CN116575001A - Al (aluminum) alloy 50 Cr 50 Al-Cr-O double-layer film with aluminum-rich corundum structure, and preparation method and application thereof - Google Patents
Al (aluminum) alloy 50 Cr 50 Al-Cr-O double-layer film with aluminum-rich corundum structure, and preparation method and application thereof Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 58
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 50
- 239000010431 corundum Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000956 alloy Substances 0.000 title description 6
- 229910045601 alloy Inorganic materials 0.000 title description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 107
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 30
- 239000010949 copper Substances 0.000 claims description 30
- 229910052802 copper Inorganic materials 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 26
- 238000000151 deposition Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 14
- 238000004544 sputter deposition Methods 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000010409 thin film Substances 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000992 sputter etching Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 59
- 239000011159 matrix material Substances 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001341 grazing-angle X-ray diffraction Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010849 ion bombardment Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000005546 reactive sputtering Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses an Al 50 Cr 50 Al-Cr-O double-layer film with aluminum-rich corundum structure, and preparation method and application thereof 50 Cr 50 A film layer and an Al-Cr-O film layer with an aluminum-rich corundum structure; the Al-Cr-O film layer with the aluminum-enriched corundum structure comprises alpha-Cr 2 O 3 Phase, alpha-Al 2 O 3 Phase sum alpha- (Al, cr) 2 O 3 Phase, free of metastable phase Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The aluminum content of the Al-Cr-O film layer with the aluminum-rich corundum structure is 32.5 to 35.1 weight percent. Al (Al) 50 Cr 50 The film layer, the base material and the Al-Cr-O film layer all have higher bonding strength and bonding effect. Al (Al) 50 Cr 50 The film layer is made of Al-Cr-The O film layer has the function of oxidizing into an Al-Cr-O film layer at a low temperature when being continuously damaged by ion etching and craftsman impact.
Description
Technical Field
The invention belongs to the field of materials, and in particular relates to an Al alloy 50 Cr 50 Al-Cr with aluminium-rich corundum structure-O double-layer film, and preparation method and application thereof.
Background
Copper has high thermal conductivity, high electrical conductivity and is resistant to CO 2 High laser reflectivity, and the like, is a radio frequency lath CO 2 Preferred strip electrode materials for lasers, however copper electrodes have poor oxidation resistance, ion bombardment resistance and laser shock damage resistance, significantly increasing the CO exposure to the electrode surface 2 Loss absorption of the laser waveguide. At present, a learner deposits alpha-Al on the surface of an oxygen-free copper polar plate at a high temperature of 800 ℃ by using a Chemical Vapor Deposition (CVD) method 2 O 3 Film, radio frequency slat CO 2 Stable output performance of oxygen-free copper electrode plate in laser. However, oxygen-free copper and alpha-Al 2 O 3 The interface compatibility between the films is poor, the difference of thermal expansion coefficients is large, and the interface thermal stress is easy to form in cold-hot fatigue and laser shock to fall off; in addition, the vapor pressure of the Wen Jiban oxygen-free copper is larger at the temperature of more than 800 ℃ during CVD deposition, and the alpha-Al is polluted 2 O 3 The film surface also reduces the surface layer alpha-Al 2 O 3 Performance of the film. Deposition of alpha-Al directly on oxygen-free copper surface by reactive sputtering 2 O 3 The copper matrix is directly oxidized at the same time of alpha-Al 2 O 3 The interface compatibility with copper is poor, the problem of larger difference of thermal expansion coefficients is not solved, and the alpha-Al is directly deposited on a copper substrate by reactive sputtering 2 O 3 Films also have difficulty in achieving a film that bonds strongly to the substrate.
Disclosure of Invention
In order to solve the above-mentioned drawbacks and disadvantages of the prior art, an object of the present invention is to provide a film.
The second object of the present invention is to provide a method for preparing the above film.
