CN109887706B - Magnetic nano-particle composite membrane and preparation method thereof - Google Patents
Magnetic nano-particle composite membrane and preparation method thereof Download PDFInfo
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- CN109887706B CN109887706B CN201910273164.4A CN201910273164A CN109887706B CN 109887706 B CN109887706 B CN 109887706B CN 201910273164 A CN201910273164 A CN 201910273164A CN 109887706 B CN109887706 B CN 109887706B
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- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 239000002122 magnetic nanoparticle Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000012528 membrane Substances 0.000 title description 7
- 239000006249 magnetic particle Substances 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000000151 deposition Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims description 23
- 230000008020 evaporation Effects 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 3
- 238000009501 film coating Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 57
- 239000002105 nanoparticle Substances 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 6
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 abstract description 5
- 230000006872 improvement Effects 0.000 abstract description 4
- 238000004891 communication Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 2
- 239000002923 metal particle Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000007709 nanocrystallization Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000005355 Hall effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 239000002772 conduction electron Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
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Abstract
A magnetic nano-particle composite film and a preparation method thereof belong to the technical field of thin film material magnetic control. A magnetic nanoparticle composite film is formed by continuously and alternately depositing a magnetic layer and an insulating layer, and the thickness of the composite film is 15-100 nm; the magnetic layer is a layer film formed by uniformly embedding magnetic particles into an insulating medium, the magnetic particle component is Fe or Fe-Ni, the volume fraction of the magnetic particles is 80-95%, and the thickness of the magnetic layer is 1-20 nm; the insulating layer is composed of an insulating medium, and the thickness of the insulating layer is 0.1-10 nm. The magnetic nano-particle composite film prepared by the invention can control the merging growth, the particle size, the distribution uniformity and the like of nano-particles, thereby realizing the improvement of magnetism while refining grains. The composite film prepared by the method is particularly suitable for electronic components in the fields of digital electronic industry and communication technology.
Description
Technical Field
The invention belongs to the technical field of thin film material magnetic control, and particularly relates to a magnetic nanoparticle composite film and a preparation method thereof.
Background
The development of the digital electronics industry and communication technology requires the development of electronic components toward high integration, high frequency, and nanocrystallization. After the magnetic thin film as the core material is subjected to nanocrystallization, special electromagnetic phenomena such as giant conductance effect, giant magnetoresistance effect, giant hall effect and the like can be generated. The magnetic nano film has wide application in the fields of high-density storage, magneto-resistance sensors, high-frequency sensors, micro-electro-mechanical systems, micro-transformers, anti-electromagnetic interference, microwave absorption and the like.
The nanocrystallization means that the grain size is controlled within the range of 1 to 100 nm. Sometimes the grain size is even smaller than 5nm in order to obtain properties that meet the application requirements. However, the reduction in grain size can cause the magnetic properties of the film to be affected by thermal perturbations, resulting in the superparamagnetic effect. Furthermore, the reduction of grain size affects the signal-to-noise ratio of the magnetic signal, and the enhancement of the scattering of conduction electrons affects the resistivity and high frequency performance of the film. Meanwhile, small-sized crystal grains are easy to generate phase change different from that of a block body, and the magnetic performance of the film is reduced. Thus, the nanoparticles are embedded in an insulating medium (e.g., SiO)2MgO, etc.) to improve the magnetic property of the film after grain refinement by utilizing the coupling effect of the insulating medium to the composite film grains, the magnetic anisotropy, the demagnetization effect, etc. And the tunnel effect of electrons among particles can also influence the magnetic property and the magneto-resistance property of the nano particle composite film, and special effects such as Hall effect, tunnel magneto-resistance and the like are generated. However, the problems of the nanoparticle composite film such as difficulty in controlling the combined growth and size, non-uniformity in particle size and distribution, etc. limit further improvement of the magnetic properties of the nanoparticle composite film. Therefore, there is a need to develop a new preparation method to improve magnetic properties through the control of nanoparticles in the composite film.
Disclosure of Invention
In order to solve the technical problems, the invention provides a magnetic nanoparticle composite film and a preparation method thereof. The magnetic nano-particle composite membrane prepared by the invention can control the merging growth, the particle size, the distribution uniformity and the like of nano-particles, thereby realizing the improvement of magnetism while refining the particles. The composite film prepared by the method is particularly suitable for electronic components in the fields of digital electronic industry and communication technology.
