CN116180067B - Preparation method of high-temperature ferromagnetic aluminum cobalt oxide parallel orientation nano-sheet array material - Google Patents
Preparation method of high-temperature ferromagnetic aluminum cobalt oxide parallel orientation nano-sheet array material Download PDFInfo
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/64—Treatment of refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/66—Treatment of aluminium or alloys based thereon
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Abstract
The invention provides a preparation method of a high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material, and belongs to the technical field of nano-materials. With Al 50 Co 50 The alloy melt-spun piece is a precursor master alloy and a substrate, and is prepared by combining a hydrothermal method and a dealloying method in Al 50 Co 50 The alloy melt-spun piece surface self-assembles to form aluminum cobalt oxide parallel orientation nano-sheet array material vertical to the matrix. Parallel orientation of nanoplatelets parallel to matrix grains [001]]The crystal orientation is consistent. In addition, the aluminum cobalt oxide nano-sheet array material has high-temperature ferromagnetism, the Curie temperature reaches 919K, and the maximum magnetic saturation strength reaches 5.22emu/g. The invention overcomes the technical problem that the lamellar direction of the nano-sheets is difficult to control in the current in-situ preparation process of the parallel orientation nano-sheets, has simple preparation process and low production cost, has the advantage of mass production, and has good application potential in the aspect of nano-ferromagnetic materials.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a high-temperature aluminum cobalt oxide parallel orientation nano sheet array material.
Background
The parallel orientation nano material not only can improve the macroscopic performance of the material through strong plasma, electron and exciton coupling, but also can provide direct and rapid ion, electron or molecule transmission paths, so that the parallel orientation nano material has wide application in various industrial fields such as sensing, catalysis, energy storage and the like. Currently, one-dimensional (nanowires, nanotubes, and nanorods) parallel oriented nanomaterials are the most studied and used materials, such as zinc oxide nanowire arrays applied to piezoelectric nanogenerators, and carbon nanotube arrays applied to field effect transistors. Two-dimensional nanomaterials possess unique electronic, mechanical, and optical properties that enable a large number of two-dimensional nanomaterials to be discovered and fabricated. However, the preparation of two-dimensional parallel oriented nanomaterials remains a difficult challenge. Compared with the one-dimensional parallel orientation nanomaterial (only control the growth direction), the two-dimensional parallel orientation nanomaterial has the difficulty of controlling the growth direction and the spatial orientation of the two-dimensional parallel orientation nanomaterial at the same time.
At present, two strategies exist for preparing the two-dimensional parallel orientation nano material, one strategy is an in-situ strategy, namely, the arrangement is completed in the growth process of the two-dimensional nano material; the other is an ex-situ strategy, namely, the two-dimensional nano material with any orientation is prepared first, and then the arrangement is completed. Most of the two-dimensional parallel oriented nanomaterials reported are prepared by an ex-situ method, for example, highly ordered layered films can be prepared by parallel stacking disordered two-dimensional nanoplatelets (mxnes (two-dimensional carbides and nitrides of transition metals), graphene oxide, and the like) by spin coating, ice template, mechanical shearing, solution evaporation, and the like. However, the two-dimensional parallel oriented nanomaterial grown by in-situ method is mostly parallel to the substrate, so that the preparation of large single crystal thin film is realized, and few researchers aim at the two-dimensional parallel oriented nanomaterial of the in-situ grown vertical substrate. In 2013, chi et al reported a method for in-situ growth of gallium arsenide parallel orientation Nano-plate array material perpendicular to a substrate by using electron beams to etch Nano-stripes with certain orientation on the substrate for the first time, however, the method has severe requirements on experimental environment, is high in cost, and cannot realize mass production (Chi et al, nano Letter,2013,13,2506-2515). In 2018, wang et al grown diamond parallel oriented nanoplates perpendicular to the substrate in situ on a diamond single crystal substrate using crystal plane epitaxy, but still were interspersed with a few other oriented nanoplates due