CN104064350B - A kind of preparation method of the thin magnetic film with positive magnetic anisotropy temperature coefficient - Google Patents
A kind of preparation method of the thin magnetic film with positive magnetic anisotropy temperature coefficient Download PDFInfo
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Abstract
The invention provides a kind of preparation method of the thin magnetic film with positive magnetic anisotropy temperature coefficient. The method is selected the substrate with anisotropic thermal expansion coefficient, first along the larger direction of the absolute value of thermal coefficient of expansion, this substrate is applied to certain and strain thermal expansion opposite direction, and described strain value is greater than the strain value that substrate produces in the time that temperature drops to thin magnetic film minimum operating temperature from room temperature, under this strain conservation condition at substrate surface growth thin magnetic film, treat to remove this strain after Magnetic Thin Film Growth Process, obtain the thin magnetic film of magnetic anisotropy. Along with the increase of temperature, the magnetic anisotropy of this magnetic membrane material increases, and has positive magnetic anisotropy temperature coefficient, has great importance for the heat endurance that improves thin magnetic film device.
Description
Technical field
The present invention relates to the preparation field of thin magnetic film in high-frequency electromagnetic device, microwave device, magnetic sensor device, especiallyRelate to a kind of preparation method of the thin magnetic film with positive magnetic anisotropy temperature coefficient.
Background technology
Magnetic anisotropy is a basic parameter of magnetic material, and its size has determined the magnetic moment energy potential that need to overcome that overturnsBuild. Along with the fast development of spintronics, thin magnetic film is widely used in magnetic storage, magnetic sensing, microwave deviceIn, play irreplaceable effect for the development of Information technology. For these thin magnetic film devices, magnetic anisotropy existsWherein bring into play important effect, such as: in magnetic storage field, along with the raising of magnetic recording density, each magnetic recording listThe size of unit, dwindling gradually, just need to increase the magnetic anisotropy of magnetic recording unit in order to overcome the impact of thermal agitation;In Magnetic Sensor, the size of magnetic anisotropy has directly determined sensitivity and the linear work interval of sensor; At microwaveIn device, the size of magnetic anisotropy has determined the size of resonant frequency, and then has determined operating point and the work frequency of deviceRate scope.
As everyone knows, heat endurance is the basic parameter of above-mentioned thin magnetic film device, in order to ensure that device is in certain temperatureIn scope, can normally work, device must have good heat endurance. But any physical parameter has certainTemperature dependent properties, magnetic anisotropy is no exception. In general, the rising of temperature causes the intensity of magnetization of thin magnetic filmDecline, and then cause magnetic anisotropy to reduce. In addition, the rising of temperature often also can cause that thin magnetic film is coercitive to fallLow. The phenomenon that this magnetic anisotropy declines with the rising of temperature shows that thin magnetic film has negative magnetic anisotropy temperature and isNumber. Negative magnetic anisotropy temperature coefficient causes required energy barrier reduction, the coercivity reduction etc. overcoming of magnetic moment upset, noBe beneficial to the thermally-stabilised of device.
Therefore,, how by structure or preparation method's improvement, obtain magnetic anisotropy and keep not with the rising of temperatureBecome the thin magnetic film even improving, this thin magnetic film has positive magnetic anisotropy temperature coefficient, to thin magnetic film deviceHeat endurance has great importance.
Summary of the invention
The present invention is directed to the thin magnetic film that existing preparation method obtains and often there is asking of negative magnetic anisotropy temperature coefficientTopic, aims to provide a kind of preparation method of thin magnetic film, utilizes the method can obtain having positive magnetic anisotropy temperature systemThe thin magnetic film of number, has great importance for the heat endurance that improves thin magnetic film device.
