CN113753847A - Thin film material with controllable crystal face orientation and preparation method thereof - Google Patents
Thin film material with controllable crystal face orientation and preparation method thereof Download PDFInfo
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- CN113753847A CN113753847A CN202111055113.8A CN202111055113A CN113753847A CN 113753847 A CN113753847 A CN 113753847A CN 202111055113 A CN202111055113 A CN 202111055113A CN 113753847 A CN113753847 A CN 113753847A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/362—Laser etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0128—Processes for removing material
- B81C2201/0143—Focussed beam, i.e. laser, ion or e-beam
Abstract
The invention discloses a thin film material with controllable crystal face orientation and a preparation method thereof, wherein the method comprises the following steps: collecting femtosecond laser on a substrate, and processing a three-dimensional structure array on the surface of the substrate; collecting femtosecond laser on the three-dimensional structure array, and processing a three-dimensional super-wetting template array on the surface of the substrate; dropwise adding water-soluble crystal particles onto a three-dimensional super-wetting template array, and heating the substrate to obtain a thin film material with controllable crystal face orientation; wherein the three-dimensional structure array comprises a plurality of three-dimensional structures, and the size and shape of the plurality of three-dimensional structures are determined by the size and shape of the water-soluble crystal particles. According to the invention, the water-soluble crystal particles are adsorbed by the super-wettability of the three-dimensional super-wetting template array, and the diffusion of the water-soluble crystal particles is limited by utilizing the surface energy difference between a processing area and an unprocessed area, so that the thin film material with consistent crystal grain orientation and uniform size is obtained, the thin film growth speed is high, the preparation method is simple, and the preparation process is not restricted by materials and substrates.
Description
Technical Field
The invention relates to the technical field of micro-nano processing, in particular to a thin film material with controllable crystal face orientation and a preparation method thereof.
Background
The crystal face orientation, the components, the grain size, the interface stress and the like of the film can greatly influence the film performance, films with different preferred orientations can show different properties, and the film can be applied to microelectronic technology, photoelectronic technology, MEMS technology and the like according to different requirements. How to prepare a film with good performance meets the requirements of integrated devices, and becomes a key link for restricting the application of the film.
The film is mainly prepared by a molecular beam epitaxy method in the prior art, but the method has slow film growth speed and requires strict matching of materials and a substrate.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a thin film material with controllable crystal plane orientation and a preparation method thereof, aiming at solving the problems that the existing thin film preparation method is slow in thin film growth speed and requires strict matching between the material and the substrate.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of a thin film material with controllable crystal face orientation comprises the following steps:
collecting femtosecond laser on a substrate, and processing a three-dimensional structure array on the surface of the substrate through the femtosecond laser;
collecting femtosecond laser on the three-dimensional structure array, and processing a three-dimensional super-wetting template array on the surface of the substrate through the femtosecond laser;
dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, and heating the substrate to obtain a thin film material with controllable crystal face orientation; wherein the three-dimensional structure array comprises a plurality of three-dimensional structures having sizes and shapes determined by sizes and shapes of the water-soluble crystal particles.
The preparation method of the film material with controllable crystal face orientation comprises the following steps of preparing a substrate, and preparing a film material with controllable crystal face orientation, wherein the substrate is one of glass, sapphire, quartz and a silicon wafer.
The preparation method of the film material with controllable crystal face orientation comprises the following steps of (1) collecting femtosecond laser on a substrate: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 3000-5000 mW, and the scanning times are 3-6.
The preparation method of the film material with controllable crystal plane orientation comprises the following steps of before the step of focusing the femtosecond laser on the substrate:
polishing the substrate;
and washing and drying the polished substrate.
The preparation method of the film material with controllable crystal face orientation comprises the following steps of (1) collecting femtosecond laser on a three-dimensional structure array: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 1500-3000 mW, and the scanning times are 1-2.
The preparation method of the film material with controllable crystal face orientation comprises the step of preparing a water-soluble crystal particle, wherein the water-soluble crystal particle is one or more of a metal organic framework material, a magnetic material, an oxide and a sulfide.
