CN113235159B - Method for preparing single crystal nickel ferrite film - Google Patents

Method for preparing single crystal nickel ferrite film Download PDF

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CN113235159B
CN113235159B CN202110370455.2A CN202110370455A CN113235159B CN 113235159 B CN113235159 B CN 113235159B CN 202110370455 A CN202110370455 A CN 202110370455A CN 113235159 B CN113235159 B CN 113235159B
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nickel ferrite
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CN113235159A (en
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王悦
薛德胜
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Lanzhou University
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Abstract

The invention discloses a method for preparing a single crystal nickel ferrite film, which comprises the following steps: at room temperature, a nickel ferrite target is adopted, and a single crystal nickel ferrite film is prepared on a single crystal substrate through magnetron sputtering. The method can prepare the single crystal nickel ferrite film at room temperature by a magnetron sputtering method, does not need to heat the substrate or perform subsequent heat treatment in the sputtering process, and has the advantages of simple operation, high repeatability and wide application prospect.

Description

Method for preparing single crystal nickel ferrite film
Technical Field
The invention relates to the technical field of magnetic thin film materials, in particular to a method for preparing a single crystal nickel ferrite thin film.
Background
The nickel ferrite material is a spinel type soft magnetic ferrite, and has the advantages of high resistivity, wide applicable frequency range of more than one hundred megahertz, low loss, good chemical stability and the like, so the nickel ferrite material is widely applied to the fields of electronic devices, communication equipment, computers and the like. With the development of new fields and the development of technologies, devices are continuously developed towards miniaturization, sheet type, high performance and the like, and the thinning of soft magnetic ferrite is also an inevitable trend.
At present, the nickel ferrite film can be mainly prepared by physical or chemical methods such as vacuum evaporation, ion plating, sputtering, gas phase reaction method and the like. The magnetron sputtering is a common physical vapor deposition technology, and has the advantages that: the method has the advantages of simple operation, good repeatability, high film deposition speed, controllable film thickness, compact and uniform obtained film, high purity and large film coating area, and can also be applied to industrial production.
Although magnetron sputtering has the advantages, molecular beam epitaxy is the first choice in preparing single crystal films, and magnetron sputtering is very difficult to prepare single crystal films. In the related technology, the nickel ferrite film directly obtained by the room temperature magnetron sputtering method generally has very poor crystallinity, even amorphous state, and the single crystal nickel ferrite film can be obtained only by heating the substrate in the sputtering process or performing heat treatment for a period of time after the sputtering is finished. If the single crystal nickel ferrite film can be directly deposited by room temperature magnetron sputtering, a new method is provided for obtaining the single crystal ferrite film in a laboratory, a high-temperature preparation process is not needed, and the application limit of the single crystal nickel ferrite film in a chip electronic device is reduced; the much faster deposition rate compared to molecular beam epitaxy also makes the preparation of single crystal films of hundred nanometers thickness much easier. Therefore, it is important and necessary to search for a method for preparing single crystal nickel ferrite by magnetron sputtering at room temperature.
Disclosure of Invention
The present invention is directed to solving at least one of the above problems in the prior art. Therefore, an object of the present invention is to provide a method for preparing a single crystal nickel ferrite thin film, which can obtain a single crystal nickel ferrite thin film directly on a single crystal substrate by rf magnetron sputtering without heating the substrate during sputtering or performing subsequent thermal treatment. The second purpose of the invention is to provide the single crystal nickel ferrite film prepared by the method. The invention also aims to provide application of the single crystal nickel ferrite film.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a first aspect of the invention provides a method of preparing a single crystal nickel ferrite thin film, comprising the steps of:
at room temperature, a nickel ferrite target is adopted, and a single crystal nickel ferrite film is prepared on a single crystal substrate through magnetron sputtering.
According to some embodiments of the method of preparing a single crystal nickel ferrite thin film of the present invention, the method of preparing the nickel ferrite target comprises the steps of:
1) preparing nickel ferrite precursor powder by an oxalate coprecipitation method;
2) sintering the nickel ferrite precursor powder to obtain nickel ferrite powder;
3) and pressing and sintering the nickel ferrite powder to obtain the nickel ferrite target material.