In order to realize above-mentioned technical purpose, the inventor finds after great many of experiments is explored, when the magnetic of growing at substrate surfaceWhen property film (this thin magnetic film has Magnetostriction, comprises direct magnetostriction performance and negative magnetostriction performance),Select the there is anisotropic thermal expansion coefficient substrate of (comprising positive thermal coefficient of expansion and negative thermal coefficient of expansion), firstAlong the larger direction of the absolute value of thermal coefficient of expansion, this substrate is applied to certain and strain thermal expansion opposite direction, that is,In the time that substrate has positive thermal coefficient of expansion, the direction larger along thermal coefficient of expansion applies certain compressive strain to substrate;In the time that substrate has negative thermal coefficient of expansion, the direction larger along thermal coefficient of expansion absolute value applies tensile strain to substrate,Under this strain conservation condition, at substrate surface growth thin magnetic film, treat to remove this strain after Magnetic Thin Film Growth Process,This thin magnetic film concrete manifestation is as follows:
(1) thin magnetic film is direct magnetostriction material, and substrate has positive thermal coefficient of expansion
In the time of this substrate surface growth thin magnetic film, should to undercoat pressurization along the direction that substrate thermal coefficient of expansion is largerBecome, after film growth finishes, remove this compressive strain, thin magnetic film bears the tensile strain from substrate, its easy magnetizing axis edgeThe direction that substrate thermal coefficient of expansion is larger, accordingly, its hard axis is perpendicular to the larger direction of substrate thermal coefficient of expansion,Along the less direction of substrate thermal coefficient of expansion, as shown in table 1 below;
In the time that temperature raises, contrast the remanent magnetism of this thin magnetic film, find that (thermal coefficient of expansion is larger along easy axisDirection) remanent magnetism increase gradually with the difference along the remanent magnetism of hard axis direction (direction that thermal coefficient of expansion is less),,, along with the rising of temperature, the magnetic anisotropy of this thin magnetic film strengthens, and presents positive magnetic anisotropy temperature coefficient.
(2) thin magnetic film is direct magnetostriction material, and substrate has negative thermal coefficient of expansion
In the time of this substrate surface growth thin magnetic film, along the larger direction of substrate thermal coefficient of expansion absolute value, substrate is appliedTensile strain, after film growth finishes, removes this tensile strain, and thin magnetic film bears the compressive strain from substrate, its easy magnetizationAxle is along the less direction of substrate thermal coefficient of expansion absolute value, perpendicular to the larger direction of substrate thermal coefficient of expansion absolute value,Accordingly, its hard axis is along the larger direction of substrate thermal coefficient of expansion absolute value, as shown in table 1 below;
In the time that temperature raises, contrast the remanent magnetism of this thin magnetic film, along easy axis, (thermal coefficient of expansion absolute value isLittle direction) remanent magnetism and difference along the remanent magnetism of hard axis direction (direction that thermal coefficient of expansion absolute value is larger)Increase gradually, that is, along with the rising of temperature, the magnetic anisotropy of this thin magnetic film strengthens, and presents positive magnetic anisotropy temperatureDegree coefficient.
(3) thin magnetic film is negative magnetostriction material, and substrate has positive thermal coefficient of expansion
In the time of this substrate surface growth thin magnetic film, should to undercoat pressurization along the direction that substrate thermal coefficient of expansion is largerBecome, after film growth finishes, remove this compressive strain, thin magnetic film bears the tensile strain from substrate, its easy magnetizing axis edgeThe direction that substrate thermal coefficient of expansion is less, perpendicular to the larger direction of substrate thermal coefficient of expansion, accordingly, its difficult magneticChange axle along the larger direction of substrate thermal coefficient of expansion, as shown in table 1 below;
In the time that temperature raises, contrast the remanent magnetism of this thin magnetic film, find that (thermal coefficient of expansion is less along easy axisDirection) remanent magnetism increase gradually with the difference along the remanent magnetism of hard axis direction (direction that thermal coefficient of expansion is larger),,, along with the rising of temperature, the magnetic anisotropy of this thin magnetic film strengthens, and presents positive magnetic anisotropy temperature coefficient.
