the ion with charge
Ion is guided into the target electrode to be sputtered by feature.In the suitable situation of ion energy, incident ion will with target surface
Atom collision process in sputter out the latter.These atoms being sputtered will have certain kinetic energy, and can be along
Certain direction directive substrate, to realize the deposition of film on substrate.
And have the drawback that (1) deposition velocity is lower using the film of sputter deposition preparation in the prior art；
(2) operating air pressure needed for is higher.In this way will be so that substrate receive high energy electron bombardment, temperature rise is very high, and film layer subject to damage,
A possibility that gas molecule generates pollution to film is improved.
Summary of the invention
The purpose of the invention is to overcome the above-mentioned prior art, a kind of direct current magnetron sputtering process is provided and prepares light
The method of electrocatalytic oxidation Ti electrode, the direct current magnetron sputtering process prepare the method for photoelectrocatalysioxidization oxidization Ti electrode using DC magnetic
The advantages of control sputtering method is prepared for thin film of titanium oxide electrode, magnetic control principle is combined with sputtering, not only maintained sputtering, but also gram
The shortcomings that having taken sputtering has its unique superiority；Substrate temperature can also be substantially reduced, deposition, sputtering speed are improved
Rate is high, also solves the problems, such as that film is contaminated.
The technical solution adopted by the present invention to solve the technical problems is: a kind of direct current magnetron sputtering process prepares photoelectrocatalysis
The method of Titanium oxide electrode, includes the following steps:
(1) substrate cleans: using titanium net as substrate, titanium net titanium net is cut into size 7.5cm × 2.8cm, is polished with sand paper,
Distilled water flushing is used after polishing, is then made ultrasonic cleaning 20min with acetone again, is then respectively cleaned with ethyl alcohol, distilled water
The titanium net substrate cleaned finally is dried up, is placed on spare in clean environment by 20min；
(2) forvacuum: titanium net substrate is put into vacuum chamber, and baffle is rotated to the underface of Ti target to cover Ti
Target, in order to avoid be splashed on titanium net substrate when pre-sputtering and generate impurity, by vacuum chamber to 2.0 × 10-4The base vacuum of Pa
Pressure；
(3) pre-sputtering: being controlled by gas flow and counted, Ar gas is passed through in vacuum chamber, is started shielding power supply, is stepped up
Sputtering voltage slowly increases sputtering voltage to starting glow discharge occur later；The pre-sputtering time 20~30 minutes, until Ti target
The color of surface glow discharge is changed into blue and white by pink, terminates pre-sputtering work；Or discharge voltage quickly falls to certain
When one stationary value, show that oxide has removed, during pre-sputtering, cannot quickly increase voltage, will affect instrument in this way
Service life.
(4) sputtered film: using Ar as working gas and O2It for reaction gas, each leads into vacuum chamber, by titanium net base
Mounted in that can have molybdenum filament on the substrate holder of center axis rotation, in substrate holder to silicon, titanium net substrate temperature is controlled 280 piece
DEG C, Ti target to titanium net substrate distance is 8.0cm, sputtering power 100W, sputtering time 60min；Direct current is successively closed later to splash
Radio source, gas control valve, molecular pump, mechanical pump and general supply turn off recirculated water in 15 minutes after closing general supply, to vacuum
The taking-up when temperature of room is down to room temperature；
(5) it makes annealing treatment: being put into Muffle furnace and heat 1 hour in 200 DEG C of constant temperature respectively and in 500 DEG C of constant temperature after sputtering
Middle heating 1 hour, after annealing, is placed 9 hours in Muffle furnace, is allowed after its natural cooling and is taken out, obtains Titanium oxide electrode.
Annealing, structure and optics, electricity, catalytic property to film etc. all have a significant impact, in order to guarantee annealing thoroughly, two
The kind heated at constant temperature time is 1 hour.
The surface state of substrate has a great impact to adhesive force.Why film can be attached on substrate, be Fan Dewa
The comprehensive function of Er Sili, diffusion attachment, mechanical sealed, electrostatic attraction, chemical bond force etc..Substrate surface it is unclean will make it is thin
Film cannot directly be contacted with substrate, and Van der Waals for weakens significantly, and diffusion attachment is also impossible to, and adhesion property can be made very poor.