In the preparation method of the nickel ferrite target material, the precursor obtained by the oxalate coprecipitation method has correct nickel-iron proportion and uniform components, so that the sintered nickel ferrite has high purity and is single-phase without impurities and impure phases.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film, step 1) of the method for preparing a nickel ferrite target material specifically comprises the steps of mixing an ammonium oxalate solution and a metal salt solution for reaction to obtain nickel ferrite precursor powder; the metal salt comprises ferrous salt and nickel salt.
The invention adopts oxalate coprecipitation method to prepare nickel ferrite powder, and the chemical reaction equation is as follows: ni2++2Fe2++3(C2O4)2-+6H2O→NiFe2(C2O4)3·6H2O ↓. Most of metal oxalates have similar crystal structures, precipitates are easy to form mixed crystal structures, metal ions are distributed at lattice points according to the proportion in the original solution, the mixing in a molecular range can be achieved, the nickel ferrite obtained after firing is uniform in chemical composition, high in purity, free of impurity phase generation and good in powder particle fluidity, and can be granulated and formed without long-time ball milling; ammonium oxalate used as a precipitator is easy to decompose and volatilize in the firing process and has no residue, the released carbon monoxide and carbon dioxide gas have no problem of sulfur smoke pollution, and ammonium sulfate in waste liquid can be used as a fertilizer after being recovered and treated, so that the environment is protected and no pollution is caused.
According to some embodiments of the method for preparing a single crystal nickel ferrite film, in step 1), ammonium oxalate, ferrous salt and nickel salt are respectively prepared into solutions with the concentration of 0.4 mol/L-0.6 mol/L, and then mixed and reacted.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, in step 1), the ferrous salt comprises ferrous sulfate.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, in step 1) of the method for preparing a nickel ferrite target, the nickel salt comprises nickel sulfate.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film, in step 1), after mixing and reacting an ammonium oxalate solution with a metal salt solution, the method further comprises the steps of washing and drying the obtained precipitate.
Thermogravimetric test is carried out on oxalate powder obtained by a precipitation method, so that along with the rise of temperature, oxalate is gradually decomposed, crystal water and oxalate are removed, and the reaction is as follows:
Figure BDA0003009072680000031
at about 400 c, the remainder was essentially ferrite phase, and after increasing to about 600 c, the sample mass tended to stabilize and no longer changed significantly. Therefore, the oxalate precursor powder is pre-sintered at about 400 ℃ to be fully decomposed; secondary sintering at about 600 ℃ promotes the formation of ferrite phase.
According to some embodiments of the method for preparing the single crystal nickel ferrite film, in the step 2) of the method for preparing the nickel ferrite target material, the sintering is specifically carried out by heating to 350-450 ℃ at a heating rate of 1.5-2.5 ℃/min, preserving the heat for 4-6 h, grinding, and then sintering at 550-650 ℃ for 4-6 h (h).
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, in step 3), a nickel ferrite powder and a binder are mixed, granulated, and then pressed.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film, in step 3), the ratio of the amount of the nickel ferrite powder to the amount of the binder is (18-22) g: 1 mL.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, in step 3) of the method for preparing a nickel ferrite target, the binder comprises ethanol. In some embodiments of the invention, absolute ethanol is used as the binder.
In the pressing process of the target material, the particle size of the nickel ferrite powder prepared by the oxalate coprecipitation method is in the micron order, the fluidity is good, the viscosity is poor, and the nickel ferrite powder is difficult to form by direct dry pressing. According to the invention, ethanol is selected as a temporary binder, and proper pressure and pressure maintaining duration are found out to obtain a formed target blank; during sintering, the heating rate of about 1 ℃/min is selected, and the heat preservation treatment is carried out at about 600 ℃, on one hand, the purpose is to fully volatilize the binder and reduce the generation of pores; on the other hand, the slow heating rate can ensure that the target blank is uniformly heated, is not easy to deform and crack and improves the density.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film, in step 3), the pressing pressure is 40 to 45MPa, and the pressure holding time is 20 to 30 min.
