CN114438448A - Magnetostrictive composite film for enhancing eddy current loss inhibition efficiency and preparation method thereof - Google Patents
Magnetostrictive composite film for enhancing eddy current loss inhibition efficiency and preparation method thereof Download PDFInfo
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- 230000002708 enhancing effect Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010408 film Substances 0.000 claims abstract description 129
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 238000000151 deposition Methods 0.000 claims abstract description 33
- 239000010409 thin film Substances 0.000 claims abstract description 21
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910003910 SiCl4 Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 3
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- 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
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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
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention provides a magnetostrictive composite film for enhancing eddy current loss inhibition efficiency and a preparation method thereof, wherein the preparation method comprises the following steps: cleaning and drying the substrate, and then pre-cleaning the substrate by using plasma under a vacuum condition; depositing a FeGaB magnetostrictive film layer on the surface of the substrate after pre-cleaning, and then depositing Al on the surface of the FeGaB magnetostrictive film layer2O3An insulating thin film layer; repeating the above operation to obtain the FeGaB magnetostrictive film layer and Al2O3Composite films with insulating film layers alternately arranged; to pairAnd etching the prepared composite film to prepare the magnetostrictive composite film. The composite membrane can effectively solve the problems of low eddy current loss inhibition efficiency and easy degradation of magnetostrictive characteristics of the existing magnetostrictive composite membrane.
Description
Technical Field
The invention belongs to the technical field of magnetostrictive films, and particularly relates to a magnetostrictive composite film for enhancing eddy current loss inhibition efficiency and a preparation method thereof.
Background
The magnetostrictive film is a metal functional film with high magnetostrictive characteristic and excellent mechanical property, and is widely applied to various magnetoelectric devices. However, due to its high electrical conductivity, severe eddy current loss is generated inside the material under high frequency conditions, which greatly limits the potential application of the magnetostrictive film in radio frequency devices. At present, researches show that the soft magnetic property of the magnetic film can be effectively improved and the eddy current loss in the magnetic film can be inhibited by inserting the insulating layer into the magnetic film; however, in the conventional method, the thicker the thickness of the inserted insulating layer is, the more the number of layers is, the more the suppression effect on the eddy current loss is significant, but the inserted insulating layer may destroy the mutual coupling action between the magnetic domains in the magnetic thin film, which may cause the deterioration of the magnetostrictive characteristic.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a magnetostrictive composite film for enhancing the eddy current loss inhibition efficiency and a preparation method thereof, and the composite film can effectively solve the problems of low eddy current loss inhibition efficiency and easy degradation of magnetostrictive characteristics of the conventional magnetostrictive composite film.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a magnetostrictive composite film for enhancing eddy current loss inhibition efficiency comprises the following steps:
(1) cleaning and drying the substrate, and then pre-cleaning the substrate by using plasma under a vacuum condition;
(2) depositing a FeGaB magnetostrictive film layer on the surface of the substrate pre-cleaned in the step (1), and then depositing Al on the surface of the FeGaB magnetostrictive film layer2O3An insulating thin film layer;
(3) repeating the operation in the step (2) to obtain the FeGaB magnetostrictive thin film layer and Al2O3Composite films with insulating film layers alternately arranged;
(4) and (4) etching the composite film prepared in the step (3) to prepare the magnetostrictive composite film.
Further, in the step (1), the substrate is subjected to ultrasonic cleaning for 5-10min by using acetone, alcohol and pure water in sequence.
Further, in step (1), the reaction is carried out at 3-5X 10-4Plasma treatment is carried out for 4-8min under the conditions of Pa vacuum, 180-200W radio frequency power and 0.4-0.6Pa air pressure.
Further, the deposition thickness of the FeGaB magnetostrictive thin film layer in the step (2) is 140-160 nm.
Further, Al in the step (2)2O3The deposition thickness of the insulating film layer is 4-6 nm.
Further, the deposition layer number of the FeGaB magnetostrictive thin film layer in the step (3) is 5, and Al is added2O3The number of deposition layers of the insulating thin film layer was 4.
Further, the FeGaB magnetostrictive thin film layer and Al in the step (2)2O3The insulating film layers are deposited by adopting a sputtering method, the sputtering power is 110-130W and the air pressure is 0.6-0.8Pa when the FeGaB magnetostrictive film layer is deposited; deposition of Al2O3The sputtering power is 90-110W and the air pressure is 0.4-0.6Pa when the insulating film layer is formed.