It is a further object of the present invention to provide a film as defined above in CO 2 Application in lasers.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a first aspect of the present invention is to provide a film comprising Al 50 Cr 50 Film layer and Al-Cr-O film with aluminum-enriched corundum structureA layer; the Al-Cr-O film layer with the aluminum-enriched corundum structure comprises alpha-Cr 2 O 3 Phase, alpha-Al 2 O 3 Phase sum alpha- (Al, cr) 2 O 3 Phase, free of metastable phase Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The aluminum content of the Al-Cr-O film layer with the aluminum-rich corundum structure is 32.5 to 35.1 weight percent. The Al-Cr-O film layer with the aluminum-rich corundum structure has the structure similar to alpha-Al 2 O 3 Similar oxidation, ion bombardment and laser shock damage resistance. Al (Al) 50 Cr 50 The film layer has better bonding effect with the base material (such as oxygen-free copper polar plate) and the Al-Cr-O film layer with an aluminum-rich corundum structure, and when Al 50 Cr 50 When the Al-Cr-O film layer of the aluminum-enriched corundum structure on the surface layer of the film layer is continuously damaged by ion etching and craftsman impact, the Al-Cr-O film layer of the aluminum-enriched corundum structure has the function of oxidizing the Al-Cr-O film layer of the aluminum-enriched corundum structure at a low temperature. Thus, the film of the invention has self-repairing function.
Preferably, the Al 50 Cr 50 The film layer is formed on the substrate; the Al-Cr-O film layer with the aluminum-rich corundum structure is positioned on Al 50 Cr 50 And a thin film layer.
Preferably, the substrate comprises an oxygen free copper substrate.
Preferably, the Al 50 Cr 50 The thickness of the film layer is 0.5-1 mu m.
Preferably, the thickness of the Al-Cr-O film layer with the aluminum-enriched corundum structure is 200-500 nm.
Another object of the present invention is to provide a method for preparing a film according to the first aspect of the present invention, the method comprising the steps of:
s1: al is formed on the surface of the base material by direct current magnetron sputtering 50 Cr 50 A thin film layer;
s2: at a temperature of 540-580 ℃ and O 2 Ar+O with partial pressure of 15-20% 2 Under the mixed gas, al is formed 50 Cr 50 Thermally oxidizing the film layer for 30-40 min;
s3: at a temperature of 500-580 ℃ and O 2 Ar+O with partial pressure of 9-11% 2 Under the mixed gas, radio frequency magnetism is adoptedControlled sputtering of Al 70 Cr 30 Target material of Al 50 Cr 50 And forming an Al-Cr-O film layer with an aluminum-rich corundum structure on the film layer to obtain the film.
Step S2 of the invention is performed on Al 50 Cr 50 Forming a corundum structure seed crystal layer on the film layer to ensure Al 50 Cr 50 The amorphous phase of the interface between the Al-Cr-O film layer with the aluminum-rich corundum structure and the Al-Cr-O film layer with the aluminum-rich corundum structure can be eliminated when the Al-Cr-O film layer with the aluminum-rich corundum structure is deposited on the surface layer of the film layer at low temperature. In addition, the invention is realized by adopting Al 50 Cr 50 The film layer can protect the substrate from oxidation and then form a protective film on the Al 50 Cr 50 Depositing Al-Cr-O film layer with aluminum-rich corundum structure on the film layer at low temperature to promote the deposition of alpha-Al on the surface of the film layer at low temperature 2 O 3 And (3) phase (C).
Preferably, in step S2, the relationship between the oxygen partial pressure and the thermal oxidation temperature is: when the partial pressure of oxygen is high, a lower thermal oxidation temperature is selected, and when the partial pressure of oxygen is low, a higher thermal oxidation temperature is selected. For example: when the O2 partial pressure was 16%, the thermal oxidation temperature was 580℃and when the O2 partial pressure was 20%, the thermal oxidation temperature was 540 ℃.
Preferably, the preparation method further comprises step S01: al is added with 50 Cr 50 Target material and Al 70 Cr 30 The targets are respectively arranged at corresponding target stations of the direct-current magnetron sputtering system and the radio-frequency magnetron sputtering system; step S02: pretreating the ground and polished base material, then placing the base material on a sample stage of a magnetron sputtering system, and adjusting the distance between the base material and the target material; step S03: and exhausting water vapor from a vacuum chamber of the magnetron sputtering system, then pumping to the background vacuum degree, heating the substrate to 90-110 ℃, and then pumping to the background vacuum degree.
Preferably, the step S1 specifically includes: sputtering Al with DC magnetic control in Ar atmosphere 50 Cr 50 The target material deposits Al on the surface of the base material with the temperature of 90-110 DEG C 50 Cr 50 A thin film layer. Al (Al) 50 Cr 50 The thin film layer is to protect the substrate from oxidation and enhance the bonding force between the thin film layer and the substrate.
Preferably, the parameter conditions of the direct current magnetron sputtering are as follows: the target power density is: 4-6W/cm 2 The sputtering time is 20-30 min.
Preferably, the parameter conditions of the radio frequency magnetron sputtering are as follows: the target power density is 6-10W/cm 2 The working air pressure is 0.6-1.4 Pa, and the deposition time is 180-360 min.