According to some embodiments of the method for preparing a single crystal nickel ferrite film, in step 3), the sintering is specifically carried out by heating to 550-650 ℃ at a heating rate of 0.5-1.5 ℃/min, keeping the temperature for 1.5-2.5 h, heating to 900-1100 ℃ at a heating rate of 0.5-1.5 ℃/min, and keeping the temperature for 7-9 h. By adopting the sectional sintering process, the binder can be ensured to be fully volatilized, and the density of the target material is improved.
In some embodiments of the method for preparing a single crystal nickel ferrite film, the sintering in step 3) of the method for preparing a nickel ferrite target material is specifically carried out by heating to 580-620 ℃ at a heating rate of 1 ℃/min, preserving heat for 1.5-2.5 h, heating to 980-1020 ℃ at a heating rate of 1 ℃/min, and preserving heat for 7-9 h.
The invention can prepare the single crystal nickel ferrite film on a plurality of single crystal substrates with different lattice constants, and the single crystal nickel ferrite film has different strain states due to different lattice mismatch degrees, so that the magnetism of the film can be regulated and controlled, and the proper single crystal substrate can be selected according to the requirement in practical application.
According to some embodiments of the method of preparing a single crystal nickel ferrite thin film of the present invention, the single crystal substrate has a lattice mismatch with nickel ferrite of less than 6.5%.
According to some embodiments of the method of preparing a single crystal nickel ferrite thin film of the present invention, the single crystal substrate includes a magnesium oxide (MgO) substrate, a lead magnesium niobate titanate (PMNPT) substrate, or a Strontium Titanate (STO) substrate.
In the preparation process of the single crystal film, the selection of a proper single crystal substrate and sputtering conditions are very important.
The choice of single crystal substrate depends on the degree of lattice mismatch between the substrate and the film
Figure BDA0003009072680000041
Wherein a issIs the substrate lattice constant, aeFor the thin film lattice constant, it is generally considered that<5% forming coherent interface, 5%<δ<25% form a semi-coherent interface, delta>The matching capability is completely lost in 25 percent; for the nickel ferrite film, the mismatching degrees with the magnesium oxide, the lead magnesium niobate titanate and the strontium titanate substrate are respectively 1.02%, 3.47% and 6.32%, and the matching capability cannot be lost.
According to some embodiments of the method of preparing a single crystal nickel ferrite film of the present invention, a single crystal substrate is pretreated before magnetron sputtering; the pretreatment method specifically comprises the following steps: and cleaning and drying the single crystal substrate. The cleaning is to put the single crystal substrate into acetone for ultrasonic cleaning, then put the single crystal substrate into ethanol for ultrasonic cleaning, and then rinse the single crystal substrate by the ethanol; the drying is specifically drying by nitrogen.
According to some embodiments of the method for preparing a single crystal nickel ferrite film of the present invention, the magnetron sputtering is performed in a magnetron sputtering apparatus, in particular: adhering a single crystal substrate on a sample holder, and placing the single crystal substrate on a sample frame of a sputtering chamber of magnetron sputtering equipment; placing a target material of the nickel ferrite on a target holder of a sputtering chamber of magnetron sputtering equipment, adjusting the distance between the target material and a substrate, vacuumizing, introducing pure argon into the sputtering chamber, adjusting the gas flow, and adjusting the gas pressure and power to perform glow starting; after glow starting, adjusting sputtering air pressure and sputtering power, and starting film coating after stabilization; and after the sputtering is finished, the power supply of the target is closed, and the gas circuit is closed, so that the single crystal nickel ferrite film deposited on the substrate can be directly obtained.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, the magnetron sputtering conditions satisfy at least one of:
the distance between the substrate and the target is 5 cm-6 cm;
the sputtering atmosphere is argon;
the flow rate of the sputtering gas is 10sccm to 20 sccm;
the sputtering pressure is 0.2Pa to 0.5 Pa;
the sputtering power is 150W-250W.
In some embodiments of the method of preparing a single crystal nickel ferrite thin film according to the present invention, the substrate to target spacing is 5.5 cm.
In some embodiments of the method of preparing a single crystal nickel ferrite film of the present invention, the sputtering gas pressure is 0.5 Pa.
In some embodiments of the method of preparing a single crystal nickel ferrite film according to the present invention, the sputtering power is 200W.
According to some embodiments of the method for preparing a single crystal nickel ferrite thin film of the present invention, a glow starting pressure is not less than 3.0Pa in the magnetron sputtering.