Further, the size of the magnetostrictive composite film prepared in step (4) is 62-102μm2。
Further, the specific etching process of the magnetostrictive composite film in the step (4) is as follows: dropping photoresist on the surface of the composite film, spin-coating uniformly, and then placing the mixture on a spin coater in a position of 90-1Baking at 10 deg.C for 0.5-2min, covering with mask plate, exposing at 20-24 deg.C and relative humidity of 40-50%, baking at 105 deg.C and 115 deg.C for 0.5-2min, and collecting at 180 deg.C and 220W, SiCl deg.C4/Cl2And carrying out reactive ion etching under the reaction pressure of 5-7Pa by using the reaction gas to obtain the silicon nitride film.
The invention has the technical effects that:
inserting multilayer Al into the magnetostrictive composite film2O3Insulating film of Al2O3The insulating film can limit the eddy current in a narrow space, so that a strong eddy current loop is divided into a plurality of weak loops, and the purpose of enhancing the eddy current loss inhibition rate is further achieved.
The magnetostrictive composite film prepared by the method can reduce the damage to the mutual coupling action between magnetic domains in the magnetic thin film, thereby reducing the degradation of the magnetostrictive characteristic.
Drawings
FIG. 1 shows Al insertion2O3A suppression trend graph of the insulating layer on the eddy current;
FIG. 2 is a comprehensive trend chart of magnetostrictive characteristics and eddy current loss suppression;
FIG. 3 is a graph showing the variation of the suppression ratio of the eddy current loss at different frequencies;
FIG. 4 is a graph showing the variation trend of the eddy current loss suppression rate and the magnetostrictive attenuation rate in different areas;
FIG. 5 is a graph showing the variation trend of the eddy current loss suppression rate and the magnetostrictive attenuation rate under different thicknesses;
FIG. 6 shows Al with different layers2O3A trend graph of the influence of the film on the eddy effect inhibition and the magnetostrictive characteristic attenuation of the magnetic film performance;
FIG. 7 is a trend graph of the variation law of the eddy current suppression rate under different frequency conditions;
fig. 8 is a schematic view of a process for preparing a magnetostrictive composite film according to the present application.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1
A magnetostrictive composite film for enhancing the eddy current loss inhibition efficiency, the preparation method of which comprises the following steps:
(1) ultrasonically cleaning the substrate with acetone, alcohol and pure water for 5min, drying with hot plate at 150 deg.C for 5min, placing the substrate on a magnetron sputtering sample stage, closing the chamber, and vacuumizing the background to 4x10-4Pa, pre-cleaning impurities and a natural oxide layer on the surface of the substrate by using plasma, wherein the process conditions are that the radio frequency power is 200W, the air pressure is 0.5Pa, and the time is 5 min;
(2) depositing a FeGaB magnetostrictive thin film layer on the surface of the substrate pre-cleaned in the step (1), and then depositing Al on the surface of the FeGaB magnetostrictive thin film layer2O3The insulating film layer, specific operation process does: loading power on a FeGaB target position, pre-sputtering for 10 minutes after plasma is started and stabilized, removing impurities and an oxide layer on the surface of the FeGaB target, shielding the FeGaB target between the target and a substrate by using a baffle plate, and attaching a pre-sputtering product to the surface of the baffle plate under the process conditions of 120W of radio frequency power and 0.7Pa of air pressure; then removing the baffle, depositing the magnetostrictive film on the substrate under the process conditions of 120W of radio frequency power and 0.7Pa of air pressure, controlling the deposition time according to the determined deposition rate, and closing the radio frequency power supply after depositing the 150nm film; then, in Al2O3Loading power on target position, pre-sputtering for 10min after plasma glow and stabilization, and adding Al2O3Removing impurities on the surface of the target material, and shielding the target material and the substrate by using a baffle plate to ensure that a pre-sputtering product is attached to the surface of the baffle plate, wherein the process conditions are that the radio frequency power is 100W and the air pressure is 0.5 Pa; removing the baffle plate, Al2O3Depositing the film on a substrate under the process conditions of radio frequency power of 100W and air pressure of 0.5Pa, controlling the deposition time according to the determined deposition rate, and closing a radio frequency power supply after depositing a 5nm film;
(3) repeating the operation in the step (2) to obtain the FeGaB magnetostrictive thin film layer and Al2O3Composite film with alternately arranged insulating film layers, wherein 5 layers of FeGaB magnetostrictive film layers are deposited, and Al is added2O3Depositing 4 layers of the insulating film layer, finally, inflating and breaking vacuum, and taking out the deposited multilayer magnetostrictive composite film;
(4) etching the composite film prepared in the step (3), wherein the specific etching process is as follows: a. coating a photoresist, dripping 2-3cm of photoresist on the surface of a substrate in a yellow region, accelerating the substrate to a constant rotating speed of 4000r/min for 30 s; b. patterning the photoresist: baking the substrate on a hot plate at 100 deg.C for 1 min; c. exposure and development: scanning exposure is carried out on the substrate by adopting a mask plate under the conditions that the temperature is 21 ℃ and the relative humidity is 45%, and the substrate is placed on a hot plate to be baked after exposure, wherein the baking temperature is 110 ℃ and the baking time is 1 min; d. reactive Ion Etching (RIE) is adopted, the radio frequency power is 200W, and the reaction gas is SiCl4/Cl2The pressure of the cavity is 6Pa, the etching time is 5min, and the area after etching is 8 μm2And preparing the magnetostrictive composite film.