to the presence of equivalent crystal planes (Wang et al, nanoscales, 2018,10,2812-2819). In the same year, huang et al reported a method for in situ growth of parallel oriented graphene arrays perpendicular to a substrate using an applied electric field (Huang et al ACS Applied Materials & Interfaces,2019,11,1294-1302). The above-mentioned growth methods all use chemical vapor deposition, and although the two-dimensional parallel oriented nanomaterial prepared by chemical vapor deposition has good crystal quality, it generally requires high reaction temperature (higher than 500 ℃) and vacuum environment, which greatly limits the choice of substrate and mass production thereof. In addition, the two-dimensional nanomaterial prepared by chemical vapor deposition is mostly perpendicular to the substrate only, and cannot be parallel to each other, which again demonstrates the limitations of the method. In view of this, it has become one of the main research directions in the art how to invent a simple, mass-producible and low-cost method for preparing two-dimensional parallel oriented nanomaterial in situ.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a preparation method of an aluminum cobalt oxide parallel orientation nano-sheet array material, which is used for solving the technical problems of disordered space orientation, high cost, high environmental requirement, low efficiency and the like existing in the conventional preparation of the parallel orientation nano-sheet array material of a vertical substrate in situ. The aluminum cobalt oxide parallel orientation nano-sheet array material prepared by the method provided by the invention has good high-temperature ferromagnetism.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a preparation method of a high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material, which is characterized by comprising the following steps of:
(1) Preparing a metal block according to an atomic ratio, selecting a vacuum induction smelting furnace for smelting, wherein the rated temperature is 1700 ℃, and cooling along with the furnace to obtain an alloy cast ingot;
(2) Polishing the obtained alloy cast ingot to remove the outermost oxide film, and crushing the alloy cast ingot into small blocks of 1cm multiplied by 1 cm;
(3) Weighing polished and crushed alloy ingot small blocks, putting the polished and crushed alloy ingot small blocks into a quartz tube, putting the quartz tube into a vacuum melt-spinning machine, re-melting the alloy ingot small blocks, and rapidly solidifying to prepare an alloy melt-spinning piece;
(4) Pouring the measured NaOH solution into a polytetrafluoroethylene lining, adding an alloy strip casting sheet into the polytetrafluoroethylene lining, immediately putting the polytetrafluoroethylene lining into a reaction kettle, screwing down a nut of the reaction kettle, ensuring that the reaction kettle is airtight, and setting a reaction time-temperature program;
(5) After the reaction is finished, cooling the reaction kettle to room temperature, taking out the polytetrafluoroethylene lining from the reaction kettle, pouring out waste alkali liquor, repeatedly cleaning the prepared product with deionized water in an ultrasonic cleaning machine for 2-4 times, and carrying out ultrasonic treatment for 1-3min each time; after the cleaning is finished, the product is put into a sample bottle, and is dried on an electric hot plate for 7-9 hours at 85-95 ℃ to obtain the aluminum cobalt oxide parallel orientation nano-sheet array material with a vertical substrate.
Further, the metal block in the step (1) is prepared from Al (99.99%), co (99.99%) according to an atomic ratio of 50:50; the alloy cast ingot is Al 50 Co 50 。
Further, the melt-spinning speed of the melt-spinning piece in the step (3) is 25m/s, and the protective atmosphere is argon.
Further, the concentration of the NaOH solution in the step (4) is 1-10 mol/L; the addition amount of the NaOH solution is 100mL; the dosage of the Al50Co50 melt-spun sheet is 2g. .
Further, the reaction kettle time-temperature program in the step (4) is that the reaction kettle is heated at room temperature for 15min to 70 ℃, then is kept at 70 ℃ for 10min, and is further heated for 10min to 100 ℃, and finally is kept at 100 ℃ for 10min to 300min, and the reaction is finished.
Furthermore, the front (free surface) and the back (roller-sticking surface) of the alloy strip casting substrate can grow the aluminum cobalt oxide parallel orientation nano sheet array material.
Further, the aluminum cobalt oxide parallel orientation nano-sheet array material is perpendicular to the alloy strip casting sheet substrate, nano-sheets grown on the surfaces of single crystal grains of the substrate are parallel to each other, and parallel orientation nano-sheet array materials grown on the surfaces of adjacent crystal grains have a certain included angle.