According to some embodiments of the method for preparing a single crystal nickel ferrite film of the present invention, the glow discharge power is not less than 50W in the magnetron sputtering.
According to some embodiments of the method for preparing a single crystal nickel ferrite film of the present invention, in the magnetron sputtering, a sputtering chamber of a magnetron sputtering apparatus is evacuated to a predetermined background vacuum of 4.0 × 10-5～5.50×10-5Pa。
According to some embodiments of the method for preparing a single crystal nickel ferrite film, the sputtering time in the magnetron sputtering is 200 seconds(s) to 4000 seconds.
In some embodiments of the method of preparing a single crystal nickel ferrite thin film according to the present invention, the sputtering time is 300 seconds to 3600 seconds.
The sputtering coating of the invention mainly comprises three processes: the argon ions bombard the target surface to enable sputtering particles to escape, the sputtering particles migrate to the substrate, and the sputtering particles reach the substrate to form a film. The main factors influencing the crystalline phase of the film are the kinetic energy of the particles reaching the substrate, which is related to whether the particles can diffuse and migrate on the surface of the substrate and form an ordered arrangement, and the sputtering rate, which is related to whether the time reserved for the particles to diffuse to the equilibrium position is sufficient. By controlling the kinetic energy of the particles reaching the substrate and the sputtering rate, a thin film with good crystallinity can be directly obtained. The sputtering power has a direct relation with the initial kinetic energy of the sputtered particles which are shot out; the sputtering gas pressure reflects the amount of introduced argon atoms, the higher the sputtering gas pressure is, the more argon atoms are, the more argon ions are generated after ionization, the more sputtering particles are bombarded, the faster the sputtering rate is, and on the other hand, the migration process of the sputtering particles can be regarded as the process that the particles pass through filling gas, the higher the sputtering gas pressure is, the higher the probability of collision of the sputtering particles is, so that kinetic energy loss and change of the moving direction are caused; the distance between the target and the substrate is the migration distance of the sputtering particles, and the longer the distance is, the higher the probability of collision of the sputtering particles is; the sputtering atmosphere is also a factor influencing sputtering, a mixed gas of argon and other gases is introduced under the same sputtering gas pressure, if other gases as reaction gases do not participate in reaction, the higher the proportion of argon as working gas is, the faster the sputtering rate is, and the smaller the probability of collision with other gases is, the smaller the kinetic energy loss is. Therefore, in order to make the particles reach the substrate to have enough kinetic energy and time for diffusion and migration to the equilibrium position to form ordered arrangement so as to obtain the single crystal nickel ferrite film, the sputtering conditions are required to be: the space between the target and the substrate is small, if reaction gas is not needed, only pure argon is introduced, the sputtering pressure is low, and the sputtering power is moderate.
According to the method for preparing the single crystal nickel ferrite film, the single crystal substrate does not need to be heated in the magnetron sputtering process, or the heat treatment step is carried out after the magnetron sputtering process.
The second aspect of the invention provides a single crystal nickel ferrite thin film prepared by the method according to the first aspect of the invention.
A third aspect of the invention provides the use of the aforementioned single crystal nickel ferrite thin film.
Use of a single crystal nickel ferrite film produced by the method according to the first aspect of the invention or a single crystal nickel ferrite film according to the second aspect of the invention in an electronic device, a communication device or a computer.
According to some embodiments of the application of the present invention, the electronic device is a chip electronic device.
The invention has the beneficial effects that:
the single crystal nickel ferrite film can be prepared by the magnetron sputtering method at room temperature, the substrate does not need to be heated or subjected to subsequent heat treatment in the sputtering process, and the method is simple to operate, high in repeatability and wide in application prospect.