Preferably, the substrate is bonded with Al 50 Cr 50 Target and/or Al 70 Cr 30 The distance between the targets is 50-80 mm.
Preferably, the step S2 specifically includes: closing the direct current magnetron sputtering system, closing Ar gas, heating the substrate to 540-580 ℃, vacuumizing to the background vacuum degree, and introducing O 2 Ar+O with partial pressure of 15-20% 2 Mixed gas of Al 50 Cr 50 The film layer is thermally oxidized for 30-40 min.
It is a third object of the present invention to provide a film as provided in the first aspect of the present invention in CO 2 Application in lasers. Application of the film of the invention to CO 2 In the laser, CO can be made 2 The laser has the excellent performances of high output power, long service life, high beam quality, good thermal stability and the like.
The beneficial effects of the invention are as follows: in the present invention, al 50 Cr 50 The film layer, the base material and the Al-Cr-O film layer with the aluminum-enriched corundum structure all have higher bonding strength and bonding effect. Al in the present invention 50 Cr 50 When the Al-Cr-O film layer with the aluminum-enriched corundum structure is continuously damaged by ion etching and craftsman impact, the film layer has the function of oxidizing the Al-Cr-O film layer with the aluminum-enriched corundum structure at low temperature, and the oxidation temperature is obviously lower than that of the preparation of alpha-Al on the surface of a substrate in the prior art document 2 O 3 Deposition temperature of the thin film. In addition, the Al-Cr-O thin film layer of the aluminum-rich corundum structure deposited at a temperature above 500 ℃ comprises alpha-Cr 2 O 3 Phase, alpha-Al 2 O 3 Phase sum alpha- (Al, cr) 2 O 3 Phase, free of metastable phase Al 2 O 3 Thus is suitable for radio frequency lath CO 2 Low temperature deposition of alpha-Al on the copper electrode surface of laser ribbon 2 O 3 A film.
In Al by the method of the invention 50 Cr 50 The Al content of the Al-Cr-O film layer with the aluminum-enriched corundum structure deposited on the surface of the film layer is in the range of 32.5wt.% to 35.1wt.%, and the content is higher than that described in the prior art.
Drawings
FIG. 1 is Al in example 1 50 Cr 50 SEM surface topography of Al-Cr-O double-layer film with aluminum-enriched corundum structure.
FIG. 2 is Al in example 1 50 Cr 50 SEM cross-sectional morphology diagram of Al-Cr-O double-layer film with aluminum-enriched corundum structure.
FIG. 3 is Al in example 1 50 Cr 50 GIXRD pattern of Al-Cr-O double-layer film with aluminum-enriched corundum structure.
Detailed Description
Specific embodiments of the present invention will be described in further detail below with reference to the drawings and examples, but the practice and protection of the present invention are not limited thereto. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
Example 1
Al in this example 50 Cr 50 The Al-Cr-O double-layer film with the aluminum-enriched corundum structure is prepared by adopting the following method, and the specific steps are as follows:
(1) Customizing phi 60 mm of Al 70 Cr 30 And Al 50 Cr 50 Alloy targets are arranged on corresponding target stations, and the base distance of the targets is adjusted to 80mm.
(2) Cutting oxygen-free copper into 10mm multiplied by 1mm, mechanically grinding, polishing to a mirror surface, then placing in acetone and absolute ethyl alcohol, ultrasonically cleaning for 15min, drying, and placing on a sample table.
(3) Pre-vacuumizing to 5.0Pa, and opening molecular pump to vacuum to background vacuum degree of 5×10 -4 Pa to remove water vapor, heating oxygen-free copper matrix to 100deg.C, and continuously vacuumizing to background vacuum degree of 5×10 -4 Pa。
(4) Introducing high-purity Ar gas into the vacuum chamber, regulating the air pressure to 1.0Pa, maintaining the temperature at 100 ℃, and sputtering Al by using a direct current power supply 50 Cr 50 Alloy target with target power density of 5W/cm 2 Sputtering time is 30min, al with thickness of 0.6 μm is prepared on the surface of the oxygen-free copper matrix 50 Cr 50 And a transition layer.
(5) Closing the DC magnetron sputtering system, closing Ar gas, heating the substrate to 540 ℃, and vacuumizing to a background vacuum degree of 5 multiplied by 10 -4 Pa, let in O 2 Ar+O with partial pressure of 20% 2 The mixed gas is used for depositing Al on the surface of oxygen-free copper 50 Cr 50 The film was thermally oxidized for 30min.
