CN105671485A - CeO2-x nano film based on flexible metal base band and preparation method of CeO2-x nano film based on flexible metal base band - Google Patents
CeO2-x nano film based on flexible metal base band and preparation method of CeO2-x nano film based on flexible metal base band Download PDFInfo
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- CN105671485A CN105671485A CN201610053749.1A CN201610053749A CN105671485A CN 105671485 A CN105671485 A CN 105671485A CN 201610053749 A CN201610053749 A CN 201610053749A CN 105671485 A CN105671485 A CN 105671485A
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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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
Abstract
The invention relates to the technical field of preparation of cerium oxide nano films and discloses a CeO2-x nano film based on a flexible metal base band and a preparation method of the CeO2-x nano film based on the flexible metal base band. The CeO2-x nano film based on the flexible metal base band is in various shapes and orientations. The structure of the CeO2-x nano film is composed of nano particles arranged in an array shape. The invention further relates to the preparation method of the CeO2-x nano film based on the flexible metal base band. The thickness of the CeO2-x nano film is precisely controlled, and a multi-layer composite nano structure can be prepared. The CeO2-x nano film has metal flexibility characteristics and can meet various application requirements. The preparation method is simple and convenient, industrial production can be achieved easily, relevant parameters can be controlled more easily compared with a traditional chemical method, and the production cost can be greatly reduced.
Description
Technical field
The invention belongs to cerium oxide nano technical field of film preparation, it is specifically related to a kind of CeO based on flexible metal base band2-xNano thin-film and its preparation method.
Background technology
Cerium oxide is a kind of typical rare earth oxide, and its crystal has cubic fluorite structure, and has Ce3+/Ce4+Two kinds of chemical combination states, it is possible to carry out Ce3++ e, Ce4+Oxidation reduction cycle. Therefore, take cerium dioxide as nanostructure prepared by material, both there is the advantage of the small-size effect of nano material, surface effects, macro quanta tunnel effect and quantum size effect, there is again the feature that rare earth nano material redox ability is strong and ligancy is changeable, can extensively for catalytic material, the fields such as luminescent material, uv-absorbing agent and fuel cell, have wide market outlook. In the face of various different demand, it is possible to adopt different preparation methods to prepare and there is cerium dioxide of different nature. At present, conventional in prior art preparation method has chemical precipitation method, hydrothermal method, solvent thermal, microemulsion method and sol-gel method, water-oil interface method and PVD method etc.
It is found by the applicant that, the method related in prior art also also exists many deficiencies, such as all more difficult control in aspect such as repeatability of the dispersion of the controllability of film thickness, the controllability of nanostructured morphologies and homogeneity, nano particle and sticking power, preparation process, and suitability for industrialized production ability is poor. Although the research synthesizing result in controlled oxidization cerium morphology control has certain progress, but also it is difficult to solve in prior art the many deficiencies existed.
Summary of the invention
The applicant of the present invention is through a large amount of experiments and further investigation, it is proposed that a kind of CeO based on flexible metal base band newly2-xNano thin-film and its preparation method, specifically induced growth has the CeO of nanostructure on the metallic substrate2-xCoating. The method of the present invention utilizes pulsed laser deposition (being later called for short PLD) or magnetron sputtering deposition (being later called for short MSD) to be prepared, and is very beneficial for carrying out industrialization production, CeO prepared by the present invention2-xNano thin-film size evenly, strong adhesion, shape looks and orientation controlled.
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of CeO based on flexible metal base band2-xNano thin-film and its preparation method.The CeO that the present invention relates to2-xNano film thickness accurately controls, and can prepare MULTILAYER COMPOSITE nanostructure; The present invention relates to CeO2-xNano thin-film has metal flexible feature, can meet multiple application demand; The method preparation of the present invention is easy, is easy to realize industrialization and produces, and correlation parameter is more prone to control relative to traditional chemical process, and production cost can reduce greatly.
The present invention is realized by following technical scheme,
First aspect, the present invention relates to a kind of CeO based on flexible metal base band2-xNano thin-film, described CeO2-xNano thin-film is different morphologies and orientation, described CeO2-xThe structure of nano thin-film is the nano particle of array-like arrangement.