The preparation method of the film material with the controllable crystal face orientation comprises the following steps of heating at the temperature of 30-80 ℃ for 5-10 min.
The preparation method of the film material with controllable crystal face orientation comprises the following steps of preparing a plurality of three-dimensional structures, and preparing a film material with controllable crystal face orientation, wherein the three-dimensional structures are in one or more of hemispheres, tetrahedrons, octahedrons and hexadecahedrons.
The preparation method of the film material with the controllable crystal face orientation comprises the following steps that the heights of the three-dimensional structures are 0.03-0.06 mm, and the lengths and the widths of the three-dimensional structures are larger than or equal to 0.2mm and smaller than or equal to the lengths and the widths of the water-soluble crystal particles.
The film material with the controllable crystal face orientation is prepared by adopting the preparation method of the film material with the controllable crystal face orientation.
Has the advantages that: according to the invention, the water-soluble crystal particles are adsorbed by the super-wettability of the three-dimensional super-wetting template array, and the diffusion of the water-soluble crystal particles is limited by utilizing the surface energy difference between a processing area and an unprocessed area on the surface of the substrate, so that the film material with the controllable crystal face orientation, which has consistent crystal grain orientation and uniform size, is obtained, the film growth speed is high, the preparation method is simple, and the preparation process is not restricted by the material and the substrate.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a thin film material with controllable crystal plane orientation according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a thin film material with controllable crystal plane orientation provided in an embodiment of the present invention.
Detailed Description
The invention provides a preparation method of a film material with controllable crystal plane orientation, and the invention is further described in detail below in order to make the purpose, technical scheme and advantages of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The crystal face orientation, the components, the grain size, the interface stress and the like of the film can greatly influence the film performance, films with different preferred orientations can show different properties, and the film can be applied to microelectronic technology, photoelectronic technology, MEMS technology and the like according to different requirements. How to prepare a film with good performance meets the requirements of integrated devices, and becomes a key link for restricting the application of the film. The film is mainly prepared by a molecular beam epitaxy method in the prior art, but the method has slow film growth speed and requires strict matching of materials and a substrate.
In order to solve the above problem, as shown in fig. 1, an embodiment of the present invention provides a method for preparing a thin film material with controllable crystal plane orientation, where the method includes:
and S1, collecting the femtosecond laser on the substrate, and processing a three-dimensional structure array on the surface of the substrate through the femtosecond laser.
The femtosecond laser technology has unique advantages in the aspects of cutting and punching, and compared with the traditional three-dimensional structure processing modes such as electron beam etching and wet etching, the femtosecond laser technology can be used for cold processing a very flat section and processing a three-dimensional structure with any shape in a controllable manner. In order to prepare a film material with controllable crystal plane orientation without the constraint of materials and a substrate, the shape and the size of a plurality of three-dimensional structures in a three-dimensional structure array are determined according to selected water-soluble crystal particles, femtosecond laser is focused on the substrate, the three-dimensional structure array is processed on the surface of the substrate through the femtosecond laser.
In a specific embodiment, the substrate is any substrate material that can be processed by laser, and in this embodiment, different substrates may be selected according to scientific requirements or according to application scenarios of the thin film material. In a specific embodiment, the substrate is one of glass, sapphire, quartz, and a silicon wafer.
Considering that the processing condition of the femtosecond laser on the substrate can affect the quality of the processed three-dimensional structure array and further affect the prepared film material with controllable crystal plane orientation, in this embodiment, when the femtosecond laser is gathered on the substrate, the wavelength of the femtosecond laser is set to 535nm, the power of the femtosecond laser is set to 3000-5000 mW, the scanning speed of the femtosecond laser on the substrate is 400mm/s, and the scanning frequency of the femtosecond laser on the substrate is 3-6 times. For example, a femtosecond laser with a wavelength and power of 535nm and 5000mW, respectively, scans the substrate 5 times at a scanning speed of 400 mm/s.
