CN104112562A - Sm-Co-based permanent-magnet thin film high in film-base binding force and preparation method thereof - Google Patents
Sm-Co-based permanent-magnet thin film high in film-base binding force and preparation method thereof Download PDFInfo
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Abstract
The invention provides an Sm-Co-based permanent-magnet thin film high in film-base binding force. A buffer layer is arranged between the Sm-Co-based permanent-magnet thin film and a base body and is of a two-layer structure, one layer is a copper thin film layer positioned on the surface of the base body while the other layer is a tungsten thin film layer positioned on the surface of the copper thin film layer, and binding force between the Sm-Co-based permanent-magnet thin film and the base body can be improved effectively. Experiments verify that heat treatment temperature of the Sm-Co-based permanent-magnet thin film of the structure during heat treatment can be increased substantially from 600-800 DEG C currently to above 900 DEG C, and the Sm-Co-based permanent-magnet thin film can still be well bound with the base body and cannot shed when the heat treatment temperature is as high as 1000 DEG C.
Description
Technical field
The invention belongs to permanent magnetic thin film technical field, relate in particular to a kind of Sm-Co base permanent magnetic thin film in high-temperature heat treatment with high film-substrate cohesion and preparation method thereof, this Sm-Co base permanent magnetic thin film can keep good film-substrate cohesion in the high-temperature heat treatment process of 1000 ℃, and do not affect permanent magnetic thin film magnetic property, permanent magnetic thin film is mainly applicable to the fields such as magnetic micromachine and micromachine.
Background technology
The Sm-Co base permanent magnetic thin film that is deposited on silicon substrate surface (for example silicon chip), due to its high Curie temperature, good corrosion resistance, has important application in magnetic MEMS (micro electro mechanical system).Generally, this Sm-Co base permanent magnetic thin film is noncrystalline state after matrix surface deposition, changes crystalline state into, thereby obtain certain magnetic property after high-temperature heat treatment.
Conventionally, along with Sm-Co base permanent magnetic thin film thickness increases, film-substrate cohesion weakens gradually; In addition, because Sm-Co base permanent magnetic thin film is different with base thermal coefficient of expansion, when the thickness of Sm-Co base permanent magnetic thin film increases, the stress in film thermal processing procedure also increases gradually, thereby causes film easily from matrix surface, to come off, and directly affects the application of film.Therefore, the thickness of the actual Sm-Co base permanent magnetic thin film using is micron dimension at present.
Due to Sm-Co base film and basis material, the marriage relation between film and matrix may be both only a kind of simple physical bond, also may have very strong chemical bonds.Physical bond comprises Van der Waals force combination and electrostatic force combination.Van der Waals force, by the generation that polarizes mutually of two kinds of materials, is a kind of short-range contingence, when interatomic distance slightly increases, just trends towards rapidly zero.While therefore realizing the combination of film and matrix by Van der Waals force, film-substrate cohesion is poor.Electrostatic force is in conjunction with also there being the problem that adhesion is less.Compare with physical bond, chemical bond power is larger, and film base, in conjunction with effective, still need to form new compound between interface.
In order to improve film-substrate cohesion, a kind of current method is, between matrix surface and Sm-Co base permanent magnetic thin film, resilient coating is set.For example, application number is that to propose to arrange thickness between the Sm-Co of matrix surface and micron dimension base permanent magnetic thin film be that the W film layer of 10nm～200nm is as resilient coating to the Chinese patent application of CN201210200142.3, can improve the adhesive force between this Sm-Co base permanent magnetic thin film and matrix, make it after 750 ℃ of the high temperature anneal, still not depart from matrix.But experimental verification is when heat treatment temperature further improves, for example, while being increased to 800 ℃, will there is obscission in this Sm-Co base permanent magnetic thin film, and when being increased to 1000 ℃, obscission is very serious.
On the other hand, in order to give full play to the magnetic property of Sm-Co base permanent magnetic thin film, often need higher heat treatment temperature.But, as described above, be subject to the restriction of film-substrate cohesion, current Sm-Co base permanent magnetic thin film heat treatment temperature is often confined to 600 ℃～800 ℃ scopes, when exceed this temperature range only tens of degree just may cause Sm-Co base permanent magnetic thin film to occur obscission.