Preferably, described CeO2-xNano thin-film comprises metal base, texture layer, CeO2-xFunctional layer.
Preferably, the shape of described nano particle is bar-shaped, sheet, the cluster shape of multiple nanometer sheet composition, starlike, or polygonized structure.
Preferably, described CeO2-xBeing oriented to (001) of nano thin-film, (110), the combination of (111) or aforementioned orientation.
As preferably, described texture layer is multilevel oxide film. Described texture layer is Al2O3/Y2O3/MgO. When the shape of described nano particle is bar-shaped, the diameter of described nanometer rod is 10nm-100nm, and length-to-diameter ratio is (1-10): 1. When the shape of described nano particle is sheet, the thickness of described nanometer sheet is 10-100nm.
Second aspect, the present invention also relates to a kind of aforementioned CeO based on flexible metal base band2-xThe preparation method of nano thin-film, comprises the steps:
Step 1, gets metal base band and is installed on transmission mechanism, get CeO2-xTarget material is also installed to target platform, is vacuumized by filming equipment afterwards; On wherein said metal base band, growth has certain orientation texture layer;
Step 2, the temperature in adjustment plated film district is to growth temperature; Adopt pulse laser deposition or magnetron sputtering deposition method; Lead to afterwards into oxygen; Coating system transport unit drives metal base band so that metal base band, by plated film district, namely forms CeO on the surface of the texture layer of metal base band2-xFunctional layer.
Preferably, in step 1, described CeO2-xTarget material is 5-25cm to the distance in plated film district.
Preferably, in step 2, described growth temperature is 450～650 DEG C.
Preferably, in step 2, described CeO2-xThe thickness of functional layer is 10～2000nm.
Preferably, in step 2, before leading to oxygen, plated film district vacuum state; After leading to oxygen, plated film district air pressure is 5～200mTorr.
Further preferably, described vacuum state air pressure is 1 × 10-4～1 × 10-7Torr。
Preferably, in step 2, described employing pulse laser deposition is specially, and regulates laser energy and the frequency of PLD, and described laser energy and frequency are specially: E=50～300mJ, f=10～200Hz.
Preferably, described metal base band is one or many by the number of times in plated film district, is specially: with the speed of 1～10m/h once by plated film district, or with the speed of 5～50m/h by hyperchannel plated film district.
Preferably, described magnetron sputtering deposition method is specially, and is wound around by the metal base band being coated with texture layer and is arranged in magnetron sputtering coating system, lead to into argon gas, control sputtering power, and metal base band, can at the surface formation CeO of texture layer by Duo Dao plated film district2-xFunctional layer; Described sputtering power is specially 50～1000W, and the described speed passed through is 1～200m/h.
As preferably, in step 1, described metal base band needs to use organic solvent to clean before use. Object is to clean the long texture layer on metal base band with certain orientation, to remove surface impurity. Described CeO2-xTarget material is prepared by chemical method.In step 2, described oxygen is pure oxygen, and purity is 99.99%.
In the method for the present invention, CeO2-xFunctional layer is prepared in common metal base band by pulsed laser deposition (PLD) or magnetron sputtering (MSD) system; CeO2-xFunctional layer surface nano-structure shape looks diversity can by changing oxygen partial pressure, growth temperature, sputtering power, excite the mode of deposition such as area, film thickness effectively to regulate and control, in preparation process, film has very high stable appearance and repeatability, and is evenly distributed at sample surfaces. With regard to production rate and cost performance, with reference to superconducting wire preparation, preparation technology of the present invention is more easy, and does not need to prepare superconducting layer and protective layer, has production rate and lower cost faster. Having benefited from function film is grown in flexible metal substrate so that the CeO of the present invention2-xNanostructure function film can be processed into desired shape according to needing in reality use, has better adaptability.