So to carry out stringent cleaning to substrate to remove the grit adhered to, the oil film adsorbed, moisture film etc. as previous in plated film
Pollutant.
Substrate temperature has important influence to the formation of film, improves the phase that substrate temperature is conducive to film and substrate atom
Counterdiffusion, and can accelerate to chemically react, to advantageously form diffusion attachment and chemical bond adhesive force, increase adhesion.
Membrane structure, the growth of product body and optical property of film etc., forming core and life of the substrate temperature to film in interface are influenced simultaneously
Length has a significant impact.When low temperature depositing, atom active is low, and Enhancing Nucleation Density is low, and there are holes at interface；When high temperature deposition, atom is living
Property increase, Enhancing Nucleation Density is high, and interface hole is few, and interface cohesion is stronger, and adhesive force is high.But substrate temperature is excessively high to make film product grain
It is coarse, increase thermal stress in film, to influence other performances of film.Therefore, titanium net substrate temperature of the invention is 280 DEG C.
Further, the purity of the Ti target is 99.99%.
In conclusion direct current magnetron sputtering process of the invention prepares the method for photoelectrocatalysioxidization oxidization Ti electrode using DC magnetic
The advantages of control sputtering method is prepared for thin film of titanium oxide electrode, magnetic control principle is combined with sputtering, not only maintained sputtering, but also gram
The shortcomings that having taken sputtering has its unique superiority；Substrate temperature can also be substantially reduced, deposition, sputtering speed are improved
Rate is high, also solves the problems, such as that film is contaminated.
Detailed description of the invention
Fig. 1 is direct current magnetron sputtering process in different annealing temperature preparation TiO2The XRD spectrum of film；
Fig. 2 is the trajectory of electron motion state diagram in crossed electric and magnetic field.
Specific embodiment
Embodiment 1
A kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode described in the present embodiment 1, including
Following steps:
(1) substrate cleans: using titanium net as substrate, titanium net titanium net is cut into size 7.5cm × 2.8cm, is polished with sand paper,
Distilled water flushing is used after polishing, is then made ultrasonic cleaning 20min with acetone again, is then respectively cleaned with ethyl alcohol, distilled water
The titanium net substrate cleaned finally is dried up, is placed on spare in clean environment by 20min；
(2) forvacuum: titanium net substrate is put into vacuum chamber, and baffle is rotated to the underface of Ti target to cover Ti
Target, in order to avoid be splashed on titanium net substrate when pre-sputtering and generate impurity, by vacuum chamber to 2.0 × 10-4The base vacuum of Pa
Pressure；
(3) pre-sputtering: being controlled by gas flow and counted, Ar gas is passed through in vacuum chamber, is started shielding power supply, is stepped up
Sputtering voltage slowly increases sputtering voltage to starting glow discharge occur later；The pre-sputtering time 20~30 minutes, until Ti target
The color of surface glow discharge is changed into blue and white by pink, terminates pre-sputtering work；Or discharge voltage quickly falls to certain
When one stationary value, show that oxide has removed, during pre-sputtering, cannot quickly increase voltage, will affect instrument in this way
Service life.
(4) sputtered film: using Ar as working gas and O2It for reaction gas, each leads into vacuum chamber, by titanium net base
Mounted in that can have molybdenum filament on the substrate holder of center axis rotation, in substrate holder to silicon, titanium net substrate temperature is controlled 280 piece
DEG C, Ti target to titanium net substrate distance is 8.0cm, sputtering power 100W, sputtering time 60min；Direct current is successively closed later to splash
Radio source, gas control valve, molecular pump, mechanical pump and general supply turn off recirculated water in 15 minutes after closing general supply, to vacuum
The taking-up when temperature of room is down to room temperature；
(5) it makes annealing treatment: being put into Muffle furnace and heat 1 hour in 200 DEG C of constant temperature respectively and in 500 DEG C of constant temperature after sputtering
Middle heating 1 hour, after annealing, is placed 9 hours in Muffle furnace, is allowed after its natural cooling and is taken out, obtains Titanium oxide electrode.