Summary of the invention
Technical purpose of the present invention is the problem easily coming off from matrix surface under higher heat treatment temperature for the above-mentioned Sm-Co base permanent magnetic thin film that is positioned at matrix surface, a kind of Sm-Co base permanent magnetic thin film is provided, the adhesion of this film and matrix is strong, thereby can improve heat treatment temperature, even when heat treatment temperature, be still combined during up to 1000 ℃ intactly with matrix, do not occur obscission.
The present invention realizes the technical scheme that above-mentioned technical purpose adopts: a kind of Sm-Co base permanent magnetic thin film with high film-substrate cohesion, described Sm-Co base permanent magnetic thin film is positioned at matrix surface, between described matrix and Sm-Co base permanent magnetic thin film, it is resilient coating, this resilient coating is double-layer structure, one deck is and the copper film layer Huo person Molybdenum thin layer that is positioned at matrix surface that another layer is tungsten (W) thin layer that is positioned at this copper film layer surface.
Described matrix is not limit, and comprises silicon chip, Si/SiO
2substrate, alumina substrate etc., as preferably, described matrix is Si/SiO
2(100) substrate, surface is with SiO
2si (100) type substrate.
As preferably, described Sm-Co base permanent magnetic thin film thickness is 0.1um～100um, more preferably 0.5um～50um, more preferably 1um～10um.
As preferably, described copper film layer thickness or Mo Molybdenum thin layer thickness are 5nm～100nm, more preferably 10nm～50nm;
As preferably, described W film layer thickness is 30nm～500nm, more preferably 100nm～300nm.
The present invention also provides a kind of above-mentioned preparation method with the Sm-Co base permanent magnetic thin film of high film-substrate cohesion, comprises the steps:
Step 1: adopt magnetron sputtering technique, take copper target as resilient coating target, at substrate material surface sputtering sedimentation copper film layer, then take tungsten target as resilient coating target, at copper film layer surface sputtering deposits tungsten thin layer;
Step 2: adopt magnetron sputtering technique, take Sm-Co based composites as target, at W film layer surface sputtering deposition Sm-Co base permanent magnetic thin film;
Step 3: the Sm-Co base permanent magnetic thin film after step 2 is processed is heat-treated.
In above-mentioned preparation method, the heat treatment temperature of step 3 reaches more than 900 ℃.
As preferably, in above-mentioned preparation method, the heat treatment time of step 3 is 5min～120min.
In sum, the present invention, by insert the double-layer bumper layer consisting of copper film layer and W film layer between matrix and Sm-Co base permanent magnetic thin film, has effectively improved the adhesion of Sm-Co base permanent magnetic thin film and matrix.Experiment confirms, the heat treatment temperature of the Sm-Co base permanent magnetic thin film of this structure in heat treatment process is greatly improved, can rise to more than 900 ℃ from existing 600 ℃～800 ℃, even when heat treatment temperature, be still combined during up to 1000 ℃ intactly with matrix, do not occur obscission.
Accompanying drawing explanation
Fig. 1 is the situation figure that the Sm-Co base permanent magnetic thin film sample A with individual layer W resilient coating for preparing in comparative example 1 anneals after 10min under 800 ℃ of conditions;
Fig. 2 is the situation figure that the Sm-Co base permanent magnetic thin film sample C with individual layer W resilient coating for preparing in comparative example 1 anneals after 10min under 1000 ℃ of conditions;
Fig. 3 is the situation figure that the Sm-Co base permanent magnetic thin film sample C with double-layer bumper layer for preparing in the embodiment of the present invention 1 anneals after 10min under 1000 ℃ of conditions.
Embodiment
Below by the drawings and specific embodiments, the present invention will be further described, but and do not mean that protection range restriction of the present invention.
Comparative example 1:
The present embodiment is the comparative example of following embodiment 1.
In the present embodiment, matrix selects surface with the thick SiO of 500nm
2si (100) type substrate, i.e. substrate Si/SiO
2(100), SiO
2matrix surface is that thickness is the W resilient coating of 300nm, and W buffer-layer surface is that thickness is the Sm-Co base permanent magnetic thin film of 2 μ m.
