CN102683003A - Method for preparing single-shaft magnetic anisotropy thin film - Google Patents
Method for preparing single-shaft magnetic anisotropy thin film Download PDFInfo
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- CN102683003A CN102683003A CN2012101348658A CN201210134865A CN102683003A CN 102683003 A CN102683003 A CN 102683003A CN 2012101348658 A CN2012101348658 A CN 2012101348658A CN 201210134865 A CN201210134865 A CN 201210134865A CN 102683003 A CN102683003 A CN 102683003A
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Abstract
The invention discloses a method for preparing a single-shaft magnetic anisotropy thin film. By means of the method, a substrate with anisotropy coefficients of thermal expansion is chosen and installed on a heater, and a temperature sensor is installed on the heater, so that the heater and the temperature sensor form a closed-loop feedback circuit; the substrate is heated to the preset temperature so that the substrate is expanded or contracted due to heating; and a magnetic thin film grows on the expanded or contracted substrate through a magnetron sputtering or pulse laser deposition method, then the temperature of the substrate is cooled to the room temperature, and the substrate is contracted or expanded, so that certain pressure stress or tension stress can be generated on the magnetic thin film, and the single-shaft magnetic anisotropy thin film can be obtained. Compared with the prior art, the method for preparing the single-shaft magnetic anisotropy thin film is simple and ingenious in structural design, can achieve the aim of controlling single-shaft magnetic anisotropy by controlling the temperature of the substrate and has good industrial application prospect.
Description
Technical field
The present invention relates to the preparation field of magnetic thin film in high-frequency electromagnetic device, the magnetic sensor device, especially relate to a kind of preparation method of uniaxial magnetic anisotropy film.
Background technology
Fast development along with magnetic material and technology of preparing; Magnetic device plays more and more important effect at information technology, sensory field, and its range of application relates to magnetic recording head, Magnetic Sensor, magnetic circuit, miniature inductance device, transformer, magnetic microwave device etc.For these magnetic devices, its core material is a magnetic thin film.When magnetic device was applied to the high frequency field, people needed magnetic thin film to have little coercive force, high saturation magnetization, high magnetic permeability and ferromagnetic resonance frequency.Yet high magnetic permeability and high ferromagnetic resonance frequency generally are difficult to obtain simultaneously, and they are all closely related with the in-plane mono-axial magnetic anisotropy of magnetic thin film.Magnetic permeability reduces along with the increase of uniaxial magnetic anisotropy; Ferromagnetic resonance frequency increases along with the increase of uniaxial magnetic anisotropy.Therefore,, select a sizeable in-plane mono-axial magnetic anisotropy for different applications, the relation between good magnetic permeability of balance and the ferromagnetic resonance frequency, the magnetic device that has good frequency response for acquisition is crucial.
The method of acquisition in-plane mono-axial magnetic anisotropy commonly used is the induced by magnetic field method at present, that is, when film growth, provide an online induced by magnetic field magnetic thin film to obtain the uniaxial magnetic anisotropy in the face.The shortcoming of this method is: the magnetic field that (1) applies is fixed often, is unfavorable for obtaining magnetic anisotropy in the best face; (2) magnetic anisotropy of inducing and the relation between the induced magnetic field are difficult to quantification; (3) for the Ferrite Material that needs the high temperature preparation, the induced magnetic field device there is higher requirement, such as, needing higher Curie temperature etc., this also can increase the cost of equipment greatly.In addition, patent CN 101429646A discloses a kind of preparation method who produces the in-plane mono-axial magnetism anisotropic film under the induced magnetic field that do not have, and this method obtains the uniaxial magnetic anisotropy in the face through rotary sample; The preparation of this method is fairly simple, but controllability is relatively poor, especially when preparation temperature changes, is difficult to the anisotropic situation of change of prediction in-plane mono-axial.
Summary of the invention
Technical purpose of the present invention is the deficiency to above-mentioned prior art, and a kind of preparation method of uniaxial magnetic anisotropy film is provided, and utilizes this method can realize the film that the in-plane mono-axial magnetic anisotropy is controlled.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is: a kind of preparation method of uniaxial magnetic anisotropy film comprises the steps:
Step 1: the substrate (as shown in Figure 1, promptly substrate is different with the thermal coefficient of expansion of Y direction along directions X) that will have the anisotropic thermal expansion coefficient is placed on the heater mounting temperature sensor on the described heater;
Step 2: through the heater heats substrate, utilize this heating-up temperature of temperature sensor monitors and it is fed back to heater, make heater, temperature sensor constitute closed feedback loop, heated substrate is to preset temperature;
Step 3: the maintenance underlayer temperature is a preset temperature, utilizes method even growth magnetic thin film on the substrate after the thermal expansion of magnetron sputtering or pulsed laser deposition;
Step 4: treat that the magnetic thin film growth finishes, underlayer temperature is reduced to room temperature, promptly obtain the uniaxial magnetic anisotropy film.