Annealing, structure and optics, electricity, catalytic property to film etc. all have a significant impact, in order to guarantee annealing thoroughly, two
The kind heated at constant temperature time is 1 hour.
The surface state of substrate has a great impact to adhesive force.Why film can be attached on substrate, be Fan Dewa
The comprehensive function of Er Sili, diffusion attachment, mechanical sealed, electrostatic attraction, chemical bond force etc..Substrate surface it is unclean will make it is thin
Film cannot directly be contacted with substrate, and Van der Waals for weakens significantly, and diffusion attachment is also impossible to, and adhesion property can be made very poor.
So to carry out stringent cleaning to substrate to remove the grit adhered to, the oil film adsorbed, moisture film etc. as previous in plated film
Pollutant.
Substrate temperature has important influence to the formation of film, improves the phase that substrate temperature is conducive to film and substrate atom
Counterdiffusion, and can accelerate to chemically react, to advantageously form diffusion attachment and chemical bond adhesive force, increase adhesion.
Membrane structure, the growth of product body and optical property of film etc., forming core and life of the substrate temperature to film in interface are influenced simultaneously
Length has a significant impact.When low temperature depositing, atom active is low, and Enhancing Nucleation Density is low, and there are holes at interface；When high temperature deposition, atom is living
Property increase, Enhancing Nucleation Density is high, and interface hole is few, and interface cohesion is stronger, and adhesive force is high.But substrate temperature is excessively high to make film product grain
It is coarse, increase thermal stress in film, to influence other performances of film.Therefore, titanium net substrate temperature of the invention is 280 DEG C.
In the present embodiment, the purity of the Ti target is 99.99%.
It will be seen from figure 1 that the TiO after 500 DEG C of cycle annealings2Film is the position 25.3o in 2 θ, have one it is clear and
The diffraction maximum in sharp Detitanium-ore-type (110) face.In addition, also being detected other than (101) face diffraction maximum for detecting anatase
To (112) face, (200) face, (215) region feature diffraction maximum of anatase.This illustrates that film has obtained relatively good crystallization, crystallization
Process is than more complete, and film crystallization is in (101) Solute Content in Grain.
Ti0 after 200 DEG C of cycle annealings2Film is to have one very weak to belong to anatase at 25.3o in 2 θ
(101) diffraction maximum in face.Illustrate under conditions of 200 DEG C of cycle annealings still also have and be orientated the sharp of mixed and disorderly crystallite a little
Titanium ore crystal grain.
TiO after 200 DEG C and 500 DEG C of cycle annealings2The crystallite dimension of film is by Scherrer formula d=k λ (β cos θ)
Calculating is about 22nm.
It is known that the electronics that speed is v will be by Lorentz force in the magnetic field that electric field E and magnetic induction intensity are B
Effect:
F=-q (E+v × B)
Wherein q is electron charge.When electric field and magnetic field exist simultaneously, if E, v, B three are parallel to each other, electronics
Track be still straight line.
It is found that being in the electric field E electronics orthogonal with magnetic field B, the equation of motion is from physics:
In formula, e and m are the electricity and quality of electronics respectively, and the motion profile of electronics is as shown in Figure 2.