The preparation method of the above-mentioned Sm-Co base permanent magnetic thin film with W resilient coating is as follows:
Adopt magnetron sputtering apparatus, using high-purity Ar gas as working gas, base vacuum is better than 6.0 * 10
-6pa, sputter temperature is room temperature, sputtering pressure is 0.5Pa; The W target that the purity of take is 99.99% is W resilient coating target, substrate Si/SiO
2(100) through acetone cleaning and after drying up with nitrogen, at its surface sputtering, deposit W resilient coating, W target power output is 130W, and sputter rate is 14nm/min, approximately deposits 21 minutes, and obtaining thickness is the W resilient coating of 300nm; Then, with Sm (Co, Cu, Fe, Zr)
xcomposite target is the sputtering target material of Sm-Co base permanent magnetic thin film, and at W buffer-layer surface sputter Sm-Co base permanent magnetic thin film, sputtering power is 200W, and sputter rate is 39nm/min, approximately deposits 60 minutes, and obtaining Sm-Co base permanent magnetic thin film thickness is 2 μ m.
By the above-mentioned Sm-Co base permanent magnetic thin film sample A with W resilient coating preparing, B, C annealing in process 10min under 800 ℃, 900 ℃, 1000 ℃ conditions respectively.There is the phenomenon coming off from matrix surface in the sample A annealing as shown in Figure 1, under 800 ℃ of conditions.Coming off of the sample B annealing under 900 ℃ of conditions is more obvious.The obscission of the sample C annealing under 1000 ℃ of conditions is very serious, as shown in Figure 2.
Example 1:
In the present embodiment, identical with above-mentioned comparative example 1, matrix is selected this Si/SiO of substrate
2(100), between matrix and Sm-Co base permanent magnetic thin film, be resilient coating, Sm-Co base permanent magnetic thin film thickness is 2 μ m.Different from above-mentioned comparative example 1, this resilient coating is double-layer structure, and one deck is and is positioned at the copper film layer that matrix surface, thickness are 30nm, and another layer is to be positioned at the W film layer that this copper film layer surface, thickness are 300nm.
The preparation method of the above-mentioned Sm-Co base permanent magnetic thin film with double-layer bumper layer is as follows:
Adopt magnetron sputtering apparatus, using high-purity Ar gas as working gas, base vacuum is better than 6.0 * 10
-6pa, sputter temperature is room temperature, sputtering pressure is 0.5Pa; The W target that the purity of take is 99.99% is W resilient coating target, and the Cu target that purity is 99.95% is Cu resilient coating target, substrate Si/SiO
2(100) through acetone cleaning and after drying up with nitrogen, at its surface sputtering, deposit Cu resilient coating, Cu target power output is 100W, and sputter rate is 15nm/min, approximately deposits 2 minutes, obtains Cu resilient coating 30nm; After deposition, deposit W resilient coating, W target power output is 1W again, and sputter rate is 14nm/min, approximately deposits 21 minutes, and obtaining thickness is the W resilient coating of 300nm; Then, with Sm (Co, Cu, Fe, Zr)
xcomposite target is the sputtering target material of Sm-Co base permanent magnetic thin film, and in the sputter of W buffer-layer surface, sputtering power is 200W, and sputter rate is 39nm/min, approximately deposits 60 minutes, and obtaining thickness is the Sm-Co base permanent magnetic thin film layer of 2 μ m.
By the above-mentioned Sm-Co base permanent magnetic thin film sample A with Cu/W double-layer bumper layer preparing, B, C annealing in process 10min under 800 ℃, 900 ℃, 1000 ℃ conditions respectively.Result demonstration, sample A, the B annealing under 800 ℃, 900 ℃ conditions is combined intact with matrix, obscission does not occur.The sample C even annealing under 1000 ℃ of conditions is still combined intact with matrix, obscission does not occur, as shown in Figure 3.
Embodiment 2:
In the present embodiment, the structure of the Sm-Co base permanent magnetic thin film of matrix surface substantially be identical in embodiment 1.Difference is, the thickness of copper film layer is 100nm, and the thickness of W film layer is 500nm, and Sm-Co base permanent magnetic thin film thickness is 5 μ m.