Example 2
A magnetostrictive composite film for enhancing the eddy current loss inhibition efficiency, the preparation method of which comprises the following steps:
(1) ultrasonically cleaning the substrate with acetone, alcohol and pure water for 5min, drying with hot plate at 150 deg.C for 10min, placing the substrate on a magnetron sputtering sample table, closing the cavity, and vacuumizing the background to 4x10-4Pa, pre-cleaning impurities and a natural oxide layer on the surface of the substrate by using plasma, wherein the process conditions are that the radio frequency power is 200W, the air pressure is 0.5Pa and the time is 5 min;
(2) depositing a FeGaB magnetostrictive film layer on the surface of the substrate pre-cleaned in the step (1), and then depositing Al on the surface of the FeGaB magnetostrictive film layer2O3The insulating film layer, specific operation process does: loading power on a FeGaB target position, pre-sputtering for 10 minutes after plasma is started and stabilized, removing impurities and an oxide layer on the surface of the FeGaB target, shielding the FeGaB target between the target and a substrate by using a baffle plate, and attaching a pre-sputtering product to the surface of the baffle plate under the process conditions of 120W of radio frequency power and 0.7Pa of air pressure; then the baffle is removed, the magnetostrictive film is deposited on the substrate, the process condition is that the radio frequency power is 120W,the air pressure is 0.7Pa, the deposition time is controlled according to the determined deposition rate, and the radio frequency power supply is closed after the 150nm film is deposited; then, in Al2O3Loading power on target position, pre-sputtering for 10min after plasma glow and stabilization, and adding Al2O3Removing impurities on the surface of the target material, and shielding the target material and the substrate by using a baffle plate to ensure that a pre-sputtering product is attached to the surface of the baffle plate, wherein the process conditions are that the radio frequency power is 100W and the air pressure is 0.5 Pa; removing the baffle plate, Al2O3Depositing the film on a substrate under the process conditions of radio frequency power of 100W and air pressure of 0.5Pa, controlling the deposition time according to the determined deposition rate, and closing a radio frequency power supply after depositing a 5nm film;
(3) repeating the operation in the step (2) to obtain the FeGaB magnetostrictive thin film layer and Al2O3Composite film with alternately arranged insulating film layers, wherein 4 layers of FeGaB magnetostrictive film layers are deposited, and Al is added2 O 33 layers of insulating thin film layers are deposited, finally, the air is filled to break vacuum, and the deposited multilayer magnetostrictive composite film is taken out;
(4) etching the composite film prepared in the step (3), wherein the specific etching process is as follows: a. coating a photoresist, dripping 2-3cm of photoresist on the surface of a substrate in a yellow region, accelerating the substrate to a constant rotating speed of 4000r/min for 30 s; b. patterning the photoresist: baking the substrate on a hot plate at 100 deg.C for 1 min; c. exposure and development: scanning exposure is carried out on the substrate by adopting a mask plate under the conditions that the temperature is 21 ℃ and the relative humidity is 45%, and the substrate is placed on a hot plate to be baked after exposure, wherein the baking temperature is 110 ℃ and the baking time is 1 min; d. reactive Ion Etching (RIE) is adopted, the radio frequency power is 200W, and the reaction gas is SiCl4/Cl2The pressure of the cavity is 6Pa, the etching time is 5min, and the area after etching is 8 μm2And preparing the magnetostrictive composite film.