Further, the average thickness of the aluminum cobalt oxide parallel orientation nano-sheet is 19nm-40nm, and the components are Al 30～40 Co 30～40 O 20～40 The crystal structure is cubic crystal system, spinel crystal structure type and space groupPDF card No.09-0418。
Further, when the aluminum cobalt oxide parallel orientation nano-sheet array material is used for 300K, the magnetic saturation intensity is 1.89-5.22 emu/g, the coercive force is 446-593 Oe, the Curie temperature is 919K, and the material has high-temperature ferromagnetism.
The growth mechanism of the invention is as follows: al is added with 50 Co 50 The alloy strip-casting piece is put into NaOH solution, and Al on the surface of the strip-casting piece can be corroded by alkali solution to form Al-containing alloy strip-casting piece because Al element is active metal in the initial stage of reaction 3+ The rest Co element is oxidized by oxygen and hydroxide dissolved in the solution to form Co-containing solution 2+ Is an oxide of various forms of (a) and (b). When the reaction product element in the solution reaches supersaturation, the reaction product element can be positioned in Al under the assistance of the hydrothermal atmosphere of the reaction kettle 50 Co 50 The surface of the alloy melt-spun piece is self-assembled, and a compact buffer layer parallel to the substrate is formed, wherein the buffer layer contains three elements of Al, co and O. Then, when the supersaturation degree of the solution is reduced to a certain degree, the nano-sheets start to orient and form nuclei and grow on the buffer layer, at the moment, the self-assembly behavior of the nano-sheets is the same as that of forming the buffer layer, the elements contained in the nano-sheets are the same as that of the buffer layer, and finally, with the extension of the reaction time, the nano-sheets can grow on Al 50 Co 50 And forming a layer of aluminum cobalt oxide parallel orientation nano-sheets perpendicular to the substrate on the alloy melt-spun sheet.
As a further improvement of the invention, the first requirement for preparing the aluminum cobalt oxide parallel orientation nano-sheet is Al 50 Co 50 The exposed crystal face of the crystal grain on the surface of the alloy melt-spun piece comprises [001]]And (5) crystal orientation. In addition, the Al 50 Co 50 The alloy strip-casting sheet is composed of AlCo phase, cubic crystal system and space groupPDF card nos. 44-1115.AlCo phase is difficult to corrode in alkali solution, and therefore Al 50 Co 50 The alloy melt-spun piece can serve as a precursor of reaction and can serve as a substrate for loading the buffer layer and parallel orientation nano-sheets.
As a further improvement of the invention, one of the most important requirements for preparing aluminum cobalt oxide parallel oriented nanoplatelets is that the [101] crystal orientation of the buffer layer is parallel to the [001] crystal orientation of the substrate, and the two can be perfectly lattice matched (the (101) crystal plane spacing of the buffer layer is 0.572nm, and the (001) crystal plane spacing of the substrate is 0.286nm, which is exactly twice as large as the latter). Furthermore, the buffer layer has mainly two roles: firstly, the conditions for vertical growth of the nano-sheets are provided, and secondly, the conditions for orientation nucleation and growth of the nano-sheets are provided.
As a further improvement of the invention, a third requirement for preparing aluminum cobalt oxide parallel oriented nanoplatelets is that the buffer layer and nanoplatelets have the same crystal structure (cubic system, spinel crystal structure type, space group)PDF card No.09-0418)。
As a further improvement of the invention, the average thickness of the aluminum cobalt oxide parallel oriented nano-sheets is between 19nm and 40nm, and the large plane of the nano-sheets is hexagonal.
The second purpose of the invention is that the prepared aluminum cobalt oxide parallel orientation nano-sheet has high-temperature ferromagnetism.
The experimental results show that: the maximum magnetic saturation strength of the aluminum cobalt oxide parallel orientation nano-sheet prepared by the method can reach 5.22emu/g at 300K; the Curie temperature can reach 919K, which proves that the aluminum cobalt oxide parallel orientation nano-sheet has high-temperature ferromagnetism.
Compared with the prior art, the invention has the beneficial effects that:
firstly, by adopting the technical scheme of the invention, the technical problem that the space orientation of the nano-sheet is difficult to control in the current process of preparing the parallel orientation nano-sheet of the vertical substrate in situ can be overcome by a perfect lattice matching strategy of the buffer layer and the substrate along a certain crystal direction, so that the aluminum cobalt oxide parallel orientation nano-sheet array of the vertical substrate is obtained.