The preparation method of the above-mentioned Sm-Co base permanent magnetic thin film with double-layer bumper layer is as follows:
Adopt magnetron sputtering apparatus, using high-purity Ar gas as working gas, base vacuum is better than 6.0 * 10
-6pa, sputter temperature is room temperature, sputtering pressure is 0.5Pa; The W target that the purity of take is 99.99% is W resilient coating target, and the Cu target that purity is 99.95% is Cu resilient coating target, substrate Si/SiO
2(100) through acetone cleaning and after drying up with nitrogen, at its surface sputtering, deposit Cu resilient coating, Cu target power output is 100W, and sputter rate is 15nm/min, approximately deposits 7 minutes, obtains Cu resilient coating 100nm; After deposition, deposit W resilient coating, W target power output is 130W again, and sputter rate is 14nm/min, approximately deposits 36 minutes, and obtaining thickness is the W resilient coating of 500nm; Then, with Sm (Co, Cu, Fe, Zr)
xcomposite target is the sputtering target material of Sm-Co base permanent magnetic thin film, and in the sputter of W buffer-layer surface, sputtering power is 200W, and sputter rate is 39nm/min, approximately deposits 128 minutes, and obtaining thickness is the Sm-Co base permanent magnetic thin film layer of 5 μ m.
By the above-mentioned Sm-Co base permanent magnetic thin film sample with Cu/W double-layer bumper layer preparing annealing in process 10min under 800 ℃, 900 ℃, 1000 ℃ conditions respectively.Result shows, Sm-Co base permanent magnetic thin film is combined intact after 800 ℃, 900 ℃ annealing in process with matrix, obscission does not occur, and even after 1000 ℃ of annealing in process, is still combined intactly with matrix, and obscission does not occur.
Embodiment 3:
In the present embodiment, the structure of the Sm-Co base permanent magnetic thin film of matrix surface substantially be identical in embodiment 1.Difference is, the thickness of copper film layer is 10nm, and the thickness of W film layer is 100nm, and Sm-Co base permanent magnetic thin film thickness is 1 μ m.
The preparation method of the above-mentioned Sm-Co base permanent magnetic thin film with double-layer bumper layer is as follows:
Adopt magnetron sputtering apparatus, using high-purity Ar gas as working gas, base vacuum is better than 6.0 * 10
-6pa, sputter temperature is room temperature, sputtering pressure is 0.5Pa; The W target that the purity of take is 99.99% is W resilient coating target, and the Cu target that purity is 99.95% is Cu resilient coating target, substrate Si/SiO
2(100) through acetone cleaning and after drying up with nitrogen, at its surface sputtering, deposit Cu resilient coating, Cu target power output is 100W, and sputter rate is 15nm/min, approximately deposits 1 minute, obtains Cu resilient coating 10nm; After deposition, deposit W resilient coating, W target power output is 130W again, and sputter rate is 14nm/min, approximately deposits 7 minutes, and obtaining thickness is the W resilient coating of 100nm; Then, with Sm (Co, Cu, Fe, Zr)
xcomposite target is the sputtering target material of Sm-Co base permanent magnetic thin film, and in the sputter of W buffer-layer surface, sputtering power is 200W, and sputter rate is 39nm/min, approximately deposits 30 minutes, and obtaining thickness is the Sm-Co base permanent magnetic thin film layer of 1 μ m.
By the above-mentioned Sm-Co base permanent magnetic thin film sample with Cu/W double-layer bumper layer preparing annealing in process 10min under 800 ℃, 900 ℃, 1000 ℃ conditions respectively.Result shows, Sm-Co base permanent magnetic thin film is combined intact after 800 ℃, 900 ℃ annealing in process with matrix, obscission does not occur, and even after 1000 ℃ of annealing in process, is still combined intactly with matrix, and obscission does not occur.
Above-described embodiment has been described in detail technical scheme of the present invention and beneficial effect; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making within the scope of principle of the present invention and improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
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| CN106252022A (en) * | 2016-08-04 | 2016-12-21 | 浙江理工大学 | A kind of Sm Co base permanent magnetic thin film and preparation method thereof |
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