Compared with prior art, the present invention has following useful effect: the cerium oxide based on flexible metal base band that the present invention relates to (is called for short CeO2-x, 0≤x≤1) and the CeO for preparing of the method for nano thin-film and preparation method the present invention2-xNanostructure homogeneity is good, is uniformly dispersed, strong adhesion, surface topography and orientation thereof, size continuously adjustabe; The CeO that the present invention relates to2-xNano film thickness accurately controls, and can prepare MULTILAYER COMPOSITE nanostructure; The present invention relates to CeO2-xNano thin-film has metal flexible feature, can meet multiple application demand; The method preparation of the present invention is easy, is easy to realize industrialization and produces, and correlation parameter is more prone to control relative to traditional chemical process, and production cost can reduce greatly.
Specifically, present invention achieves many unexpected technique effects:
1, CeO prepared by the present invention is utilized2-xNanostructure homogeneity is good, is uniformly dispersed, strong adhesion, surface topography and orientation, size continuously adjustabe;
2, CeO prepared by the present invention is utilized2-xFilm thickness can accurately control, it is possible to preparation MULTILAYER COMPOSITE nanostructure;
3, the present invention has metal flexible feature, can meet multiple application demand, and sample can be mechanically cut into required size, reduces use cost;
4, relative growth mechanism and industrialization growth method are by big quantity research, and accurately the industrialization under control is produced and easily realized;
5, the preparation method of the present invention simultaneously is simple, and the experiment parameter relative chemical method in process of growth is more prone to control, and industrialization preparation cost can lower than 0.3 dollar/cm2。
Accompanying drawing explanation
By reading with reference to the detailed description that non-limiting example is done by the following drawings, the other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is CeO prepared by RABiT technology2-xNano thin-film sectional view;
Fig. 2 is the schematic diagram of hyperchannel dynamic laser pulsed deposition coating system;
Fig. 3 is the CeO of the preparation when high-energy-density2-xThe SEM measuring result of nano coating;
Fig. 4 is the CeO of the preparation when middle energy density2-xThe SEM measuring result of nano coating;
Fig. 5 is the CeO of the preparation when low energy densities2-xThe SEM measuring result of nano coating;
Fig. 6 is CeO2-xThe nanometer rod SEM picture of different orientation in nano coating;
Fig. 7 is CeO2-xNano coating XRD diffractogram;
Fig. 8 is laboratory sample.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail. The technician contributing to this area is understood the present invention by following examples further, but does not limit the present invention in any form.It should be appreciated that to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some distortion and improvement. These all belong to protection scope of the present invention.
As shown in Figure of description 1, it is the CeO adopting IBAD technology to prepare in the invention process process2-xNano thin-film sectional view, the method for the present invention makes CeO2-xGrowth is on the substrate with certain texture. Below, the present embodiment is implemented under premised on technical solution of the present invention, gives detailed enforcement mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment provides one to prepare CeO with PLD on the metallic substrate2-xThe preparation method of nano functional coating, comprises the following steps:
Step 1, preparation of samples;
Step 1.1, growing desired length have the metal base band of orientation texture layer to take out and clean with organic solvent; Object is to clean the long texture layer on metal base band with certain orientation, to remove surface impurity.