A magnetic nanoparticle composite film is formed by continuously and alternately depositing a magnetic layer and an insulating layer, and the thickness of the composite film is 15-100 nm;
the magnetic layer is a layer film formed by uniformly embedding magnetic particles with uniform size into an insulating medium, wherein the magnetic particle component is Fe or Fe-Ni, the volume fraction of the magnetic particles is 80-95%, the diameter of the magnetic particles is 1-20 nm, and the thickness of the magnetic layer is 1-20 nm;
the insulating layer is composed of an insulating medium, and the thickness of the insulating layer is 0.1-10 nm.
In the invention, the magnetic layer is formed by wrapping magnetic particles by an insulating medium SiO, and the magnetic particles are regularly arranged in the insulating medium in the magnetic layer.
The magnetic particles in the invention are uniform in size, that is, the size distribution of the magnetic particles in the magnetic layer is concentrated, and the variation range is 1-2% of the size of the magnetic particles.
Preferably, the Fe-Ni is Fe20Ni80。
Preferably, the insulating medium is SiO.
Another object of the present invention is to provide a method for preparing a magnetic nanoparticle composite film, comprising the steps of: taking a pretreated quartz wafer or monocrystalline silicon wafer as a substrate; depositing a composite film by using metal particles and SiO particles as raw materials, wherein the diameters of the metal particles and the SiO particles are 1-3 mm, the purity is more than or equal to 99.99%, and the metal particles are Fe or Fe-Ni particles; deposition parameters: the vacuum degree of the film coating chamber is better than or equal to 5.0 multiplied by 10-5Pa, the temperature of a molecular beam evaporation source is 900-1600 ℃, and the temperature of a sample stage is 25-500 ℃; continuously and alternately depositing the magnetic layer and the insulating layer until the thickness of the composite film is 15-100 nm;
deposition of the magnetic layer: opening a molecular beam evaporation source baffle and a substrate baffle which are provided with metal particles and SiO particles at the same time, wherein the deposition rate ratio of the metal particles to the SiO particles is 1: 1-20: 1, and the thickness of the magnetic layer is controlled to be 1-20 nm;
deposition of the insulating layer: closing the molecular beam evaporation source baffle plate containing the metal particles, independently depositing SiO, and controlling the thickness of the insulating layer to be 0.1-10 nm.
According to the invention, the magnetic layer and the insulating layer are continuously and alternately deposited, so that the combined growth of the nano particles in the magnetic nano particle composite film, the size and the distribution uniformity of the nano particles and the like can be controlled.
In the invention, the substrate is close to the evaporation source and is positioned in the uniform area, and the deposition rate is the evaporation rate in the area.
Preferably, in the deposition of the magnetic layer and the insulating layer, the film thickness is controlled by evaporation time.
Preferably, the Fe-Ni is Fe20Ni80。
Preferably, the pretreated quartz wafer or monocrystalline silicon wafer is a polished quartz wafer or monocrystalline silicon wafer with the surface roughness less than 0.5nm, and is ultrasonically cleaned in acetone, deionized water and alcohol solution for 15min in sequence and dried by a high-pressure spray gun of high-purity argon.
Preferably, after the composite film is deposited, the molecular beam evaporation source baffle is closed, the substrate temperature is reduced to room temperature, the temperature reduction rate is less than 15 ℃/min, and the composite film is taken out.
The magnetic layer is formed by co-evaporating metal particles and an insulating medium by two molecular beam evaporation sources, so that the magnetic particles are uniformly embedded into the insulating medium, and the magnetic nano particles are transversely and orderly arranged; in the preparation of the insulating layer, a molecular beam evaporation source separately evaporates an insulating medium to separate metal particles in the longitudinal direction, thereby controlling the magnetic particle size.