(4) thin magnetic film is negative magnetostriction material, and substrate has negative thermal coefficient of expansion
In the time of this substrate surface growth thin magnetic film, along the larger direction of substrate Coefficient of Thermal Expansion value, substrate is applied to open and answerBecome, after film growth finishes, remove this tensile strain, thin magnetic film bears the compressive strain from substrate, its easy magnetizing axis edgeThe direction that substrate thermal coefficient of expansion absolute value is larger, accordingly, its hard axis is absolute perpendicular to substrate thermal coefficient of expansionBe worth larger direction, along the less direction of substrate thermal coefficient of expansion, as shown in table 1 below;
In the time that temperature raises, contrast the remanent magnetism of this thin magnetic film, find that (thermal coefficient of expansion is absolute along easy axisBe worth larger direction) remanent magnetism with along the remanent magnetism of hard axis direction (direction that thermal coefficient of expansion absolute value is less)Difference increases gradually, that is, along with the rising of temperature, the magnetic anisotropy of this thin magnetic film strengthens, and presents positive magnetic respectively to differentProperty temperature coefficient.
Table 1: the deformation type applying when the substrate combination of different magnetostriction materials and different heat expansion performance and easily magneticChange the direction list of axle;
Therefore, while carrying out according to the method described above the growth of thin magnetic film, no matter just or negative magnetostriction material with just orHow the substrate of negative expansion coefficient combines, and in the time that temperature raises, the uniaxial magnetic anisotropy of thin magnetic film all increases,Be that composite magnetic sheet has positive magnetic anisotropy temperature coefficient; In addition, in the time that temperature raises, magnetic field is along easy magnetizing axis,Coercivity also increases, and this is conducive to the heat endurance of high temperature magnetic device.
, the technical solution adopted in the present invention is: a kind of preparation of the thin magnetic film with the different property of positive magnetic temperature coefficientMethod, described thin magnetic film is to make in substrate surface growth, comprises the steps:
Step 1: described substrate has anisotropic thermal expansion coefficient, as shown in Figure 1, substrate hangs down mutually along a certainStraight directions X is different from the thermal coefficient of expansion of Y-direction; In directions X and Y-direction, along thermal coefficient of expansion definitelyThe direction that value is larger applies strain to this substrate, specific as follows:
In the time that substrate has positive thermal coefficient of expansion, the direction larger along thermal coefficient of expansion adds compressive strain to undercoat, forMake prepared thin magnetic film all present positive magnetic anisotropy temperature coefficient in whole operating temperature interval, as preferably,Described compressive strain value is greater than with reference to strain value, and the method for testing of described reference strain value is: at described thin magnetic filmOperating temperature interval, selecting minimum operating temperature is probe temperature, in the time that temperature drops to this probe temperature from room temperature,The strain value that described substrate generation thermal expansion or thermal contraction produce;
In the time that substrate has negative thermal coefficient of expansion, along the larger direction of thermal coefficient of expansion absolute value, substrate is applied to open and answerBecome, in order to make prepared thin magnetic film all present positive magnetic anisotropy temperature coefficient in whole operating temperature interval, asPreferably, described tensile strain value is greater than with reference to strain value, and the method for testing of described reference strain value is: at described magneticThe operating temperature interval of property film, selecting minimum operating temperature is probe temperature, when temperature drops to this test from room temperatureWhen temperature, the strain value that described substrate generation thermal expansion or thermal contraction produce;
Step 2: under room temperature, keep substrate to apply the strain described in step (1), substrate surface growth describedThin magnetic film;
Step 3: treat that described Magnetic Thin Film Growth Process is complete, remove the strain described in step (1) and (comprise described pressureStrain and tensile strain), obtain having the thin magnetic film of uniaxial magnetic anisotropy.
In technique scheme:
Described substrate is selected the substrate with anisotropic thermal expansion coefficient, and substrate is along a certain orthogonal directions XDifferent from the thermal coefficient of expansion of Y-direction. This substrate includes but not limited to single crystalline substrate, ceramic substrate, metal substrate, hasMachine thing substrate, plastic supporting base, ferroelectric substrate etc., as preferably, select flexible organic matter substrate.