Step 1.2, the base band being coated with texture layer is repeatedly wound around it is arranged in multi-channel laser coating system;
Step 2, Preparatory work of experiment;
Step 2.1, opening device, the CeO prepared through chemical method2-xTarget material is contained in the target holder in cavity;
Step 2.2, adjustment target material are 25cm to the distance in base band plated film district;
Step 2.3, the Vacuum door closing coating system, and it is evacuated to 1 × 10-7Torr;
Step 3, startup well heater, rotate CeO simultaneously2-xTarget material, is warming up to required growth temperature 450 DEG C;
Step 4, closure molecule pump, lead to oxygen into coating system, and total gas pressure controls to required atmospheric pressure value, such as 200mTorr;
Step 5, startup excimer laser, and laser energy and frequency are raised to CeO2-xValue needed for nano functional layer coating process, E=300mJ, f=200Hz;
Step 6, etc. air pressure, temperature, laser energy, laser frequency stable after, open laser optical path switch, start the pre-evaporative process in laser target surface, this process approximately continues 5 minutes;
Step 7, etc. after the ellipsoid shape plasma stability that formed of laser evaporation, start coating system transmission mechanism, make the base band being fixed in coating system in advance with the speed of 10m/h once by plated film district, or with the speed of 50m/h by hyperchannel plated film district;
Step 8, complete CeO2-xAfter nano functional layer plated film, close laser optical path switch, close heater power source switch, close oxygen gas under meter valve, open pumped vacuum systems, progressively reduce office's device frequency and close excimer laser;
Step 9, actuator temperature to be heated are reduced to less than 50 DEG C, open nitrogen charging valve, make to fill in vacuum chamber air to 1 normal atmosphere, take out sample and cut into required size;
Embodiment 2
The present embodiment provides one to utilize PLD to prepare CeO on the metallic substrate2-xThe preparation method of nano functional coating, comprises the following steps:
Step 1, preparation of samples;
Step 1.1, growing desired length have the metal base band of orientation texture layer to take out and clean with organic solvent;
Step 1.2, the base band being coated with texture layer is repeatedly wound around it is arranged in multi-channel laser coating system;
Step 2, Preparatory work of experiment;
Step 2.1, opening device, the CeO prepared through chemical method2-xTarget material is contained in the target holder in cavity;
Step 2.2, adjustment target material are 5cm to the distance in base band plated film district;
Step 2.3, the Vacuum door closing coating system, and it is evacuated to 1 × 10-4Torr;
Step 3, startup well heater, rotate CeO simultaneously2-xTarget material, is warming up to required growth temperature 650 DEG C;
Step 4, closure molecule pump, lead to oxygen into coating system, and total gas pressure controls to required atmospheric pressure value, such as 200mTorr;
Step 5, startup excimer laser, and laser energy and frequency are raised to CeO2-xValue needed for nano functional layer coating process, E=50mJ, f=10Hz;
Step 6, etc. air pressure, temperature, laser energy, laser frequency stable after, open laser optical path switch, start the pre-evaporative process in laser target surface, this process approximately continues 5 minutes;
Step 7, etc. after the ellipsoid shape plasma stability that formed of laser evaporation, start coating system transmission mechanism, make the base band being fixed in coating system in advance with the speed of 1m/h once by plated film district, or with the speed of 5m/h by hyperchannel plated film district;
Step 8, complete CeO2-xAfter nano functional layer plated film, close laser optical path switch, close heater power source switch, close oxygen gas under meter valve, open pumped vacuum systems, progressively reduce office's device frequency and close excimer laser;
Step 9, actuator temperature to be heated are reduced to less than 50 DEG C, open nitrogen charging valve, make to fill in vacuum chamber air to 1 normal atmosphere, take out sample and cut into required size;
Embodiment 3
The present embodiment provides one to utilize MSD to prepare CeO on the metallic substrate2-xThe preparation method of nano functional coating, comprises the following steps:
Step 1, preparation of samples;
Step 1.1, growing desired length have the metal base band of orientation texture layer to take out and clean with organic solvent;
Step 1.2, the cerium oxide substrate base band with biaxial texture is repeatedly wound around it is arranged in multi-channel magnetic control coating system;
Step 2, Preparatory work of experiment;
Step 2.1, opening device, the CeO prepared through chemical method2-xTarget material is contained in the target holder in cavity;
Step 2.2, adjustment target material are 5cm to the distance in base band plated film district;
Step 2.3, the Vacuum door closing coating system, and it is evacuated to 1 × 10-6Torr;
Step 3, startup well heater, rotate CeO simultaneously2-xTarget material, is warming up to required growth temperature 550 DEG C;
Step 4, closure molecule pump, lead to oxygen into coating system, and total gas pressure controls to required atmospheric pressure value, such as 100mTorr; Can playing brightness after leading to argon gas to starting current, the power of control sputtering is 50W simultaneously;