Secondly, the technical scheme of the invention adopts a hydrothermal method and a dealloying method which are combined, and essentially belongs to the liquid phase method for in-situ preparation of the parallel orientation nano-sheets of the vertical substrate, and compared with the chemical vapor deposition method (gas phase method) mentioned in the background of the invention, the liquid phase method has the remarkable advantages of low cost, simple operation and mass production. In addition, the method can prepare the large-area aluminum cobalt oxide parallel orientation nano-sheet array on the front side (free surface) and the back side (roller surface) of the alloy melt-spun sheet at the same time, and the gas phase method can only prepare the parallel orientation nano-sheet on the front side of the substrate. Meanwhile, in the growth process of the nano-sheets, the thickness and the orientation of the aluminum cobalt oxide parallel orientation nano-sheets can be effectively controlled by changing the concentration of alkali liquor, the reaction time and the temperature.
Thirdly, the alloy design component in the technical proposal of the invention is Al 50 Co 50 The phase composition is AlCo phase, which is difficult to corrode as a precursor master alloy, which is a disadvantage in the traditional design strategy of dealloying experimental components (generally Al content is more than 75% and matrix alloy is corroded completely), but we ingeniously utilize this point, so that it can be used as both a precursor master alloy and a substrate for loading a buffer layer and parallel oriented nano-sheets.
Drawings
FIG. 1 is a scanning electron microscope image of the front (a and b) and back (c and d) sides of the product obtained in example 1;
FIG. 2 is a single nanoplatelet large plane transmission electron microscope image (a) and a selected area electron diffraction image (b) of the product obtained in example 1;
FIG. 3 is a single nanoplatelet large plane transmission electron microscope high resolution image (a) and cross-section high resolution image (b) of the product obtained in example 1;
FIG. 4 is an electron diffraction image (e-g) of adjacent three-grain scanning electron microscope images (a-d) and corresponding selected areas of the substrate of the product obtained in example 1;
FIG. 5 is a cross-sectional high-resolution image (a) and an inverse Fourier transform image (b-d) of the corresponding location of the product obtained in example 1;
FIG. 6 is a hysteresis curve of the product obtained in example 1;
FIG. 7 is a scanning electron microscope image of the front (a and b) and back (c and d) sides of the product obtained in example 2;
FIG. 8 is a hysteresis curve of the product obtained in example 2;
FIG. 9 is a scanning electron microscope image of the front (a and b) reverse (c and d) sides of the product obtained in example 3;
FIG. 10 is a hysteresis curve of the product obtained in example 3;
FIG. 11 is a plot of magnetization versus temperature for the product obtained in example 3;
FIG. 12 is a front scanning electron microscope image (a and b) of the product obtained in example 4;
FIG. 13 is a front scanning electron microscope image (a and b) of the product obtained in example 5;
fig. 14 is front scanning electron microscope images (a and b) of the product obtained in example 6.
Detailed Description
The following examples are further illustrative of the invention, but not limiting thereof, and the core of the present disclosure is the preparation of aluminum cobalt oxide parallel oriented nanoplatelet array materials. The way in which the invention can be implemented is illustrated by means of specific examples.