Described thin magnetic film is not limit, and comprises magnetic metal Fe, Co, Ni, magnetic alloy Fe-Ni, Fe-Ga, Co-Fe-B,Magnetic oxide Fe3O4、La-Sr-Mn-O3Film etc.
In described step 1, applying of strain, comprises that the mode that applies of tensile strain or compressive strain is not limit, wherein a kind ofThe mode of applying is substrate to be placed on to bending convex mold or negative mold realizes, and this convex mold or negative mold produceStrain is t/2r, and wherein t is the thickness of thin magnetic film and substrate, the radius of curvature that r is mould.
In described step 2, the growing method of thin magnetic film is not limit, and comprises the method for magnetron sputtering or pulsed laser depositionDeng.
In sum, the present invention by direct magnetostriction material or negative magnetostriction material with have positive thermal coefficient of expansion orThe substrate of negative expansion coefficient combines, and during by growth magnetic material, substrate is applied to strain, and growth finishes recession and goesThis strain, can effectively control this thin magnetic film and have initial magnetic anisotropy; By controlling this strain value, it is greater thanSubstrate generation thermal expansion when temperature drops to the minimum operating temperature of this thin magnetic film in operating temperature interval from room temperatureThe strain value producing, can effectively control the initial magnetic anisotropy of this magnetic membrane material in operation temperature area; And then,Along with the increase of temperature, the magnetic anisotropy of this magnetic membrane material increases, and has positive magnetic anisotropy temperature coefficient;In addition, this preparation method is simply easy to control, therefore a kind of preparation method with application prospect, and for improving, magnetic is thinThe heat endurance of membrane module has great importance.
Brief description of the drawings
Fig. 1 is the substrate signal with anisotropic thermal expansion coefficient selected in thin magnetic film preparation method of the present inventionFigure;
Fig. 2 is that the normalization remanent magnetism variation with temperature of the CoFeB/PVDF thin magnetic film in the embodiment of the present invention 1 is closedSystem.
Fig. 3 is the normalization remanent magnetism variation with temperature relation of the Ni/PVDF thin magnetic film in the embodiment of the present invention 2.
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiment is described in further detail the present invention, it is pointed out that the following stated embodimentBe intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
Embodiment 1:
In the present embodiment, adopt Organic Iron electric material PVDF as anisotropic thermal expansion substrate, its thickness is 30 μ m.As shown in Figure 1, PVDF has negative anisotropic thermal expansion coefficient, 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, in the face that PVDF substrate causes owing to heating, maximum strain is-145×10-6× T, minimum strain is-13 × 10-6× T, wherein T is temperature.
The magnetic CoFeB material in this substrate surface growth with direct magnetostriction coefficient, its thickness is 60nm. This magneticProperty material operating temperature interval be-60 degree to 60 degree, room temperature is 27 degree. Concrete preparation method comprises the steps:
Step 1: in the operating temperature interval of this magnetic CoFeB material, selecting minimum operating temperature-60 degree is testTemperature, in the time that temperature drops to this probe temperature from room temperature (27 DEG C), the heat that PVDF substrate produces along directions XExpansion strain is 1.3%, and this strain value 1.3% is set to directions X with reference to strain value, and the heat producing along Y-direction is swollenSwollen strain is 0.11%, and this strain value 0.11% is set to Y-direction with reference to strain value.
Along directions X, substrate is applied to tensile strain, the strain value that substrate is produced is greater than directions X with reference to strain value 1.3%,In the present embodiment, selecting this tensile strain value is 1.5%. This tensile strain is by being placed on substrate in bending convex mold to come in factExisting.
The strain producing according to t/2r estimation convex mold, wherein t is the thickness of thin magnetic film and substrate, the curvature that r is mouldRadius. Because tensile strain value is 1.5%, the radius of curvature that obtains convex mold is 1mm.