Drawings
FIG. 1 is an XRD pattern of the (110) plane of a single crystal nickel ferrite film obtained in example 1 of the present invention;
FIG. 2 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 1 of the present invention;
FIG. 3 is a phi scan of the (100) plane of the single crystal nickel ferrite film obtained in example 1 of the present invention;
FIG. 4 is a rocking curve diagram of the single crystal nickel ferrite thin film obtained in example 1 of the present invention;
FIG. 5 is an XRR diagram of a single crystal nickel ferrite thin film obtained in example 1 of the present invention;
FIG. 6 is a VSM of the single crystal nickel ferrite thin film obtained in example 1 of the present invention;
FIG. 7 is an XRD pattern of the (110) plane of the single crystal nickel ferrite film obtained in example 2 of the present invention;
FIG. 8 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 2 of the present invention;
FIG. 9 is a phi scan of the (100) plane of the single crystal nickel ferrite film obtained in example 2 of the present invention;
FIG. 10 is a VSM of the single crystal nickel ferrite thin film obtained in example 2 of the present invention;
FIG. 11 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 3 of the present invention;
FIG. 12 is an XRD pattern of the (110) plane of a single crystal nickel ferrite film obtained in example 3 of the present invention;
FIG. 13 is a phi scan of the (110) plane of the single crystal nickel ferrite film obtained in example 3 of the present invention;
FIG. 14 is a VSM of the single crystal nickel ferrite thin film obtained in example 3 of the present invention;
FIG. 15 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 4 of the present invention;
FIG. 16 is an XRD pattern of the (110) plane of the single crystal nickel ferrite film obtained in example 4 of the present invention;
FIG. 17 is a phi scan of the (110) plane of the single crystal nickel ferrite film obtained in example 4 of the present invention;
FIG. 18 is a VSM of the single crystal nickel ferrite thin film obtained in example 4 of the present invention;
FIG. 19 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 5 of the present invention;
FIG. 20 is an XRD pattern of the (110) plane of the single crystal nickel ferrite film obtained in example 5 of the present invention;
FIG. 21 is a phi scan of the (110) plane of the single crystal nickel ferrite film obtained in example 5 of the present invention;
FIG. 22 is a VSM of the single crystal nickel ferrite thin film obtained in example 5 of the present invention;
FIG. 23 is an XRD pattern of the (100) plane of the single crystal nickel ferrite film obtained in example 6 of the present invention;
FIG. 24 is an XRD pattern of the (110) plane of the single crystal nickel ferrite film obtained in example 6 of the present invention;
FIG. 25 is a phi scan of the (110) plane of the single crystal nickel ferrite film obtained in example 6 of the present invention;
FIG. 26 is a VSM of the single crystal nickel ferrite thin film obtained in example 6 of the present invention;
FIG. 27 is an XRD pattern of a polycrystalline nickel ferrite thin film obtained in comparative example 1 of the present invention;
FIG. 28 is an XRD pattern of the polycrystalline nickel ferrite thin film obtained in comparative example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples and comparative examples were obtained from conventional commercial sources or can be obtained by a method of the prior art, unless otherwise specified. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
The embodiment provides a single crystal nickel ferrite film prepared by room temperature magnetron sputtering, which comprises the following specific preparation method:
the method comprises the following steps: weighing ferrous sulfate heptahydrate, nickel sulfate hexahydrate and equivalent ammonium oxalate according to the proportion of nickel ferrite, and respectively dissolving the ferrous sulfate heptahydrate, the nickel sulfate hexahydrate and the equivalent ammonium oxalate into deionized water at about 60 ℃ to prepare solutions with the concentration of 0.5 mol/L; under the condition of violent stirring, quickly injecting an ammonium oxalate solution into a metal sulfate solution to generate yellow-green precipitates; washing the precipitate by a suction filtration method, and drying in a drying oven at 70 ℃ for 4 hours to obtain oxalate precursor powder of the nickel ferrite.
Step two: putting oxalate precursor powder of the nickel ferrite into a box-type furnace, heating to 400 ℃ at the heating rate of 2 ℃/min for pre-sintering, and taking out after heat preservation for 5 hours; fully grinding the pre-sintered powder, secondarily sintering at 600 ℃ for 5 hours, taking out, fully grinding and refining.
Step three: weighing 60g of fully ground nickel ferrite powder, dropwise adding 3mL of absolute ethyl alcohol serving as a binder, uniformly mixing, grinding and granulating; pouring into a mold with an inner diameter of 76mm, stably and slowly applying pressure to 45MPa by using a jack, and maintaining the pressure for 30 min; and demolding the formed target blank, placing the molded target blank on an alumina sintering plate, putting the molded target blank into a box-type furnace, raising the temperature to 600 ℃ at the heating rate of 1 ℃/min, preserving the heat for 2h, raising the temperature to 1000 ℃ for 8h, cooling the target blank along with the furnace, and taking out the target blank when the temperature is reduced to below 30 ℃ to obtain the nickel ferrite target material with the diameter of 76mm and the thickness of about 3 mm.