Example 1
1.1 preparation of aluminum cobalt oxide parallel orientation nano-sheet array material, comprising the following steps:
mixing metal Al (99.99%), co (99.99%) blocks according to an atomic ratio of 50:50, selecting a vacuum induction smelting furnace for smelting, wherein the rated temperature is 1700 ℃, and cooling along with the furnace to obtain Al 50 Co 50 Alloy ingot 2kg. Then Al is obtained 50 Co 50 The alloy ingot is polished by a grinder to remove the outermost oxide film, and is crushed into small pieces of about 1cm x 1cm by a hammer. Weighing polished and crushed Al 50 Co 50 Placing 10g of alloy ingot into a quartz tube, then placing the quartz tube into a vacuum belt casting machine, setting the belt casting speed to 25m/s, and protecting the atmosphere to argon, and carrying out Al treatment 50 Co 50 Remelting small alloy ingot blocks and rapidly solidifying to prepare Al 50 Co 50 Alloy melt-spun piece. 100mL of 10mol/L NaOH solution was measured in a beaker, poured into a polytetrafluoroethylene liner, and 2g of the solution was weighedAl 50 Co 50 The alloy strip throwing piece is added into the polytetrafluoroethylene lining, then the polytetrafluoroethylene lining is immediately put into the reaction kettle, the nut of the reaction kettle is screwed down, the reaction kettle is ensured to be airtight, and the reaction time-temperature program is set, namely: heating at room temperature for 15min to 70 ℃, then preserving heat at 70 ℃ for 10min, further heating at 10min to 100 ℃, and finally preserving heat at 100 ℃ for 30min, and finishing the reaction. After the reaction is finished, the reaction kettle is cooled to room temperature, the polytetrafluoroethylene lining is taken out from the reaction kettle, the waste alkali liquid is poured out, the prepared sample is repeatedly washed for three times by deionized water in an ultrasonic cleaner, and each time is subjected to ultrasonic treatment for 2 minutes. After the cleaning is finished, the sample is put into a sample bottle, and is dried on an electric hot plate for 8 hours at 90 ℃, and then the aluminum cobalt oxide parallel orientation nano-sheet array material with a vertical substrate is obtained.
1.2 characterization of the product
Directly attaching the product prepared in 1.1 onto conductive adhesive, and observing the integral morphology and components of the product aluminum cobalt oxide parallel orientation nano-plate array by using a Zeiss Super 55 field emission scanning electron microscope, wherein the front surface (free surface) is upward and the back surface (roller surface) is upward; observing the microscopic morphology and crystal structure of the product by using a Tecnai F30 transmission electron microscope; preparing a section transmission sample of the Nano-sheet by using an FEI Helios Nano-lab 600i FIB/SEM double-beam system; and (5) observing the cross-sectional morphology of the product by using a double spherical aberration correcting JEM-ARM200F scanning transmission electron microscope. The characterization results are shown in fig. 1-5 (wherein fig. 1 is a front and back scanning electron microscope image of the product obtained in this embodiment; fig. 2 is a single nano-plate large-plane transmission electron microscope image and a selected area electron diffraction image of the product obtained in this embodiment; fig. 3 is a single nano-plate large-plane transmission electron microscope high-resolution image and a cross-section high-resolution image of the product obtained in this embodiment; fig. 4 is an adjacent three-grain scanning electron microscope image and a corresponding selected area electron diffraction image of the substrate of the product obtained in this embodiment; and fig. 5 is an inverse fourier transform image of the cross-section high-resolution image and a corresponding position of the product obtained in this embodiment).
As can be seen from FIG. 1, the obtained product grows an aluminum cobalt oxide parallel orientation nano-sheet array with a vertical substrate on the front side and the back side of the melt-spun sheet, wherein the parallel orientation of the front side growth is superior to that of the front side growthAnd the reverse side. The aluminum cobalt oxide parallel orientation nano-sheet arrays grown on adjacent grains have a certain included angle. The average thickness of the parallel orientation nano-sheet array is 24.4nm, and the average element component of the nano-sheet is Al 33 Co 36 O 31 . As can be seen from FIG. 2, the large plane of a single nanosheet is hexagonal, and the selected area electron diffraction pattern comprises two sets of diffraction spots, wherein the diffraction spots circled by white circles can be used for preliminarily obtaining that the crystal structure of the nanosheet is cubic crystal system, spinel crystal structure type and space groupPDF card No.09-0418; the diffraction spots circled by the black circles have the crystal plane spacing slightly smaller than that of the diffraction spots circled by the white circles, and the crystal structure of the nano-sheet can be preliminarily obtained to be rhombohedral system, alpha-Al 2 O 3 Crystal structure type, space group->PDF card No.10-0173. From the large-plane high-resolution picture of the nanoplatelets of fig. 3, only the lattice fringes