In the technique scheme:
Described substrate is selected the substrate with anisotropic thermal expansion coefficient for use; Be that substrate is different with the thermal coefficient of expansion of Y direction along directions X, this substrate includes but not limited to single crystalline substrate, ceramic substrate, metal substrate, organic substance substrate, plastic, ferroelectric substrate etc.
The uniformity of the magnetic thin film that deposits in order to improve; Preferably described heater is installed on the rotating shaft, during depositing magnetic film, at first opens rotating shaft and rotate; The drive heater is rotated, thereby makes the substrate depositing magnetic film in rotation that is arranged on the heater.Preferred as further; Through at the bottom of the external fixator reinforcing line with the friction of heater; Thereby improve the rotation consistency of substrate and heater, for example can select for use but be not limited to the mode that screw combines with compressing tablet, soon compressing tablet one end is fixed on the heater; The compressing tablet other end is gently pressed certain position of substrate, at the bottom of the reinforcing line with the frictional rotation of heater.
Technique scheme is divided following two kinds of patterns according to the actual conditions of thermal coefficient of expansion.
1, when thermal coefficient of expansion be on the occasion of the time
At first, in step 2, during heated substrate to preset temperature, substrate along directions X and the thermal expansion of Y direction to certain position; Then, in step 3, the maintenance underlayer temperature is a preset temperature, utilizes method even growth magnetic thin film on the substrate after the thermal expansion of magnetron sputtering or pulsed laser deposition; At last, treat that in step 4 the magnetic thin film growth finishes, and reduces to room temperature with underlayer temperature; This moment, substrate was contracted to certain position along directions X and Y direction; Because the thermal expansion of substrate is anisotropic, in magnetic thin film, form certain stress distribution like this, such as: the compression that directions X receives is maximum; The compression that the Y direction receives is minimum, thereby in magnetic thin film, obtains being prone to the uniaxial magnetic anisotropy film of axle along directions X;
2, when thermal coefficient of expansion is negative value
At first, in step 2, during heated substrate to preset temperature, substrate is heat-shrinkable to certain position along directions X and Y direction; Then, in step 3, the maintenance underlayer temperature is a preset temperature, utilizes method even growth magnetic thin film on the substrate after the thermal contraction of magnetron sputtering or pulsed laser deposition; At last, treat that in step 4 the magnetic thin film growth finishes, and reduces to room temperature with underlayer temperature; This moment, substrate was expanded to certain position along directions X and Y direction; Because the thermal expansion of substrate is anisotropic, in magnetic thin film, form certain stress distribution like this, such as: the tensile stress that directions X receives is maximum; The tensile stress that the Y direction is received is minimum, thereby in magnetic thin film, obtains being prone to the uniaxial magnetic anisotropy film of axle along directions X;
In sum; The preparation method of uniaxial magnetic anisotropy film provided by the invention utilizes the anisotropic thermal expansion characteristic of substrate; Through substrate temperature control, the magnetic thin film that is grown on the substrate is produced certain compression or tensile stress, thereby obtain controlled uniaxial magnetic anisotropy.Compare with the preparation method of existing uniaxial magnetic anisotropy film, have following beneficial effect:
(1) structural design is simply ingenious, selects the substrate with anisotropic thermal expansion coefficient for use, and it is installed on the heater; Mounting temperature sensor on the heater makes heater, temperature sensor constitute closed feedback loop, and heated substrate is to preset temperature; Make substrate expanded by heating or contraction, utilize rotating shaft to drive the substrate rotation then, the method for utilizing magnetron sputtering or pulsed laser deposition expand or shrink after substrate on the magnetic thin film of growing; At last underlayer temperature is reduced to room temperature; Make the substrate contraction or expansion, thereby magnetic thin film is produced certain compression or tensile stress, obtain the uniaxial magnetic anisotropy film;
(2) compression of magnetic thin film generation or the size and the substrate temperature of tensile stress are varied to direct ratio; The substrate temperature variation can be accurately controlled through the feedback loop of heater, temperature sensor, thereby the size of this compression or tensile stress can be accurately controlled;
(3) the growth temperature interval that is suitable for is wide, process stabilizing, easy operating, be suitable for producing in batches;
Therefore, that the preparation method of a kind of uniaxial magnetic anisotropy film of the present invention has is simple in structure, equipment requirements is low, in the controlled advantage of uniaxial stress, can prepare to have controlled in-plane mono-axial magnetism anisotropic film, has favorable industrial application prospect.