In a specific embodiment, the step of focusing the femtosecond laser on the substrate in the step S100 includes:
s01, polishing the substrate;
and S02, washing and drying the polished substrate.
Specifically, in this embodiment, before the femtosecond laser is used to process the substrate, the polishing pretreatment is performed on the surface of the substrate to obtain a substrate with a polished surface, and then the substrate with the polished surface is washed and dried to remove the residual contaminants on the surface of the substrate, so as to obtain a smooth and bright substrate.
In a specific embodiment, the method for preparing the thin film material with controllable crystal plane orientation further comprises:
and S2, collecting the femtosecond laser on the three-dimensional structure array, and processing the three-dimensional super-wetting template array on the surface of the substrate through the femtosecond laser.
Considering that the surface of the three-dimensional structure array processed by the femtosecond laser is rough, in this embodiment, after the three-dimensional structure array is processed on the surface of the substrate, the femtosecond laser is focused on the three-dimensional structure array, the three-dimensional structure array is further processed by the femtosecond laser, and the three-dimensional super-wetting template array is processed on the surface of the substrate, wherein the power of the femtosecond laser collected on the three-dimensional structure array is smaller than that of the femtosecond laser collected on the substrate, the shape and the size of each three-dimensional super-wetting template in the three-dimensional super-wetting template array are substantially the same as those of each three-dimensional structure in the three-dimensional structure array, and only each three-dimensional super-wetting template is smoother relative to each three-dimensional structure surface. In a specific embodiment, when the femtosecond laser is focused on the three-dimensional structure array, the scanning speed of the femtosecond laser is 400mm/s, the wavelength of the femtosecond laser is 535nm, the power of the femtosecond laser is 1500-3000 mW, and the scanning times of the femtosecond laser are 1-2 times. For example, a femtosecond laser with wavelength and power of 535nm and 3000mW, respectively, scans the three-dimensional structure array 2 times at a scanning speed of 400 mm/s.
In a specific embodiment, the method for preparing the thin film material with controllable crystal plane orientation further comprises:
s3, dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, and heating the substrate to obtain a thin film material with controllable crystal face orientation; wherein the three-dimensional structure array comprises a plurality of three-dimensional structures having sizes and shapes determined by sizes and shapes of the water-soluble crystal particles.
In this embodiment, after a three-dimensional super-wetting template array is processed on the surface of the substrate, water-soluble crystal particles are dripped onto the three-dimensional super-wetting template array, the water-soluble crystal particles are adsorbed by using super-wettability of the three-dimensional super-wetting template array, then the substrate is subjected to heating treatment, and in the heating treatment process, excess water in the water-soluble crystal particles adsorbed on the surface of the three-dimensional super-wetting template array is evaporated, so that the thin film material with controllable crystal face orientation is prepared. According to the invention, the water-soluble crystal particles are adsorbed by the super-wettability of the three-dimensional super-wetting template array, the diffusion of the water-soluble crystal particles is limited by utilizing the surface energy difference between a processing area and an unprocessed area on the surface of the substrate, and the film material with controllable crystal face orientation, which has consistent crystal grain orientation and uniform size, is obtained according to the orientation and size limited by the three-dimensional super-wetting template array.
In a specific embodiment, the water-soluble crystal particles are crystal materials with uniform particle size, and different types of film materials with controllable crystal plane orientation can be obtained by adopting different water-soluble crystal particles. In a specific embodiment, the water-soluble crystal particles are one or more of a micro-nano-scale metal organic framework material, a magnetic material, an oxide and a sulfide.
Considering that the temperature and the time of the heating treatment in the heating treatment process affect the quality of the prepared controllable crystal plane orientation thin film material, in a specific embodiment, the temperature of the heating treatment is 30-80 ℃, and the time of the heating treatment is 5-10 min, so that the high-quality controllable crystal plane orientation thin film material can be prepared under the heating condition. For example, heating at 70 ℃ for 5min, or heating at 40 ℃ for 10 min.