of the cubic system can be seen, and no lattice fringes of the hexagonal system are found; the high-resolution image of the section of the nano-sheet is also a lattice fringe image of a cubic system, the lattice fringe of the hexagonal system is not found, and meanwhile {111} twin crystal defects are also included in the nano-sheet, which is very common in the growth of face-centered cubic structure crystals, so that the crystal structure of the nano-sheet can be determined to be the cubic system, the spinel crystal structure type and the space group>PDF card No.09-0418. The diffraction spots circled in the black in fig. 2 may be caused by lattice distortion due to incomplete crystallization of the edge portion positions in the nanoplatelets. As can be seen from FIG. 4, the aluminum-cobalt oxide parallel orientation nano-sheet array grown on the adjacent grains of the obtained product has a certain included angle, wherein the aluminum-cobalt oxide parallel orientation nano-sheet arrays on the grains A and B are well oriented, and the aluminum-cobalt oxide parallel orientation nano-sheet grown on the grains C is mixed with a large amount of impuritiesA quantity of disordered nanoplatelets. The FIB is utilized to cut the nano-sheet along the parallel direction of the vertical nano-sheet to prepare a section transmission sample, and the band axes of the A crystal grain and the B crystal grain are respectively [001] as can be seen from the corresponding selective electron diffraction]And the band axis of the C crystal grain is [111 ]](the direction of the axis of the band is the parallel direction of the nanoplatelets) thereby determining the growth of the aluminum cobalt oxide parallel oriented nanoplatelet array and the [001] of the substrate]The grain orientation is related. As can be seen from fig. 5 again, a buffer layer is arranged below the parallel alignment nano-sheet of aluminum cobalt oxide, the crystal structure and alignment of the buffer layer are the same as those of the nano-sheet, and the inverse fourier image of the corresponding position shows that the alignment relationship among the nano-sheet, the buffer layer and the substrate is that: [101] N //[101] B //[001] S . Analysis found that the substrate was along [001]] S Direction (001) S The surface distance is just the buffer layer and the nano-sheet edge [101]] B,N Direction (101) B,N Half of the interplanar spacing. Thus, the parallel oriented growth mechanism of the prepared product can be derived, namely: buffer layer [101]] B [001] with the crystal orientation parallel to the substrate] S The crystal orientation, both of which can be perfectly lattice matched, results in subsequent nanoplatelets along the substrate on the buffer layer [001]] S The crystal orientation is nucleated and grown, so that the aluminum cobalt oxide parallel orientation nano-sheet array vertical to the substrate is grown. Whether a buffer layer which is perfectly lattice matched with a substrate along a certain crystallographic direction can be grown is a key point for controlling the space orientation of the nano-sheets, and is also a key point for growing the nano-sheets with parallel orientation.
1.3 magnetic Property testing
The product prepared in 1.1 is tested for room temperature magnetic property by utilizing a multifunctional physical property measuring system of Quantum Design company in the United states, and the result is shown in figure 6, and the obtained product can be seen to have magnetic saturation strength of 1.89emu/g and coercivity of about 593Oe at 300K and room temperature ferromagnetism. From the black curve in the figure, the original Al can be seen 50 Co 50 The alloy melt-spun sheet has almost no magnetism, so that the ferromagnetism of the obtained product can be concluded to be derived from an aluminum-cobalt-oxygen parallel orientation nano-sheet array.
Example 2
In this example, an aluminum cobalt oxide parallel alignment nanoplatelet array material was prepared under the same conditions as in example 1 except that the heat preservation time in the reaction vessel at 100 ℃ was changed to 60 min.
According to the characterization method of example 1, the front and back sides of the product are observed by a field emission scanning electron microscope, as shown in fig. 7, the obtained product grows an aluminum cobalt oxide parallel orientation nano-sheet array material with a vertical substrate on the front and back sides of the melt-spun sheet, the parallel orientation of the nano-sheets on the front and back sides is very good, and the average thickness of the nano-sheets is 28.9nm. The structure, elemental composition and growth mechanism of the nanoplatelets are the same as those of example 1 and will not be described in detail here.
The magnetic properties of the product were measured according to the magnetic property characterization method of example 1, as shown in fig. 8, and it can be seen that the magnetic saturation strength of the obtained product can reach 2.56emu/g at 300K, the coercivity can reach about 583Oe, and the product has room temperature ferromagnetism. Original Al 50 Co 50 The alloy melt-spun sheet is the same as example 1, so it can be concluded that the ferromagnetism of the obtained product is derived from an aluminum-cobalt-oxygen parallel orientation nano-sheet array.