Description of drawings
Fig. 1 is the sketch map of the substrate with anisotropic thermal expansion coefficient selected for use among the preparation method of uniaxial magnetic anisotropy film of the present invention;
Fig. 2 is the substrate mounting structure sketch map of preparation uniaxial magnetic anisotropy FeGa film in the embodiment of the invention 1;
Fig. 3 adopts magnetron sputtering method to prepare the structural representation of uniaxial magnetic anisotropy FeGa film in the embodiment of the invention 1;
Fig. 4 is that the uniaxial magnetic anisotropy FeGa film edge that makes in the embodiment of the invention 1 is prone to a normalization magnetization curve of (directions X) and hard axis (Y direction).
Embodiment
Embodiment does further explain to the present invention below in conjunction with accompanying drawing, it is pointed out that the following stated embodiment is intended to be convenient to understanding of the present invention, and it is not played any qualification effect.
Reference numeral wherein is: heater 1, temperature sensor 2, rotating shaft 3, substrate 4, screw 5, compressing tablet 6, target stand 7, target cover 8, target 9, deposition and atomic group 10.
In the present embodiment, adopt ferroelectric substrate PVDF as substrate 4 materials, as shown in Figure 1, PVDF is-145 * 10 along the thermal coefficient of expansion of directions X
-6K
-1, be-13 * 10 along the thermal coefficient of expansion of Y direction
-6K
-1, the PVDF substrate is because the interior maximum strain of face that causes of heating is-145 * 10
-6* T, minimum strain are-13 * 10
-6* T, wherein T is a temperature.
According to substrate scheme of installation shown in Figure 2, PVDF substrate 4 is placed on the heater 1, this heater 1 is installed on the rotating shaft 3, and on the heater 1 temperature sensor 2 is installed, and heater 1, temperature sensor 2 constitute closed feedback loop.Compressing tablet 6 one ends are fixed on the heater 1 through screw 5, and the other end is gently pressed PVDF substrate 4 along directions X, to strengthen the frictional rotation of PVDF substrate 4 and heater 1.
Adopt magnetron sputtering method on PVDF substrate 4 mounting structures shown in Figure 2, to deposit magnetic Fe Ga film, its structural representation is as shown in Figure 3, and concrete grammar is following.
Step 1: according to installation PVDF substrate 4 shown in Figure 2; Then through heater 1 this PVDF substrate 4 of heating; Utilize temperature sensor 2 these heating-up temperatures of monitoring and it is fed back to heater 1; Make heater 1, TEMP 2 devices constitute closed feedback loop, heating PVDF substrate 4 is to 40 ℃ of preset temperatures, and PVDF substrate 4 is stablized after being heat-shrinkable to certain position.
Step 2: keeping the temperature of PVDF substrate 4 is 40 ℃ of preset temperatures, starts rotating shaft 3, utilizes magnetron sputtering method even growth magnetic Fe Ga film on the PVDF substrate 4 after this thermal contraction; Wherein, target 9 is the FeGa target, and vacuum is 7 * 10 at the bottom of the back of the body of magnetron sputtering
-5Pa, sputtering atmosphere are Ar, and sputter pressure is 1Pa, and direct current sputtering, sedimentation time are 6 minutes, drive 4 rotations of PVDF substrate through rotating shaft 3, and target stand 7,8 on target cover apply voltage, and the deposition FeGa atomic group 10 that sputters deposits on the PVDF substrate 4.
Step 4: treat that magnetic Fe Ga film growth finishes, measuring its thickness is 60nm; Then PVDF substrate 4 temperature are reduced to room temperature (27 ℃), this moment PVDF substrate 4 to certain position, magnetic Fe Ga film is along the tensile strain of directions X about 0.19% along directions X and the thermal expansion of Y direction; Tensile strain along the Y direction is about 0.02%, so, in magnetic Fe Ga film, obtain being prone to the uniaxial magnetic anisotropy film of axle along directions X.
Fig. 4 is that the uniaxial magnetic anisotropy FeGa film edge that makes in the embodiment of the invention 1 is prone to a normalization magnetization curve of (directions X) and hard axis (Y direction).Can find out that this magnetic Fe Ga film has tangible in-plane mono-axial magnetic anisotropy, directions X is an easy magnetizing axis, and the Y direction is a hard axis.
Above-described embodiment specifies technical scheme of the present invention; Be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All any modifications of in principle scope of the present invention, being made, replenish or similar fashion substitutes etc., all should be included within protection scope of the present invention.