In a specific embodiment, the inclination angles of the three-dimensional structures in the three-dimensional structure array can be designed as required, and by designing the three-dimensional structures with different inclination angles, the thin film material with nanoparticles having different inclination angles can be prepared. In one embodiment, the inclination angles of the three-dimensional structures in the three-dimensional structure array are 0-30 °.
In a specific embodiment, the shape of the plurality of three-dimensional structures in the array of three-dimensional structures is determined by the shape of the water-soluble crystal particles, since the shape of each three-dimensional super-wetting template in the array of three-dimensional super-wetting templates is substantially the same as the shape of each three-dimensional structure in the array of three-dimensional structures, i.e. the shape of each three-dimensional super-wetting template is also determined by the shape of the water-soluble crystal particles. For example, when the shape of the water-soluble crystal particle is a cube, the shape of the plurality of three-dimensional structures is a cube; when the water-soluble crystal particles are in the shape of a sheet having a thickness, the plurality of three-dimensional structures are in the shape of cuboids; when the water-soluble crystal particles are spherical in shape, the shape of the plurality of three-dimensional structures is hemispherical. In a specific embodiment, the three-dimensional structure has a shape of one or more of a hemisphere, a tetrahedron, an octahedron, and a hexadecahedron.
In a specific embodiment, the size of the plurality of three-dimensional structures in the three-dimensional structure array is determined by the size of the water-soluble crystal particles, and since the size of each three-dimensional super-wetting template in the three-dimensional super-wetting template array is substantially the same as the size of each three-dimensional structure in the three-dimensional structure array, that is, the size of each three-dimensional super-wetting template is also determined by the size of the water-soluble crystal particles. In a specific embodiment, the height of the three-dimensional structures is 0.03-0.06 mm, and the length and width of the three-dimensional structures are greater than or equal to 0.2mm and less than or equal to the length and width of the water-soluble crystal particles.
In a specific embodiment, the invention also provides a film material with controllable crystal plane orientation, which is prepared by the preparation method of the film material with controllable crystal plane orientation. As shown in fig. 2, the thin film material 2 with controllable crystal plane orientation is deposited on the substrate 1, and the substrate 1 is one of glass, sapphire, quartz and silicon wafer. The preparation method of the film material 2 with controllable crystal face orientation is simple, the growth speed is high, the film material is not restricted by materials and substrates, the crystal grain orientation is consistent, and the size is uniform.
The invention is further illustrated by the following specific examples.
Example 1
(1) Focusing femtosecond laser with wavelength and power of 535nm and 5000mW on a silicon wafer, scanning the silicon wafer for 5 times at a scanning speed of 400mm/s to strip a layer of silicon wafer surface, and processing a three-dimensional structure array on the silicon wafer surface; the inclination angles of a plurality of three-dimensional structures in the three-dimensional structure array are 3 degrees, the shapes of the three-dimensional structures are cuboids, the lengths of the three-dimensional structures are 5mm, the widths of the three-dimensional structures are 0.4mm, and the depths of the three-dimensional structures are 0.06 mm;
(2) focusing femtosecond laser with wavelength and power of 535nm and 3000mW on the three-dimensional structure array, scanning the three-dimensional structure array for 2 times at a scanning speed of 400mm/s, and processing a three-dimensional super-wetting template array on the surface of the substrate;
(3) and dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, placing the substrate on a heating table, and heating the substrate at 60 ℃ for 10min to obtain the thin film material with controllable crystal face orientation.
Example 2
(1) Focusing femtosecond laser with wavelength and power of 535nm and 5000mW on a silicon wafer, scanning the silicon wafer for 5 times at a scanning speed of 400mm/s to strip a layer of silicon wafer surface, and processing a three-dimensional structure array on the silicon wafer surface; the three-dimensional structure array comprises a plurality of first three-dimensional structures and a plurality of second three-dimensional structures which are alternately arranged in rows, wherein the first three-dimensional structures are cuboid in shape, the first three-dimensional structures are 5mm in length, 0.4mm in width and 0.06mm in depth, the second three-dimensional structures are hemispherical in shape, and the radiuses of the second three-dimensional structures are 1 mm;
(2) focusing femtosecond laser with wavelength and power of 535nm and 3000mW on the three-dimensional structure array, scanning the three-dimensional structure array for 2 times at a scanning speed of 400mm/s, and processing a three-dimensional super-wetting template array on the surface of the substrate;
(3) and dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, placing the substrate on a heating table, and heating the substrate at 60 ℃ for 10min to obtain the thin film material with controllable crystal face orientation.