Example 3
In this example, an aluminum cobalt oxide parallel alignment nanoplatelet array material was prepared under the same conditions as in example 1 except that the heat preservation time in the reaction vessel at 100 ℃ was changed to 300 min.
According to the characterization method of example 1, the front and back sides of the product are observed by a field emission scanning electron microscope, as shown in FIG. 9, the obtained product grows an aluminum cobalt oxide parallel orientation nano-plate array with a vertical substrate on the front and back sides of the melt-spun piece, the parallel orientation of the nano-plates on the front and back sides is very good, the average thickness of the nano-plates is 36.7nm, and the average element component of the nano-plates is Al 35 Co 38 O 27 . The structure, elemental composition and growth mechanism of the nanoplatelets are the same as those of example 1 and will not be described in detail here.
As shown in FIG. 10, the magnetic saturation strength of the obtained product can reach 5.22emu/g and the coercivity can be seen when the magnetic performance of the product is measured according to the magnetic performance characterization method of example 1Can reach about 446Oe and has room-temperature ferromagnetism. Original Al 50 Co 50 The alloy melt-spun sheet is the same as example 1, so it can be concluded that the ferromagnetism of the obtained product is derived from an aluminum-cobalt-oxygen parallel orientation nano-sheet array. Meanwhile, the magnetization-temperature curve of the obtained product is also measured in the embodiment, the measurement result is shown in fig. 11, and the curie temperature of the sample is up to 919K, and the sample has obvious high-temperature ferromagnetism.
Comparative examples 1,2, and 3 show that the orientation of the obtained aluminum cobalt oxide parallel orientation nanoplatelet array is better and better along with the extension of the reaction time, the thickness of the nanoplatelets is increased, and the magnetic performance is also enhanced.
Example 4
In this example, an aluminum cobalt oxide parallel alignment nanoplatelet array material was prepared under the same conditions as in example 3, except that the concentration of the NaOH solution was changed to 1 mol/L.
The front side of the product was observed by field emission scanning electron microscopy according to the characterization method of example 1, as shown in fig. 12, and the obtained product grew an array of parallel oriented nano-sheets of aluminum cobalt oxide with a vertical substrate on the front side of the melt-spun sheet, but a large number of random nano-sheets were interposed between the parallel oriented nano-sheets.
Example 5
In this example, an aluminum cobalt oxide parallel alignment nanoplatelet array material was prepared under the same conditions as in example 3, except that the concentration of the NaOH solution was changed to 3 mol/L.
The front side of the product was observed by field emission scanning electron microscopy according to the characterization method of example 1, as shown in fig. 13, and the obtained product grew an array of parallel oriented nano-sheets of aluminum cobalt oxide with a vertical substrate on the front side of the melt-spun sheet, but a small amount of disordered nano-sheets were interposed between the parallel oriented nano-sheets.
Comparative examples 3,4, and 5 show that other experimental conditions remain unchanged, and the orientation of the obtained aluminum cobalt oxide parallel orientation nanoplatelet array becomes better as the concentration of the NaOH solution increases.
Example 6
In this example, an aluminum cobalt oxide parallel alignment nanoplatelet array material was prepared under the same conditions as in example 3, except that the reaction temperature was changed to room temperature.
The front side of the product was observed by field emission scanning electron microscopy according to the characterization method of example 1, as shown in fig. 14, and the obtained product grew an array of parallel oriented nano-sheets of aluminum cobalt oxide with a vertical substrate on the front side of the melt-spun sheet, but a large number of random nano-sheets were interposed between the parallel oriented nano-sheets.
Comparative examples 3,6 show that the orientation of the resulting aluminum cobalt oxide parallel oriented nanoplatelet array becomes better as the reaction temperature increases.