Compared with the prior art, the magnetic nanoparticle composite film and the preparation method thereof have the beneficial effects that:
1. the invention relates to a magnetic nano-particle composite film and a preparation method thereof, wherein the magnetic nano-particle composite film with controllable size and orderly arrangement of magnetic particles is prepared by alternately depositing a magnetic layer and a non-magnetic layer;
2. in the preparation process of the magnetic layer, the metal and the insulating medium are co-evaporated by a molecular beam source, so that the metal magnetic particles of the composite film are uniformly embedded into the insulating medium, the size of the magnetic particles is influenced, and the particles are transversely arranged orderly; the method for alternately depositing the layers to grow can form magnetic particles through the difference of the surface energy of the magnetic layers and the surface energy of the non-magnetic layers, so that the particles are longitudinally arranged orderly, and the thickness of the magnetic layers can be controlled to achieve the purpose of controlling the size of the magnetic particles;
3. the growth rate is adjusted by the temperature of a beam source, the merging growth of particles can be influenced, the size of the particles and the distribution uniformity thereof can be controlled, and the volume fraction of the magnetic particles in the composite film can be controlled;
4. the magnetic nano-particle composite film realizes the improvement of the saturation magnetization of the composite film and the change of the coercive force from a few oersteds to a few hundred oersteds; the magnetic particle has magnetism when the particle size is 3.6nm, and the grain size of the superparamagnetic effect is reduced; the electrical property of the nano-particle composite film is changed;
5. the magnetic nanoparticle composite film and the preparation method thereof have the advantages of simple equipment, good repeatability, good film growth controllability, high purity and good quality of the prepared composite film and low cost.
Drawings
FIG. 1 is a schematic cross-sectional structural view of a magnetic nanoparticle composite film according to an embodiment of the present invention; wherein, 1-a magnetic layer; 2-SiO insulating layer; magnetic nanoparticles Fe in 3-magnetic layer20Ni80-SiO; 4-insulating medium SiO in magnetic layer. Wherein the thickness of the magnetic layer is 6nm, and the thickness of the SiO insulating layer is 1 nm;
FIG. 2 shows Fe prepared in example 1 of the present invention20Ni80-a TEM image of a cross section of the SiO magnetic nanoparticle composite film;
FIG. 3 shows Fe prepared in example 1 of the present invention20Ni80-a high resolution TEM image of the SiO magnetic nanoparticle composite film cross section;
FIG. 4 is Fe20Ni80Metal film (a) of (a) and Fe prepared in example 1 of the present invention20Ni80-a magnetic contrast of the SiO magnetic nanoparticle composite film (b);
FIG. 5 is Fe20Ni80Metal film (a) of (a) and Fe prepared in example 1 of the present invention20Ni80-a comparison graph of surface topography of the SiO magnetic nanoparticle composite film (b);
FIG. 6 is Fe20Ni80Metal film (a) of (a) and Fe prepared in example 1 of the present invention20Ni80-magnetic domain contrast of SiO magnetic nanoparticle composite films (b).
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
The test methods described in the following examples are, unless otherwise specified, conventional; the reagents and materials used, unless otherwise indicated, are commercially available.
Example 1
Fe20Ni80The evaporation rate at 1375 ℃ was 0.916nm/min, and the evaporation rate of SiO at 982 ℃ was 0.238 nm/min. Fe20Ni80SiO layer was deposited for 6min33s at the above rate, and insulating layer SiO was deposited for 4min12s at the above rate, alternately 5 times. The preparation method of the magnetic nanoparticle composite membrane comprises the following steps:
selecting a polished silicon wafer with the surface roughness of less than 0.5nm and the crystal orientation of (100), ultrasonically cleaning the silicon wafer in acetone, deionized water and alcohol solution for 15min in sequence, and drying the silicon wafer by using a high-pressure spray gun of high-purity argon;
the raw material is Fe with the diameter of 1mm20Ni80The purity of the raw materials of the particles and SiO particles with the diameter of 3mm is 99.999 percent, the two raw materials are respectively placed into 2 customized large-opening crucibles, the crucibles are respectively placed into two beam sources, and beam source baffles are closed;
and (3) placing the substrate processed in the step (1) on a sample table. When the vacuum degree of the film coating chamber is better than 5.0 multiplied by 10-5When Pa is needed, the sample table is heated to 200 ℃ at the speed of 15 ℃/min; will contain Fe20Ni80Heating a molecular beam evaporation source of the particles to 1375 ℃, heating the molecular beam evaporation source containing SiO particles to 982 ℃, and depositing a composite film:
(1) preparing a magnetic layer: opening two molecular beam evaporation source baffles at the same time, opening a substrate baffle after the evaporation rate is stable, starting timing at the same time, wherein the deposition time is 6min33s, and closing the substrate baffle after timing is finished;
(2) preparing an insulating layer: will contain Fe20Ni80Particle molecular beam evaporation source baffle plate is closed, and molecular beam evaporation with SiO particlesKeeping the source baffle in an open state, opening the substrate baffle, simultaneously starting timing, wherein the deposition time is 4min12s, and closing the substrate baffle after timing is finished;
repeating the steps (1) and (2) for 5 times, closing the substrate baffle and the beam source baffle, and realizing the alternate growth of the magnetic layer and the insulating layer;
and 4, cooling the substrate to room temperature, and taking out the composite membrane, wherein the cooling rate is 15 ℃/min.