(6) Adjusting Ar+O 2 O in the mixed gas 2 Partial pressure to 11%, regulating air pressure to 1.0Pa, controlling matrix temperature to 540 deg.C, and opening Al 70 Cr 30 The RF power source of the target pre-sputters for 15min to remove contaminants and oxides from the target surface. Subsequently increasing the target power density to 8W/cm 2 Sputtering Al with radio frequency reaction 70 Cr 30 After 180min of target material deposition, copper-based Al is deposited 50 Cr 50 The Al-Cr-O film with the corundum structure of 0.3 mu m is obtained on the surface of the transition layer.
(7) After the deposition is finished, the sputtering power supply and the gas are sequentially turned off, and then the vacuum is pumped until the background vacuum degree is 5 multiplied by 10 -4 Pa. Maintaining the temperature of the substrate for 20-30 min to remove O remained in the film 2 The matrix heating power is then turned off. After the substrate temperature is lower than 100deg.C, the vacuum chamber can be opened and the sample taken out to obtain Al in this example 50 Cr 50 Al-Cr-O double-layer film with aluminum-enriched corundum structure 50 Cr 50 An Al-Cr-O double-layer film with an aluminum-rich corundum structure is formed on the surface of an oxygen-free copper substrate, wherein Al 50 Cr 50 The film is positioned between the Al-Cr-O film with the aluminum-enriched corundum structure and the copper substrate.
Al in this example 50 Cr 50 The SEM surface morphology of the Al-Cr-O double-layer film with the aluminum-rich corundum structure is shown in figure 1, and figure 1 shows that the film has an island growth form, a compact and flat surface and uniform nano particles. Al in this example 50 Cr 50 SEM cross-sectional morphology of Al-Cr-O bilayer film with aluminum-rich corundum structure is shown in FIG. 2, FIG. 2 reflects thickness and deposition rate of deposited film and it can be seen from FIG. 2 that oxygen-free copper matrix, al 50 Cr 50 The interface bonding between the film and the Al-Cr-O film is firm, and no obvious cracks exist. The GIXRD pattern of the Al-Cr-O film in this example is shown in FIG. 3, which shows that the Al-Cr-O film is composed of alpha-Cr 2 O 3 、α-Al 2 O 3 And alpha- (Al, cr) 2 O 3 Three corundum structural phases.
Example 2
Al in this example 50 Cr 50 The Al-Cr-O double-layer film with the aluminum-enriched corundum structure is prepared by adopting the following method, and the specific steps are as follows:
(1) Customizing phi 60 mm of Al 70 Cr 30 And Al 50 Cr 50 Alloy targets are arranged on corresponding target stations, and the base distance of the targets is adjusted to 80mm.
(2) Cutting oxygen-free copper into 10mm multiplied by 1mm, mechanically grinding, polishing to a mirror surface, then placing in acetone and absolute ethyl alcohol, ultrasonically cleaning for 15min, drying, and placing on a sample table.
(3) Pre-vacuumizing to 5.0Pa, and opening molecular pump to vacuum to background vacuum degree of 5×10 -4 Pa, heating oxygen-free copper matrix to 100deg.C, and continuously vacuumizing to background vacuum degree of 5×10 -4 Pa。
(4) Introducing high-purity Ar gas into the vacuum chamber, regulating the air pressure to 1.0Pa, maintaining the temperature at 100 ℃, and sputtering Al by using a direct current power supply 50 Cr 50 Alloy target with target power density of 5W/cm 2 Sputtering time is 30min, al with thickness of 0.6 μm is prepared on the surface of the oxygen-free copper matrix 50 Cr 50 And a transition layer.
(5) Closing the DC magnetron sputtering system, closing Ar gas, heating the substrate to 540 ℃, and vacuumizing to a background vacuum degree of 5 multiplied by 10 -4 Pa, let in O 2 Ar+O with partial pressure of 20% 2 The mixed gas is used for depositing Al on the surface of oxygen-free copper 50 Cr 50 The film was thermally oxidized for 30min.
(6) Adjusting Ar+O 2 Mixed gasIn vivo O 2 Partial pressure to 11%, regulating air pressure to 1.0Pa, controlling matrix temperature to 500 deg.C, and opening Al 70 Cr 30 The RF power source of the target pre-sputters for 15min to remove contaminants and oxides from the target surface. Subsequently increasing the target power density to 8W/cm 2 Sputtering Al with radio frequency reaction 70 Cr 30 After 180min of target material deposition, copper-based Al is deposited 50 Cr 50 The Al-Cr-O film with the corundum structure of 0.3 mu m is obtained on the surface of the transition layer.