Step four: selecting a PMNPT single crystal substrate in the (110) direction, placing the substrate in acetone, performing ultrasonic treatment for 15min, and placing the substrate in absolute ethyl alcoholPerforming ultrasonic treatment for 15min, clamping the substrate, washing with absolute ethanol, and blow-drying with nitrogen; adhering a substrate on a sample support by using a high-temperature adhesive tape, and placing the substrate on a sample rack of a sputtering chamber of magnetron sputtering equipment; placing the target material of nickel ferrite on a target holder of a sputtering chamber of magnetron sputtering equipment, adjusting the distance between the target material and a substrate to be 5.5cm, and vacuumizing to a preset background vacuum of 4.0 multiplied by 10-5-5.50×10-5Pa; introducing pure argon into the sputtering chamber, adjusting the gas flow to 10sccm, adjusting the gas pressure and power to start the glow, wherein the glow starting gas pressure is not less than 3.0Pa, and the glow starting power is not less than 50W; after glow starting, adjusting the sputtering pressure to be 0.5Pa, the sputtering power to be 200W, starting coating after stabilization, and the sputtering time is 300 s; and after the sputtering is finished, the power supply of the target is closed, and the gas circuit is closed, so that the single crystal nickel ferrite film deposited on the substrate can be directly obtained.
FIGS. 1 to 6 are respectively an XRD pattern of a (110) plane, an XRD pattern of a (100) plane, a phi scan pattern of a (100) plane, a rocking curve diagram, an XRR pattern and a VSM pattern of the single-crystal nickel ferrite thin film obtained in example 1. The test results shown in fig. 1 to 3 show that the single crystal nickel ferrite thin film obtained in example 1 grows along the (110) crystal plane of the PMNPT single crystal substrate, and no impurity phase occurs. From the phi scan of FIG. 3, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (110) [100 ]]‖PMNPT(110)[100]. As can be seen from the rocking graph of FIG. 4, the full width at half maximum of the (400) diffraction peak is 2.2, indicating that the crystallization quality of the film is good. Fitting the XRR results of FIG. 5 revealed that the film thickness was 71 nm. As can be seen from the VSM graph of FIG. 6, the thin film obtained in this example exhibited ferrimagnetism at room temperature and saturation magnetization Ms118emu/cc, residual magnetization BrIs 25emu/cc, coercive force Hc979 Oe.
Example 2
The method for preparing the single crystal nickel ferrite film by room temperature magnetron sputtering of the present example is different from that of example 1 only in that the sputtering time of the present example is 2248s, and the rest is the same as that of example 1.
The single crystal nickel ferrite thin film obtained in example 2 was changed only in the sputtering time length compared to the single crystal nickel ferrite thin film obtained in example 1,the film thickness was 500 nm. FIGS. 7 to 10 are respectively an XRD pattern of the (110) plane, an XRD pattern of the (100) plane, a phi scan pattern of the (100) plane and a VSM pattern of the single-crystal nickel ferrite thin film obtained in example 2. The test results shown in fig. 7-8 show that the single crystal nickel ferrite thin film obtained in example 2 still grows along the (110) crystal plane of the PMNPT single crystal substrate, and no impurity phase occurs. From the phi scan of fig. 9, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (110) [100 ]]‖PMNPT(110)[100]. As is clear from FIG. 10, the thin film obtained in this example exhibited ferrimagnetism and saturation magnetization M at room temperatures185emu/cc, residual magnetization Br38emu/cc, coercive force HcIs 700 Oe.
Example 3
The method for preparing the single crystal nickel ferrite film by room temperature magnetron sputtering in this example is different from that of example 1 only in that the PMNPT single crystal substrate in the (100) direction is selected in the fourth step of this example, and the rest is the same as that of example 1.