Step 5, etc. sputtering stable after, start coating system transmission mechanism, make base band with the speed of 1m/h once by plated film district, or with the speed of 5m/h by hyperchannel plated film district;
Step 6, complete CeO2-xAfter nano functional layer plated film, close sputtering power switch, close heater power source switch, close oxygen gas under meter valve;
Step 7, when temperature is down to below 50 DEG C, open nitrogen charging valve, make normal atmosphere to normal atmosphere in vacuum chamber, take out sample and cut into required size;
Embodiment 4
The present embodiment provides one to utilize MSD to prepare CeO on the metallic substrate2-xThe preparation method of nano functional coating, comprises the following steps:
Step 1, preparation of samples;
Step 1.1, growing desired length have the metal base band of orientation texture layer to take out and clean with organic solvent;
Step 1.2, the cerium oxide substrate base band with biaxial texture is repeatedly wound around it is arranged in multi-channel magnetic control coating system;
Step 2, Preparatory work of experiment;
Step 2.1, opening device, the CeO prepared through chemical method2-xTarget material is contained in the target holder in cavity;
Step 2.2, adjustment target material are 10cm to the distance in base band plated film district;
Step 2.3, the Vacuum door closing coating system, and it is evacuated to 1 × 10-6Torr;
Step 3, startup well heater, rotate CeO simultaneously2-xTarget material, is warming up to required growth temperature 550 DEG C;
Step 4, closure molecule pump, lead to oxygen into coating system, and total gas pressure controls to required atmospheric pressure value, such as 100mTorr; Can playing brightness after leading to argon gas to starting current, the power of control sputtering is 1000W simultaneously;
Step 5, etc. sputtering stable after, start coating system transmission mechanism, make base band with the speed of 40m/h once by plated film district, or with the speed of 200m/h by hyperchannel plated film district;
Step 6, complete CeO2-xAfter nano functional layer plated film, close sputtering power switch, close heater power source switch, close oxygen gas under meter valve;
Step 7, when temperature is down to below 50 DEG C, open nitrogen charging valve, make normal atmosphere to normal atmosphere in vacuum chamber, take out sample and cut into required size;
Fig. 1 is CeO prepared by RABiT technology2-xNano thin-film sectional view; Fig. 2 is the schematic diagram of hyperchannel dynamic laser pulsed deposition coating system, wherein: label 1 is guiding hyperchannel runner, and label 2 is leader tape, and label 3 is well heater, and label 4 is for focusing on lens, and label 5 is target material, and label 6 is laser beam; Fig. 3 is the CeO of the preparation when high-energy-density2-xThe SEM measuring result of nano coating, right figure is office's territory enlarged image of left figure, presents the columnar nanometer shape looks of rule; Fig. 4 is the CeO of the preparation when middle energy density2-xThe SEM measuring result of nano coating, right figure is office's territory enlarged image of left figure, and the column presenting rule mixes nanotopography with triangle sheet; Fig. 5 is the CeO of the preparation when low energy densities2-xThe SEM measuring result of nano coating, right figure is office's territory enlarged image of left figure, presents starlike nanotopography; Fig. 6 is CeO2-xThe nanometer rod SEM picture of different orientation in nano coating, under 650 DEG C of growth temperatures, CeO2-xThe shape looks feature of nano coating when different range, it can be seen that along with range reduces, the orientation of nano-pillar is consistent gradually; Fig. 7 is CeO2-xNano coating XRD diffractogram, by completely, (001) derives (110) and (111) gradually on its surface; Fig. 8 is laboratory sample.
In sum, the present invention relates to the cerium oxide based on flexible metal base band and (it is called for short CeO2-x, 0≤x≤1) and the CeO for preparing of the method for nano thin-film and preparation method the present invention2-xNanostructure homogeneity is good, is uniformly dispersed, strong adhesion, surface topography and orientation thereof, size continuously adjustabe; The CeO that the present invention relates to2-xNano film thickness accurately controls, and can prepare MULTILAYER COMPOSITE nanostructure; The present invention relates to CeO2-xNano thin-film has metal flexible feature, can meet multiple application demand; The method preparation of the present invention is easy, is easy to realize industrialization and produces, and correlation parameter is more prone to control relative to traditional chemical process, and production cost can reduce greatly.
Above specific embodiments of the invention are described. It is understood that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect the flesh and blood of the present invention.
Claims (13)
1. the CeO based on flexible metal base band2-xNano thin-film, it is characterised in that, described CeO2-xNano thin-film is different morphologies and orientation, described CeO2-xThe structure of nano thin-film is the nano particle of array-like arrangement.