Test examples
Based on the specific operation method in the embodiment 1-2, the invention establishes the magnetostrictive composite film (FeGaB/Al) in COMSOL multi-physical field simulation software2O3) The eddy current loss model of (1) adopts finite elementsAnalysis (FEA) simulation method, verifying that Al with different thickness/layer number is inserted into FeGaB magnetic film2O3After the film is formed, the specific operation method for inhibiting the eddy current loss of the magnetic film and attenuating the magnetostrictive characteristic comprises the following steps:
1. the frequency of the external magnetic field is set to 1GHz, and the dimensions of the area and the thickness of the magnetostrictive composite film are 8 multiplied by 1 mu m3. The eddy current loss suppression results are shown in FIGS. 1 and 2, and the insertion of a single 5nm layer of Al is shown by FIGS. 1(a), (b), and (c)2O3A thin film for effectively suppressing eddy current loss and inserting a multi-layered Al2O3The suppression ratio can reach more than 90%, because the inserted insulating film can limit the eddy current in a narrow space, thereby dividing the strong eddy current loop into several weaker loops, see fig. 1 c; as shown in FIGS. 2(a) (b), it is shown that Al is inserted2O3The magnetostrictive attenuation rate of the film is approximately linearly increased after the film is larger than 4 layers, and the comprehensive determination is that Al is inserted2O3The thickness of the film is 5nm, and when 4 layers are inserted, the magnetostrictive characteristic attenuation of the magnetic film is ensured to be less than 1.8%, and the eddy current loss can be inhibited by more than 85%.
2. Inserting Al with different thickness and layer number in the frequency range of 0.01-10GHz2O3The effect of frequency on the suppression of eddy current loss of the magnetic film after the film is thinned is shown in FIG. 3. The results of FIG. 3(a) show that a single Al layer is used to reduce the energy loss of FeGaB magnetic films in high frequency devices2O3The thickness of the film is controlled to be 5nm most suitably; FIG. 3(b) shows that the thickness of the inserted multilayer is 5nm for Al2O3After the film is formed, the eddy current loss inhibition rate is almost insensitive to frequency, and the whole attenuation is maintained within 0.5%.
3. The thickness of the FeGaB magnetic film is changed within the range of 0.1-3 mu m, and the area of the magnetic film is changed within 12～142μm2The range was varied, and the suppression effect of the eddy current loss and the attenuation result of the magnetostrictive characteristic were shown in fig. 4. FIG. 4(a) shows magnetic films (1) at different areas2～142 μm 21 μm in thickness and 1GHz in frequency of applied magnetic field) was inserted with a single layer of 5nm Al2O3After film formation, the suppression rate of eddy current loss is dependent on the area of magnetic filmThe increase of (A) is changed like a rainbow. When the area of the magnetic film is less than 102μm2Of (i) is Al2O3The influence of the thickness of the film on the suppression rate of the eddy current loss is not obvious and is more than 102μm2The thinner the rear insulating layer is, the faster the attenuation is; FIG. 4(b) shows that the magnetic film area is less than 62μm2In this case, the area of the magnetic film has a certain influence on the magnetostrictive attenuation rate, but the overall change is less than 5%.
4. Fixed magnetic film area of 82μm2Changing the thickness of the FeGaB magnetic film within the range of 0.1-3 mu m, wherein the inhibition effect of the eddy current loss and the attenuation of the magnetostriction characteristic are shown in figure 5, and when the total thickness of the FeGaB magnetic film is within the range of 0.5-1.5 mu m, the eddy current inhibition rate can be kept to be more than or equal to 65%; the thicker the FeGaB magnetic film is (more than or equal to 0.6 μm), the more stable the magnetostriction property of the FeGaB magnetic film is.