FIGS. 11 to 14 are respectively an XRD pattern of the (100) plane, an XRD pattern of the (110) plane, a phi scan pattern of the (110) plane and a VSM pattern of the single-crystal nickel ferrite thin film obtained in example 3. The test results shown in FIGS. 11 to 12 show that the single crystal nickel ferrite thin film obtained in example 3 grows along the (100) crystal plane of the PMNPT single crystal substrate, and no impurity phase occurs. From the phi scan of fig. 13, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (100) [110 ]]‖PMNPT(100)[110]. As can be seen from the VSM chart in FIG. 14, the thin film obtained in this example exhibited ferrimagnetism at room temperature and saturation magnetization Ms90emu/cc, residual magnetization Br31emu/cc, coercive force HcIs 2596 Oe.
Example 4
The difference between the method for preparing the single crystal nickel ferrite film by room temperature magnetron sputtering and the method of the embodiment 1 is that the PMNPT single crystal substrate in the (100) direction is selected in the fourth step of the embodiment, the sputtering time is 2128s, and the rest is the same as the embodiment 1.
FIGS. 15 to 18 show single crystal ferronickel obtained in example 4An XRD pattern of a (100) plane of the ferrite film, an XRD pattern of a (110) plane, a phi scan pattern and a VSM pattern of the (110) plane. The test results shown in fig. 15-16 show that the single crystal nickel ferrite thin film obtained in example 4 grows along the (100) crystal plane of the PMNPT single crystal substrate, and no impurity phase occurs. From the phi scan of FIG. 17, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (100) [110 ]]‖PMNPT(100)[110]. As can be seen from the VSM chart in FIG. 18, the thin film obtained in this example exhibited ferrimagnetism and saturation magnetization M at room temperatures114emu/cc, residual magnetization Br16emu/cc, coercive force Hc349 Oe.
Example 5
The method for preparing the single crystal nickel ferrite film by room temperature magnetron sputtering in this example is different from that of example 1 only in that the STO single crystal substrate in the (100) direction is selected in the fourth step of this example, and the rest is the same as that of example 1.
FIGS. 19 to 22 are respectively an XRD pattern of the (100) plane, an XRD pattern of the (110) plane, a phi scan pattern of the (110) plane and a VSM pattern of the single-crystal nickel ferrite thin film obtained in example 5. The test results shown in fig. 19 to 20 show that the single crystal nickel ferrite film obtained in example 5 grows along the (100) crystal plane of the PMNPT single crystal substrate, and no impurity phase appears. From the phi scan of FIG. 21, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (100) [110 ]]‖PMNPT(100)[110]. From the VSM chart of FIG. 22, it can be seen that the thin film obtained in this example exhibits ferrimagnetism and saturation magnetization M at room temperatures97emu/cc, residual magnetization Br36emu/cc, coercive force Hc2583 Oe.
Example 6
The method for preparing the single crystal nickel ferrite film by room temperature magnetron sputtering in the present example is different from that of example 1 only in that the MgO single crystal substrate in the (100) direction is selected in the fourth step of the present example, and the rest is the same as that of example 1.
FIGS. 23 to 26 are respectively an XRD pattern of the (100) plane, an XRD pattern of the (110) plane, a phi scan pattern of the (110) plane and a VSM pattern of the single-crystal nickel ferrite thin film obtained in example 6. Bonding ofThe test results in fig. 23 to 24 show that the single crystal nickel ferrite thin film obtained in example 6 grows along the (100) crystal plane of the PMNPT single crystal substrate, and no impurity phase appears. From the phi scan of FIG. 25, it can be seen that the nickel ferrite and PMNPT diffraction peaks correspond one-to-one, and the in-plane epitaxial orientation is better, indicating that the epitaxial relationship between the film and the substrate is NFO (100) [110 ]]‖PMNPT(100)[110]. From the VSM chart of FIG. 26, it can be seen that the thin film obtained in this example exhibits ferrimagnetism and saturation magnetization M at room temperatures73emu/cc, residual magnetization BrIs 4emu/cc, coercive force HcIs 121 Oe.
Comparative example 1
The method for preparing the nickel ferrite thin film in this example is different from that in example 1 in that in the fourth step of this example, an amorphous substrate of Corning glass is selected, the sputtering time is 3600s, and the rest is the same as that in example 1.