In summary, the invention discloses a thin film material with controllable crystal plane orientation and a preparation method thereof, comprising the following steps: collecting femtosecond laser on a substrate, and processing a three-dimensional structure array on the surface of the substrate through the femtosecond laser; collecting femtosecond laser on the three-dimensional structure array, and processing a three-dimensional super-wetting template array on the surface of the substrate through the femtosecond laser; dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, and heating the substrate to obtain a thin film material with controllable crystal face orientation; wherein the three-dimensional structure array comprises a plurality of three-dimensional structures having sizes and shapes determined by sizes and shapes of the water-soluble crystal particles. According to the invention, the water-soluble crystal particles are adsorbed by the super-wettability of the three-dimensional super-wetting template array, and the diffusion of the water-soluble crystal particles is limited by utilizing the surface energy difference between a processing area and an unprocessed area on the surface of the substrate, so that the film material with the controllable crystal face orientation, which has consistent crystal grain orientation and uniform size, is obtained, the film growth speed is high, the preparation method is simple, and the preparation process is not restricted by the material and the substrate.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a thin film material with controllable crystal face orientation is characterized by comprising the following steps:
collecting femtosecond laser on a substrate, and processing a three-dimensional structure array on the surface of the substrate through the femtosecond laser;
collecting femtosecond laser on the three-dimensional structure array, and processing a three-dimensional super-wetting template array on the surface of the substrate through the femtosecond laser;
dropwise adding water-soluble crystal particles onto the three-dimensional super-wetting template array, and heating the substrate to obtain a thin film material with controllable crystal face orientation; wherein the three-dimensional structure array comprises a plurality of three-dimensional structures having sizes and shapes determined by sizes and shapes of the water-soluble crystal particles.
2. The method for preparing a thin film material with controllable crystal plane orientation according to claim 1, wherein the substrate is one of glass, sapphire, quartz and silicon wafer.
3. The method for preparing the thin film material with controllable crystal plane orientation according to claim 1, wherein the femtosecond laser focused on the substrate satisfies the following conditions: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 3000-5000 mW, and the scanning times are 3-6.
4. The method for preparing a thin film material with controllable crystal plane orientation according to claim 1, wherein the step of focusing the femtosecond laser on the substrate is preceded by:
polishing the substrate;
and washing and drying the polished substrate.
5. The method for preparing the thin film material with controllable crystal plane orientation according to claim 1, wherein the femtosecond laser focused on the three-dimensional structure array satisfies the following conditions: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 1500-3000 mW, and the scanning times are 1-2.
6. The method for preparing a thin film material with controllable crystal plane orientation according to claim 1, wherein the water-soluble crystal particles are one or more of metal organic framework materials, magnetic materials, oxides and sulfides.
7. The preparation method of the film material with the controllable crystal plane orientation, according to claim 1, is characterized in that the heating treatment temperature is 30-80 ℃, and the heating treatment time is 5-10 min.
8. The method of claim 1, wherein the plurality of three-dimensional structures have one or more of hemispherical, tetrahedral, octahedral, and hexadecahedral shapes.
9. The method for preparing a thin film material with controllable crystal plane orientation according to claim 8, wherein the height of the plurality of three-dimensional structures is 0.03-0.06 mm, and the length and width of the plurality of three-dimensional structures are greater than or equal to 0.2mm and less than or equal to the length and width of the water-soluble crystal particles.
10. A thin film material with controllable crystal plane orientation is characterized by being prepared by the preparation method of the thin film material with controllable crystal plane orientation according to any one of claims 1 to 9.
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