(7) After the deposition is finished, the sputtering power supply and the gas are sequentially turned off, and then the vacuum is pumped until the background vacuum degree is 5 multiplied by 10 -4 Pa. Maintaining the temperature of the substrate for 20-30 min to remove O remained in the film 2 The matrix heating power is then turned off. After the temperature of the substrate is lower than 100deg.C, the vacuum chamber is opened and the sample is taken out to obtain Al formed on the surface of the copper substrate 50 Cr 50 Al-Cr-O double-layer film with aluminum-enriched corundum structure.
Tested, al deposited on the surface of the copper substrate in this example 50 Cr 50 Al-Cr-O double-layer film with aluminum-enriched corundum structure and compact and smooth surface, good nano-particle uniformity and Al 50 Cr 50 Between the film layers of the film and the Al-Cr-O film with aluminum-enriched corundum structure, al 50 Cr 50 The film and the copper substrate are well combined, and the deposited Al-Cr-O film is formed by alpha phase (alpha phase is alpha-Cr 2 O 3 、α-Al 2 O 3 And alpha- (Al, cr) 2 O 3 ) Composition is prepared.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A film, characterized in that: the film comprises Al 50 Cr 50 A film layer and an Al-Cr-O film layer with an aluminum-rich corundum structure; the Al-Cr-O film layer with the aluminum-enriched corundum structure comprises alpha-Cr 2 O 3 Phase, alpha-Al 2 O 3 Phase sum alpha- (Al, cr) 2 O 3 Phase, free of metastable phase Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The aluminum content of the Al-Cr-O film layer with the aluminum-rich corundum structure is 32.5 to 35.1 weight percent.
2. The film according to claim 1, wherein: the Al is 50 Cr 50 The film layer is formed on the substrate; the Al-Cr-O film layer with the aluminum-rich corundum structure is positioned on Al 50 Cr 50 And a thin film layer.
3. A film according to claim 2, wherein: the substrate comprises an oxygen free copper substrate.
4. The film according to claim 1, wherein: the Al is 50 Cr 50 The thickness of the film layer is 0.5-1 mu m.
5. The film according to claim 1, wherein: the thickness of the Al-Cr-O film layer with the aluminum-enriched corundum structure is 200-500 nm.
6. The method for producing a film according to any one of claims 1 to 5, characterized in that: the method comprises the following steps:
s1: al is formed on the surface of the base material by direct current magnetron sputtering 50 Cr 50 A thin film layer;
s2: at a temperature of 540-580 ℃ and O 2 Ar+O with partial pressure of 15-20% 2 Under the mixed gas, al is formed 50 Cr 50 Thermally oxidizing the film layer for 30-40 min;
s3: at a temperature of 500-580 ℃ and O 2 Ar+O with partial pressure of 9-11% 2 Under the mixed gas, adopting radio frequency magnetron sputtering Al 70 Cr 30 Target material of Al 50 Cr 50 And forming an Al-Cr-O film layer with an aluminum-rich corundum structure on the film layer to obtain the film.
7. According to claim 6The preparation method of the film is characterized in that: the step S1 specifically comprises the following steps: sputtering Al with DC magnetic control in Ar atmosphere 50 Cr 50 The target material deposits Al on the surface of the base material with the temperature of 90-110 DEG C 50 Cr 50 And a transition layer.
8. The method for producing a film according to claim 6 or 7, characterized in that: the parameter conditions of the direct current magnetron sputtering are as follows: the target power density is: 4-6W/cm 2 The sputtering time is 20-30 min.
9. The method for producing a film according to claim 6, wherein: the parameter conditions of the radio frequency magnetron sputtering are as follows: the target power density is 6-10W/cm 2 The working air pressure is 0.6-1.4 Pa, and the deposition time is 180-360 min.
10. A film according to any one of claims 1 to 5 in CO 2 Application in lasers.
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| CN202310404349.0A CN116575001A (en) | 2023-04-14 | 2023-04-14 | Al (aluminum) alloy 50 Cr 50 Al-Cr-O double-layer film with aluminum-rich corundum structure, and preparation method and application thereof |
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| CN202310404349.0A CN116575001A (en) | 2023-04-14 | 2023-04-14 | Al (aluminum) alloy 50 Cr 50 Al-Cr-O double-layer film with aluminum-rich corundum structure, and preparation method and application thereof |
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