FIG. 27 is an XRD pattern of the polycrystalline nickel ferrite thin film obtained in comparative example 1. The peaks appearing in FIG. 27 are all the peaks that should be found in ferrite, and among them, the (400) and (800) peaks are much stronger than the (311) main peak, sharp in peak shape and small in full width at half maximum, indicating that the film is a polycrystalline film with good crystallinity and preferred orientation of (100).
Comparative example 2
The method for preparing the nickel ferrite thin film of this example is different from that of example 1 in that a single crystal Si substrate in the (100) direction is selected in the fourth step of this example, the sputtering time is 3600s, and the rest is the same as that of example 1.
FIG. 28 is an XRD pattern of the polycrystalline nickel ferrite thin film obtained in comparative example 2. As can be seen from fig. 28, comparative example 2 also obtained a polycrystalline thin film having good crystallinity and a preferred orientation of (100), in agreement with the results of comparative example 1.
NFO in FIGS. 1-3, 7-9, 11-13, 15-17, 19-21, 23-25, and 27-28 all represent nickel ferrite (NiFe)2O4)。
According to the test results, the self-made nickel ferrite target material is used, the room-temperature magnetron sputtering method is adopted to directly prepare the spinel-phase single crystal nickel ferrite film on the single crystal substrate under the conditions of selecting the proper single crystal substrate and sputtering, the substrate does not need to be heated or subjected to subsequent heat treatment in the sputtering process, and the method is simple to operate and high in repeatability.
The single crystal nickel ferrite film provided by the invention has wide application prospect in electronic devices, communication equipment or computers, and is particularly suitable for chip electronic devices adopting a low-temperature co-firing technology.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A method for preparing a single crystal nickel ferrite film is characterized by comprising the following steps: the method comprises the following steps:
preparing a single crystal nickel ferrite film on a single crystal substrate by adopting a nickel ferrite target material through magnetron sputtering at room temperature;
the lattice mismatch degree of the single crystal substrate and the nickel ferrite is less than 6.5 percent;
the preparation method of the nickel ferrite target material comprises the following steps:
1) preparing nickel ferrite precursor powder by an oxalate coprecipitation method;
2) sintering the nickel ferrite precursor powder to obtain nickel ferrite powder;
3) pressing and sintering the nickel ferrite powder to obtain a nickel ferrite target material; the sintering is specifically carried out by heating to 550-650 ℃ at a heating rate of 0.5-1.5 ℃/min, keeping the temperature for 1.5-2.5 h, heating to 900-1100 ℃ at a heating rate of 0.5-1.5 ℃/min, and keeping the temperature for 7-9 h;
in the magnetron sputtering, the distance between the substrate and the target is 5 cm-6 cm; the sputtering atmosphere is argon; the flow rate of the sputtering gas is 10sccm to 20 sccm; the sputtering pressure is 0.2Pa to 0.5 Pa; the sputtering power is 150W-250W.
2. The method of preparing a single crystal nickel ferrite thin film according to claim 1, characterized in that: the preparation method of the nickel ferrite target comprises the following steps of 1), specifically, mixing an ammonium oxalate solution and a metal salt solution for reaction to obtain nickel ferrite precursor powder; the metal salt comprises ferrous salt and nickel salt.
3. The method of preparing a single crystal nickel ferrite thin film according to claim 1, characterized in that: in the step 3) of the preparation method of the nickel ferrite target material, the nickel ferrite powder and the binder are mixed, granulated and then pressed.
4. The method of preparing a single crystal nickel ferrite thin film according to claim 3, characterized in that: the binder comprises ethanol; the pressing pressure is 40 MPa-45 MPa, and the pressure maintaining time is 20 min-30 min.
5. The method of manufacturing a single crystal nickel ferrite thin film according to claim 1, characterized in that: the single crystal substrate comprises a magnesium oxide substrate, a lead magnesium niobate titanate substrate or a strontium titanate substrate.
6. A single crystal nickel ferrite thin film produced by the method of any one of claims 1 to 5.
7. The application of the single crystal nickel ferrite film in electronic devices, communication equipment or computers is characterized in that: the single crystal nickel ferrite thin film is obtained by the method of any one of claims 1 to 5, or the single crystal nickel ferrite thin film of claim 6.
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