To obtain Fe20Ni80The structure of the-SiO magnetic nanoparticle composite film sample is shown in FIG. 1, and the TEM cross section and the high resolution cross section are shown in FIG. 2 and FIG. 3, respectively; in fig. 2, it can be seen that the composite film is significantly delaminated, and a significant SiO layer is present between each layer in the longitudinal direction, i.e., the white bright line portion in the figure. Fe is clearly seen in FIG. 320Ni80SiO magnetic particles, and the arrangement of the particles in the magnetic layer is uniform.
To obtain Fe20Ni80-SiO magnetic nanoparticle composite membrane sample and Fe20Ni80The comparison graphs of the magnetic property, the surface morphology and the magnetic domain structure of the metal film are respectively shown in FIGS. 3, 4 and 5, and it can be seen through comparison that Fe in FIG. 320Ni80The coercive force of the-SiO magnetic nanoparticle composite film is larger than that of the metal film Fe20Ni80The difference between the saturation magnetization and the saturation magnetization is not great. Fe due to nanoparticle incorporation in FIG. 420Ni80The surface particles of the-SiO magnetic nanoparticle composite film are larger than those of a pure FeNi film. From FIG. 5 Fe20Ni80The obvious magnetic domain structure can be seen from the-SiO magnetic nanoparticle composite film.
Claims (4)
1. A preparation method of a magnetic nanoparticle composite film is characterized by comprising the following steps: taking a pretreated quartz wafer or monocrystalline silicon wafer as a substrate; the composite film is deposited by taking magnetic particles and SiO particles as raw materials, the diameters of the magnetic particles and the SiO particles are 1-3 mm, the purity is more than or equal to 99.99%, and the magnetic particles are Fe20Ni80Particles; deposition parameters: the vacuum degree of the film coating chamber is better than or equal to 5.0 multiplied by 10-5Pa, the temperature of a molecular beam evaporation source is 900-1600 ℃, and a sample tableThe temperature is 25-500 ℃; the composite film is formed by continuously and alternately depositing a magnetic layer and an insulating layer, and the thickness of the composite film is 15-100 nm; the magnetic layer is a layer film formed by uniformly embedding magnetic particles with uniform sizes into an insulating medium, the volume fraction of the magnetic particles is 80-95%, the diameter of the magnetic particles is 1-20 nm, and the thickness of the magnetic layer is 1-20 nm; the insulating layer is composed of an insulating medium, the thickness of the insulating layer is 0.1-10 nm, and the insulating medium is SiO;
deposition of the magnetic layer: opening a molecular beam evaporation source baffle and a substrate baffle which are provided with magnetic particles and SiO particles at the same time, wherein the deposition rate ratio of the magnetic particles to the SiO particles is 1: 1-20: 1, and the thickness of the magnetic layer is controlled to be 1-20 nm;
deposition of the insulating layer: closing the molecular beam evaporation source baffle plate containing the magnetic particles, independently depositing SiO, and controlling the thickness of the insulating layer to be 0.1-10 nm.
2. The method of claim 1, wherein the magnetic layer and the insulating layer are deposited with a film thickness controlled by evaporation time.
3. The method of claim 1, wherein the pretreated quartz wafer or single crystal silicon wafer is a polished quartz wafer or single crystal silicon wafer having a selected surface roughness of less than 0.5nm, and is ultrasonically cleaned in acetone, deionized water and alcohol solution for 15min in sequence, and then blown dry with a high pressure spray gun of high purity argon gas.
4. The method according to claim 1, wherein the molecular beam evaporation source baffle is closed after the composite film is deposited, the temperature of the substrate is reduced to room temperature, the temperature reduction rate is less than 15 ℃/min, and the composite film is taken out.
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