, by PVDF along directions X bending having in the convex mold of 1mm radius of curvature.
Step 2: under room temperature, keep PVDF substrate to apply the tensile strain described in step 1, utilize magnetron sputtering methodAt this PVDF substrate surface magnetic CoFeB film of evenly growing, concrete technology parameter is: the back end of magnetron sputtering is trueSky is 7 × 10-5Pa, sputtering atmosphere is Ar, sputtering pressure is 0.5Pa, d.c. sputtering 35W, sedimentation time is 6 pointsClock;
Step 3: treat that magnetic CoFeB film growth is complete, remove this convex mold, at room temperature obtain thering is uniaxial magnetic eachHeterotropic magnetic CoFeB film, and its easy magnetizing axis is along Y-direction.
Respectively by magnetic direction along directions X and Y-direction, the remanent magnetism of testing the above-mentioned magnetic CoFeB film making withThe variation relation of temperature, test result as shown in Figure 2. As can see from Figure 2, when magnetic field is during along Y-direction, withThe rising of temperature, the remanent magnetism of this magnetic CoFeB film increases gradually; On the contrary, when magnetic field is during along directions X, withThe rising of temperature, the remanent magnetism of this magnetic CoFeB film reduces gradually; ,, along with the rising of temperature, magnetic field is along YThe remanent magnetism of direction and magnetic field increase gradually along the difference of the remanent magnetism of directions X, and this explanation is along with the rising of temperature, this magneticThe magnetic anisotropy of CoFeB film, strengthening, have positive magnetic anisotropy temperature coefficient, and its easy magnetizing axis is in Y-axisDirection.
Embodiment 2:
In the present embodiment, adopt Organic Iron electric material PVDF as anisotropic thermal expansion substrate, its thickness is 30 μ m.As shown in Figure 1, PVDF has negative anisotropic thermal expansion coefficient, 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, in the face that PVDF substrate causes owing to heating, maximum strain is-145×10-6× T, minimum strain is-13 × 10-6× T, wherein T is temperature.
The magnetic Ni material in this substrate surface growth with negative magnetostriction coefficient, its thickness is 60nm. This magnetic materialMaterial operating temperature interval be-60 spend to 60 degree, room temperature is 27 degree. Concrete preparation method comprises the steps:
Step 1: in the operating temperature interval of this magnetic Ni material, selecting minimum operating temperature-60 degree is probe temperature,In the time that temperature drops to this probe temperature from room temperature (27 DEG C), the thermal expansion that PVDF substrate produces along directions X shouldBecome 1.3%, this strain value 1.3% is set to directions X with reference to strain value, the thermal expansion strain producing along Y-directionBe 0.11%, this strain value 0.11% is set to Y-direction with reference to strain value.
Along directions X, substrate is applied to tensile strain, the strain value that substrate is produced is greater than directions X with reference to strain value 1.3%,In the present embodiment, selecting this tensile strain value is 1.5%. This tensile strain is by being placed on substrate in bending convex mold to come in factExisting.
The strain producing according to t/2r estimation convex mold, wherein t is the thickness of thin magnetic film and substrate, the curvature that r is mouldRadius. Because tensile strain value is 1.5%, the radius of curvature that obtains convex mold is 1mm.
, by PVDF along directions X bending having in the convex mold of 1mm radius of curvature.
Step 2: under room temperature, keep PVDF substrate to apply the tensile strain described in step 1, utilize magnetron sputtering methodAt this PVDF substrate surface magnetic Ni film of evenly growing, concrete technology parameter is: the back end vacuum of magnetron sputtering is7×10-5Pa, sputtering atmosphere is Ar, sputtering pressure is 0.6Pa, d.c. sputtering 45W, sedimentation time is 5 minutes;
Step 3: treat that magnetic Ni film growth is complete, remove this convex mold, at room temperature obtain having uniaxial magnetic respectively to differentThe magnetic Ni film of property, and its easy magnetizing axis is along directions X.