Claims (5)
1. the preparation method of a uniaxial magnetic anisotropy film is characterized in that: comprise the steps:
Step 1: the substrate that will have the anisotropic thermal expansion coefficient is placed on the heater, mounting temperature sensor on the described heater;
Step 2: through the heater heats substrate, utilize this heating-up temperature of temperature sensor monitors and it is fed back to heater, make heater, temperature sensor constitute closed feedback loop, heated substrate is to preset temperature;
Step 3: the maintenance underlayer temperature is a preset temperature, utilizes method even growth magnetic thin film on the substrate after the thermal expansion of magnetron sputtering or pulsed laser deposition;
Step 4: treat that the magnetic thin film growth finishes, underlayer temperature is reduced to room temperature, promptly obtain the uniaxial magnetic anisotropy film.
2. the preparation method of uniaxial magnetic anisotropy film according to claim 1; It is characterized in that: described heater is installed on the rotating shaft; When in step 3, growing magnetic thin film, at first open rotating shaft and rotate, magnetic thin film thereby the drive substrate is grown in rotation.
3. the preparation method of uniaxial magnetic anisotropy film according to claim 2 is characterized in that: described substrate is through the friction between external fixator increase and heater.
4. the preparation method of uniaxial magnetic anisotropy film according to claim 3 is characterized in that: described external fixator is made up of screw and compressing tablet, and on heater, the other end is gently pressed substrate one end to compressing tablet one end through screw.
5. according to the preparation method of the described uniaxial magnetic anisotropy film of arbitrary claim in the claim 1 to 4, it is characterized in that: described substrate comprises single crystalline substrate, ceramic substrate, metal substrate, organic substance substrate, plastic or ferroelectric substrate.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104064350A (en) * | 2014-06-27 | 2014-09-24 | 中国科学院宁波材料技术与工程研究所 | Preparation method of magnetic film with positive magnetic anisotropy temperature coefficient |
CN110246673A (en) * | 2019-07-22 | 2019-09-17 | 蚌埠市正园电子科技有限公司 | A kind of gluing device and its encapsulation methods for high frequency transformer |
CN113406541A (en) * | 2021-06-18 | 2021-09-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Resonant type double-shaft magnetic sensor and double-shaft magnetic sensor testing system |
CN115612988A (en) * | 2022-10-18 | 2023-01-17 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof |
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JPS62238614A (en) * | 1986-04-09 | 1987-10-19 | Fujitsu Ltd | Manufacture of anistropic magnetic film |
CN1890587A (en) * | 2003-12-18 | 2007-01-03 | 日东电工株式会社 | Method and device for transferring anisotropic crystal film from donor to receptor, and the donor |
CN101206945A (en) * | 2007-11-20 | 2008-06-25 | 福建师范大学 | Method of preparing multi-component high-frequency thin ferromagnetic film material with component gradient |
CN201151740Y (en) * | 2007-11-22 | 2008-11-19 | 福建师范大学 | Gradient sputtering apparatus for preparing film material with compositional gradient |
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JPS62238614A (en) * | 1986-04-09 | 1987-10-19 | Fujitsu Ltd | Manufacture of anistropic magnetic film |
CN1890587A (en) * | 2003-12-18 | 2007-01-03 | 日东电工株式会社 | Method and device for transferring anisotropic crystal film from donor to receptor, and the donor |
CN101206945A (en) * | 2007-11-20 | 2008-06-25 | 福建师范大学 | Method of preparing multi-component high-frequency thin ferromagnetic film material with component gradient |
CN201151740Y (en) * | 2007-11-22 | 2008-11-19 | 福建师范大学 | Gradient sputtering apparatus for preparing film material with compositional gradient |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104064350A (en) * | 2014-06-27 | 2014-09-24 | 中国科学院宁波材料技术与工程研究所 | Preparation method of magnetic film with positive magnetic anisotropy temperature coefficient |
CN110246673A (en) * | 2019-07-22 | 2019-09-17 | 蚌埠市正园电子科技有限公司 | A kind of gluing device and its encapsulation methods for high frequency transformer |
CN110246673B (en) * | 2019-07-22 | 2023-10-13 | 蚌埠市正园电子科技股份有限公司 | Rubber coating device for high-frequency transformer and rubber coating method thereof |
CN113406541A (en) * | 2021-06-18 | 2021-09-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Resonant type double-shaft magnetic sensor and double-shaft magnetic sensor testing system |
CN113406541B (en) * | 2021-06-18 | 2023-03-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Resonant type double-shaft magnetic sensor and double-shaft magnetic sensor testing system |
CN115612988A (en) * | 2022-10-18 | 2023-01-17 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof |
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Application publication date: 20120919 |