The characteristics of magnetron sputtering is to be mutually perpendicular to electric and magnetic fields direction above target material surface.It is above-mentioned by solving
Equation, the motion profile of above-mentioned electronics can be found out are as follows:
Wherein, x, y are respectively the coordinate for being parallel and perpendicular to target surface.The angular frequency of rotary electronic movement is ω=qB/m,
It is proportional to the charge-mass ratio q/m of magnetic induction density B and electronics.Above formula shows under the action of the magnetic field parallel with target surface,
Electronics is in the form of taking turns cycloid along target surface to the direction advance perpendicular to E, B plane.Electron motion is bound in certain sky
In, to greatly reduce the recombination loss of electronics on the wall.Such crossed electric and magnetic field can be effectively by electronics
Travel control near target surface, and extend the travel of electronics significantly, increase the ionization probability of electronics, because
And plasma density is increased, it improves with causing the magnetron sputtering rate order of magnitude.It is lost since electronics is every by primary collision
Part energy loses energy and enters as " final electronics " from the farther away weak electric field area of cathode target after multiple impacts,
It has been the low-energy electron of energy consumption totally when finally reaching anode, also just substrate can have not been made to heat again, therefore can be significantly
Reduce substrate temperature.High-density plasma is strapped near target surface by magnetic field simultaneously, and is not contacted with substrate, and ionization in this way produces
Raw cation can highly desirable bombard target surface, and substrate can be from the bombardment of plasma, thus substrate temperature again may be used
It reduces.Further, since operating air pressure is reduced to several pas of zero point, reduce the collision to the atom or molecule that sputter out, therefore
Deposition is improved, the contaminated tendency of film is also reduced.Sputtering voltage is lower, about several hundred volts, but target current density
It can achieve tens milliamperes every square centimeter.It is increased in this way, magnetron sputtering just efficiently solves substrate temperature in cathodic sputtering,
The problems such as sputter rate is low, and film is contaminated.
The above described is only a preferred embodiment of the present invention, not making any form to technical solution of the present invention
On limitation.According to the technical essence of the invention any simple modification to the above embodiments, equivalent variations and repair
Decorations, in the range of still falling within technical solution of the present invention.
Claims (3)
1. a kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode, which comprises the steps of:
(1) substrate cleans: using titanium net as substrate, titanium net titanium net being cut into size 7.5cm × 2.8cm, is polished with sand paper, polished
Distilled water flushing is used later, is then made ultrasonic cleaning 20min with acetone again, is then respectively cleaned 20min with ethyl alcohol, distilled water,
Finally the titanium net substrate cleaned is dried up, is placed on spare in clean environment；
(2) forvacuum: titanium net substrate is put into vacuum chamber, and baffle is rotated to the underface of Ti target to cover Ti target, is incited somebody to action
Vacuum chamber is to 2.0 × 10-4The base vacuum pressure of Pa；
(3) pre-sputtering: being controlled by gas flow and counted, Ar gas is passed through in vacuum chamber, is started shielding power supply, is stepped up sputtering
Voltage slowly increases sputtering voltage to starting glow discharge occur later；The pre-sputtering time 20~30 minutes, until Ti target surface
The color of glow discharge is changed into blue and white by pink, terminates pre-sputtering work；
(4) sputtered film: using Ar as working gas and O2It for reaction gas, each leads into vacuum chamber, titanium net substrate is mounted in
There can be molybdenum filament on the substrate holder of center axis rotation, in substrate holder to silicon, the control of titanium net substrate temperature is at 280 DEG C, Ti
Target to titanium net substrate distance be 8.0cm, sputtering power 100W, sputtering time 60min；D.c. sputtering electricity is successively closed later
Source, gas control valve, molecular pump, mechanical pump and general supply turn off recirculated water in 15 minutes after closing general supply, to vacuum chamber
Taking-up when temperature is down to room temperature；
(5) it makes annealing treatment: being put into after sputtering in Muffle furnace and heat 1 hour in 200 DEG C of constant temperature and add in 500 DEG C of constant temperature respectively
Heat 1 hour, after annealing, is placed 9 hours in Muffle furnace, is allowed after its natural cooling and is taken out, obtains Titanium oxide electrode.
2. the method that a kind of direct current magnetron sputtering process according to claim 1 prepares photoelectrocatalysioxidization oxidization Ti electrode, special
Sign is that the purity of the Ti target is 99.99%.
3. the method that a kind of direct current magnetron sputtering process according to claim 2 prepares photoelectrocatalysioxidization oxidization Ti electrode, special
Sign is that the crystal grain of obtained Titanium oxide electrode is 22nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811535506.7A CN109457227A (en) | 2018-12-14 | 2018-12-14 | A kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode |
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| CN201811535506.7A CN109457227A (en) | 2018-12-14 | 2018-12-14 | A kind of method that direct current magnetron sputtering process prepares photoelectrocatalysioxidization oxidization Ti electrode |
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