Respectively by magnetic direction along directions X and Y-direction, test the remanent magnetism of the above-mentioned magnetic Ni film making with temperatureVariation relation, test result is as shown in Figure 3. As can see from Figure 3, when magnetic field is during along directions X, along with temperatureThe rising of degree, the remanent magnetism of this magnetic Ni film increases gradually; On the contrary, when magnetic field is during along Y-direction, along with temperatureRaise, the remanent magnetism of this magnetic Ni film reduces gradually; ,, along with the rising of temperature, magnetic field is along the remanent magnetism of directions XIncrease gradually along the difference of the remanent magnetism of Y-direction with magnetic field, this explanation is along with the rising of temperature, the magnetic of this magnetic Ni filmAnisotropy, strengthening, have positive magnetic anisotropy temperature coefficient, and its easy magnetizing axis is in X-direction.
Above-described embodiment has been described in detail technical scheme of the present invention, is understood that and the foregoing is onlySpecific embodiments of the invention, are not limited to the present invention, all any amendments of making within the scope of principle of the present invention,Supplementary or similar fashion is alternative etc., within all should being included in protection scope of the present invention.
Claims (4)
1. there is a preparation method for the thin magnetic film of positive magnetic anisotropy temperature coefficient, described thin magnetic film beSubstrate surface growth makes, and it is characterized in that: comprise the steps:
Step (1): described substrate has anisotropic thermal expansion coefficient, along a certain mutually perpendicular directions X and YThe thermal coefficient of expansion difference of direction; In directions X and Y-direction, along the larger direction pair of the absolute value of thermal coefficient of expansionThis substrate applies strain, specific as follows:
In the time that substrate has positive thermal coefficient of expansion, the direction larger along thermal coefficient of expansion adds compressive strain to undercoat, instituteThe compressive strain value of stating is greater than with reference to strain value, and the method for testing of described reference strain value is: at described thin magnetic filmOperating temperature interval, selecting minimum operating temperature is probe temperature, in the time that temperature drops to this probe temperature from room temperature,Test the strain value that described substrate generation thermal expansion or thermal contraction produce;
In the time that substrate has negative thermal coefficient of expansion, along the larger direction of thermal coefficient of expansion absolute value, substrate is applied to open and answerBecome, described tensile strain value is greater than with reference to strain value, and the method for testing of described reference strain value is: in described magneticThe operating temperature interval of film, selecting minimum operating temperature is probe temperature, when temperature drops to this test temperature from room temperatureWhile spending, test the strain value that described substrate generation thermal expansion or thermal contraction produce;
Step (2): under room temperature, keep substrate to apply the strain described in step (1), in substrate surface growth instituteThe thin magnetic film of stating;
Step (3): treat that described Magnetic Thin Film Growth Process is complete, remove the strain described in step (1), obtain toolThere is the thin magnetic film of uniaxial magnetic anisotropy.
2. the preparation method of a kind of thin magnetic film with positive magnetic anisotropy temperature coefficient according to claim 1,It is characterized in that: described substrate comprise single crystalline substrate, ceramic substrate, metal substrate, organic matter substrate, plastic supporting base orFerroelectric substrate.
3. the preparation method of a kind of thin magnetic film with positive magnetic anisotropy temperature coefficient according to claim 1,It is characterized in that: described thin magnetic film comprises magnetic metal, magnetic alloy or magnetic oxide; Described magnetic metalComprise Fe, Co or Ni, described magnetic alloy comprises Fe-Ni, Fe-Ga or Co-Fe-B, described magnetic oxideComprise Fe3O4Or La-Sr-Mn-O3。
4. the preparation method of a kind of thin magnetic film with positive magnetic anisotropy temperature coefficient according to claim 1,It is characterized in that: in described step (1), by substrate being placed on to convex mold or negative mold applies strain to substrate,The strain that described convex mold or negative mold produce is t/2r, and wherein t is the thickness of thin magnetic film and substrate, and r is mouldRadius of curvature.
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