In combination with the above examples 1,2,3,4,5,6, it can be concluded that the preparation of the al-co-oxy parallel oriented nanoplatelet array material is influenced by external experimental conditions, such as reaction time, lye concentration and reaction temperature, in addition to the intrinsic base grain orientation. Only under the proper external experimental conditions can a buffer layer which is perfectly lattice matched with the substrate crystal grains along a certain orientation be formed, and then the parallel orientation nano-sheet array vertical to the substrate is grown.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (5)
1. The preparation method of the high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material is characterized by comprising the following steps of:
(1) Preparing a metal block according to an atomic ratio, selecting a vacuum induction smelting furnace for smelting, wherein the rated temperature is 1700 ℃, and cooling along with the furnace to obtain an alloy cast ingot;
(2) Polishing the obtained alloy cast ingot to remove the outermost oxide film, and crushing the alloy cast ingot into small blocks of 1cm multiplied by 1 cm;
(3) Weighing polished and crushed alloy ingot small blocks, putting the polished and crushed alloy ingot small blocks into a quartz tube, putting the quartz tube into a vacuum melt-spinning machine, re-melting the alloy ingot small blocks, and rapidly solidifying to prepare an alloy melt-spinning piece;
(4) Pouring the measured NaOH solution into a polytetrafluoroethylene lining, adding an alloy strip casting sheet into the polytetrafluoroethylene lining, immediately putting the polytetrafluoroethylene lining into a reaction kettle, screwing down a nut of the reaction kettle, ensuring that the reaction kettle is airtight, and setting a reaction time-temperature program;
(5) After the reaction is finished, cooling the reaction kettle to room temperature, taking out the polytetrafluoroethylene lining from the reaction kettle, pouring out waste alkali liquor, repeatedly cleaning the prepared product with deionized water in an ultrasonic cleaning machine for 2-4 times, and carrying out ultrasonic treatment for 1-3min each time; after the cleaning is finished, the product is put into a sample bottle, and is dried on an electric heating plate for 7-9 hours at 85-95 ℃ to obtain an aluminum cobalt oxide parallel orientation nano-sheet array material with a vertical substrate;
the reaction kettle time-temperature program is that the reaction kettle is heated at room temperature for 15min to 70 ℃, then is kept at 70 ℃ for 10min, and is further heated for 10min to 100 ℃, and finally is kept at 100 ℃ for 10min to 300min, and the reaction is finished;
the front and the back of the alloy strip substrate can grow aluminum cobalt oxide parallel orientation nano-sheet array materials;
when the aluminum cobalt oxide parallel orientation nano sheet array material is at 300K, the magnetic saturation strength is 1.89-5.22 emu/g, the coercive force is 446-593 Oe, the Curie temperature is 919K, and the material has high-temperature ferromagnetism;
the metal block materials in the step (1) are Al and Co, and are mixed according to the atomic ratio of 50:50; the alloy cast ingot is Al 50 Co 50 。
2. The method for preparing the high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material according to claim 1, which is characterized in that: and (3) the melt-spinning speed of the melt-spinning piece is 25m/s, and the protective atmosphere is argon.
3. The method for preparing the high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material according to claim 1, which is characterized in that: the concentration of the NaOH solution in the step (4) is 1-10 mol/L, and the addition amount of the NaOH solution is 100mL; the dosage of the Al50Co50 melt-spun sheet is 2g.
4. The method for preparing the high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material according to claim 1, which is characterized in that: the aluminum cobalt oxide parallel orientation nano-sheet array material is perpendicular to the alloy strip casting sheet substrate, nano-sheets grown on the surfaces of single crystal grains of the substrate are parallel to each other, and parallel orientation nano-sheet array materials grown on the surfaces of adjacent crystal grains have a certain included angle.
5. The method for preparing the high Wen Tieci aluminum cobalt oxide parallel orientation nano-sheet array material according to claim 1, which is characterized in that: the average thickness of the aluminum cobalt oxide parallel orientation nano-sheet is 19nm-40nm, and the components are Al 30~ 40 Co 30~40 O 20~40 The crystal structure is cubic crystal system, spinel crystal structure type and space group，PDF card No. 09-0418。
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| CN102921960A (en) * | 2012-11-19 | 2013-02-13 | 扬州大学 | Preparation method of magnetic cobalt nanometer material |
| CN113215559A (en) * | 2021-04-01 | 2021-08-06 | 北京科技大学 | Class I parallel orientation (Al-Co)xOyPreparation method of nanosheet |
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| CN102921960A (en) * | 2012-11-19 | 2013-02-13 | 扬州大学 | Preparation method of magnetic cobalt nanometer material |
| CN113215559A (en) * | 2021-04-01 | 2021-08-06 | 北京科技大学 | Class I parallel orientation (Al-Co)xOyPreparation method of nanosheet |
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