2. the CeO based on flexible metal base band according to claim 12-xNano thin-film, is characterized in that, described CeO2-xNano thin-film comprises metal base, texture layer, CeO2-xFunctional layer.
3. the CeO2-x nano thin-film based on flexible metal base band according to claim 1, is characterized in that, the shape of described nano particle is bar-shaped, sheet, the cluster shape of multiple nanometer sheet composition, starlike, or polygonized structure.
4. the CeO based on flexible metal base band according to claim 12-xNano thin-film, is characterized in that, described CeO2-xBeing oriented to (001) of nano thin-film, (110), the combination of (111) or aforementioned orientation.
5. the CeO based on flexible metal base band as claimed in claim 12-xThe preparation method of nano thin-film, it is characterised in that, comprise the steps:
Step 1, gets metal base band and is installed on transmission mechanism, get CeO2-xTarget material is also installed to target platform, is vacuumized by filming equipment afterwards; On wherein said metal base band, growth has certain orientation texture layer;
Step 2, the temperature in adjustment plated film district is to growth temperature; Adopt pulse laser deposition or magnetron sputtering deposition method; Lead to afterwards into oxygen; Coating system transport unit drives metal base band so that metal base band, by plated film district, namely forms CeO on the surface of the texture layer of metal base band2-xFunctional layer.
6. preparation method according to claim 5, is characterized in that, in step 1, and described CeO2-xTarget material is 5-25cm to the distance in plated film district.
7. preparation method according to claim 5, is characterized in that, in step 2, described growth temperature is 450～650 DEG C.
8. preparation method according to claim 5, is characterized in that, in step 2, and described CeO2-xThe thickness of functional layer is 10～2000nm.
9. preparation method according to claim 5, is characterized in that, in step 2, before leading to oxygen, and plated film district vacuum state; After leading to oxygen, plated film district air pressure is 5～200mTorr.
10. preparation method according to claim 9, is characterized in that, described vacuum state air pressure is 1 × 10-4～1 × 10-7Torr。
11. preparation methods according to claim 5, is characterized in that, in step 2, described employing pulse laser deposition is specially, and regulate laser energy and the frequency of PLD, and described laser energy and frequency are specially: E=50～300mJ, f=10～200Hz.
12. preparation methods according to claim 5, is characterized in that, described metal base band is one or many by the number of times in plated film district, is specially: with the speed of 1～10m/h once by plated film district, or with the speed of 5～50m/h by hyperchannel plated film district.
13. preparation methods according to claim 5, it is characterized in that, described magnetron sputtering deposition method is specially, being wound around by the metal base band being coated with texture layer is arranged in magnetron sputtering coating system, lead to into argon gas, control sputtering power, metal base band, can at the surface formation CeO of texture layer by Duo Dao plated film district2-xFunctional layer; Described sputtering power is specially 50～1000W, and the described speed passed through is 1～200m/h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109132999A (en) * | 2018-09-05 | 2019-01-04 | 天津瑞晟晖能科技有限公司 | Metal oxide nano array film and preparation method thereof and the electrode comprising it, battery |
| CN110724922A (en) * | 2019-10-31 | 2020-01-24 | 汕头大学 | Epitaxial AZO film with controllable crystal orientation and polarity on flexible substrate and preparation method thereof |
| CN113388874A (en) * | 2020-03-13 | 2021-09-14 | 中国科学院上海硅酸盐研究所 | Cerium oxide/titanium oxide heterojunction film with biological oxidation resistance function and preparation method and application thereof |
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| CN109132999A (en) * | 2018-09-05 | 2019-01-04 | 天津瑞晟晖能科技有限公司 | Metal oxide nano array film and preparation method thereof and the electrode comprising it, battery |
| CN110724922A (en) * | 2019-10-31 | 2020-01-24 | 汕头大学 | Epitaxial AZO film with controllable crystal orientation and polarity on flexible substrate and preparation method thereof |
| CN113388874A (en) * | 2020-03-13 | 2021-09-14 | 中国科学院上海硅酸盐研究所 | Cerium oxide/titanium oxide heterojunction film with biological oxidation resistance function and preparation method and application thereof |
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