5. Under the frequency condition of 1GHz, selecting FeGaB/Al2O3Composite magnetic film area 62～102μm2And a total thickness of 0.5 to 1.5 μm, and the results of the number of layers of the interposed insulating layer for different magnetic film sizes are shown in FIG. 6. The results are shown in FIG. 6, which shows that for different magnetic film sizes, 4 layers of 5nm Al are preferably inserted2O3The composite magnetic film formed by the film has the optimal combination performance of eddy current inhibition efficiency and magnetostriction characteristics. Based on the composite magnetic film, the influence of eddy current suppression and characteristic attenuation of the magnetic film under different frequency (10MHz-10GHz) conditions is tested, and the specific result is shown in FIG. 7, and the area of the composite magnetic film can be designed to be 62～102μm2The eddy current inhibition efficiency can reach 85.5%; the thickness of the magnetic composite material is very sensitive to the application frequency, and FeGaB/Al is mixed under the conditions of low frequency (0.01-1GHz) and high frequency (more than or equal to 1GHz)2O3The composite magnetic film has a thickness of 0.8-2.5 μm and a thickness of 0.6-1 μm, respectively, and has better comprehensive performance.
Claims (10)
1. A preparation method of a magnetostrictive composite film for enhancing eddy current loss inhibition efficiency is characterized by comprising the following steps:
(1) cleaning and drying the substrate, and then pre-cleaning the substrate by using plasma under a vacuum condition;
(2) depositing a FeGaB magnetostrictive film layer on the surface of the substrate pre-cleaned in the step (1), and then depositing Al on the surface of the FeGaB magnetostrictive film layer2O3An insulating thin film layer;
(3) repeating the operation in the step (2) to obtain the FeGaB magnetostrictive thin film layer and Al2O3Composite films with alternately arranged insulating film layers;
(4) and (4) etching the composite film prepared in the step (3) to prepare the magnetostrictive composite film.
2. The method of preparing a magnetostrictive composite film with enhanced eddy current loss suppression efficiency according to claim 1, wherein the substrate is ultrasonically cleaned with acetone, alcohol and pure water in sequence for 5-10min in step (1).
3. The method of preparing a magnetostrictive composite film with enhanced eddy current loss suppression efficiency according to claim 1, wherein in step (1) 3 to 5 x10-4Plasma treatment is carried out for 4-8min under the conditions of Pa vacuum, 180-200W radio frequency power and 0.4-0.6Pa air pressure.
4. The method according to claim 1, wherein the deposition thickness of the FeGaB magnetostrictive thin film layer in step (2) is 140-160 nm.
5. The method of claim 1, wherein Al is added in step (2) to form a magnetostrictive composite film with enhanced eddy current loss suppression efficiency2O3The deposition thickness of the insulating film layer is 4-6 nm.
6. The method of claim 1, wherein the number of deposited FeGaB magnetostrictive thin film layers in step (3) is 4-5, and Al is added to the deposited FeGaB magnetostrictive thin film layers2O3The number of deposited layers of the insulating film layers is 3-4.
7. The method of claim 1, wherein the FeGaB magnetostrictive thin film layer and Al in step (2) are formed by a method comprising forming a magnetostrictive composite film with enhanced eddy current loss suppression efficiency2O3The insulating film layers are deposited by adopting a sputtering method, the sputtering power is 110-130W and the air pressure is 0.6-0.8Pa when the FeGaB magnetostrictive film layer is deposited; deposition of Al2O3The sputtering power is 90-110W and the air pressure is 0.4-0.6Pa when the insulating film layer is formed.
8. The method of preparing a magnetostrictive composite film with enhanced eddy current loss suppression efficiency according to claim 1, wherein the magnetostrictive composite film prepared in step (4) has a size of 62-102μm2。
9. The method for preparing a magnetostrictive composite film with enhanced eddy current loss suppression efficiency according to claim 1, wherein the specific etching process of the magnetostrictive composite film in the step (4) is as follows: dropping photoresist on the surface of the composite film, uniformly spin-coating, baking at 90-110 deg.C for 0.5-2min, covering with mask plate, exposing at 20-24 deg.C and relative humidity of 40-50%, baking at 105-115 deg.C for 0.5-2min, and collecting the product obtained by 180-220W, SiCl4/Cl2And carrying out reactive ion etching under the reaction pressure of 5-7Pa by using the reaction gas to obtain the silicon nitride film.
10. A magnetostrictive composite film with enhanced eddy current loss suppression efficiency, characterized in that it is obtained by a process according to any one of claims 1 to 9.
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| CN110970716A (en) * | 2019-12-26 | 2020-04-07 | 四川爆米微纳科技有限公司 | Eddy current suppression structure and preparation method thereof |
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| CN110970716A (en) * | 2019-12-26 | 2020-04-07 | 四川爆米微纳科技有限公司 | Eddy current suppression structure and preparation method thereof |
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