CN113753847B - Thin film material with controllable crystal face orientation and preparation method thereof - Google Patents

Abstract

The invention discloses a thin film material with controllable crystal plane orientation and a preparation method thereof. on the surface of the substrate, a three-dimensional super-wetting template array is processed; water-soluble crystal particles are dropped onto the three-dimensional super-wetting template array, and the substrate is heated to obtain a film material with controllable crystal plane orientation; , the three-dimensional structure array includes several three-dimensional structures, and the size and shape of the several three-dimensional structures are determined by the size and shape of the water-soluble crystal particles. The invention absorbs the water-soluble crystal particles through the super-wetting of the three-dimensional super-wetting template array, and uses the surface energy difference between the processed area and the unprocessed area to limit the diffusion of the water-soluble crystal particles, so as to obtain consistent crystal grain orientation and size. The uniform thin film material, the thin film growth rate is fast, the preparation method is simple, and the preparation process is not restricted by the material and the substrate.

Description

A kind of film material with controllable crystal plane orientation and preparation method thereof

technical field

The invention relates to the technical field of micro-nano processing, in particular to a film material with controllable crystal plane orientation and a preparation method thereof.

Background technique

The crystal plane orientation, composition, grain size and interface stress of the film will greatly affect the performance of the film. Films with different preferred orientations can show different properties, and can be applied to microelectronics technology, optoelectronics technology, MEMS technology, etc. according to different requirements. . How to prepare thin films with good performance to meet the requirements of integrated devices has become a key link restricting the application of thin films.

At present, molecular beam epitaxy is mainly used to prepare thin films, but this method has a slow growth rate of thin films and requires strict matching of materials and substrates.

Therefore, the existing technology still needs to be improved and developed.

SUMMARY OF THE INVENTION

The technical problem to be solved by the present invention is to provide a film material with controllable crystal plane orientation and a preparation method thereof in view of the above-mentioned defects of the prior art. The problem of strict matching at the bottom.

The technical solution adopted by the present invention to solve the technical problem is: a preparation method of a film material with controllable crystal plane orientation, wherein, comprising:

collecting the femtosecond laser on the substrate, and processing the three-dimensional structure array on the surface of the substrate by the femtosecond laser;

Focusing the femtosecond laser on the three-dimensional structure array, and processing the three-dimensional super-wetting template array on the surface of the substrate by the femtosecond laser;

The water-soluble crystal particles are dropped onto the three-dimensional super-wetting template array, and the substrate is heated to obtain a film material with controllable crystal plane orientation; wherein, the three-dimensional structure array includes several three-dimensional structures, The size and shape of the several three-dimensional structures are determined by the size and shape of the water-soluble crystalline particles.

In the method for preparing the thin film material with controllable crystal plane orientation, the substrate is one of glass, sapphire, quartz and silicon wafer.

The method for preparing a thin film material with controllable crystal plane orientation, wherein the femtosecond laser gathered on the substrate satisfies: the scanning speed is 400 mm/s, the wavelength is 535 nm, the power is 3000-5000 mW, and the number of scans is 3-3 6 times.

The method for preparing the thin film material with controllable crystal plane orientation, wherein, before the step of focusing the femtosecond laser on the substrate, it includes:

polishing the substrate;

The polished substrate is washed and dried.

The preparation method of the film material with controllable crystal plane orientation, wherein the femtosecond laser gathered on the three-dimensional structure array satisfies: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 1500-3000mW, and the number of scans is 1 ~ 2 times.

In the method for preparing the thin film material with controllable crystal plane orientation, the water-soluble crystal particles are one or more of metal organic framework materials, magnetic materials, oxides and sulfides.

In the method for preparing the thin film material with controllable crystal plane orientation, the temperature of the heat treatment is 30°C to 80°C, and the time of the heat treatment is 5 to 10 minutes.

In the method for preparing the thin film material with controllable crystal plane orientation, the shapes of the several three-dimensional structures are one or more of hemisphere, tetrahedron, octahedron and hexahedron.

The method for preparing the film material with controllable crystal plane orientation, wherein the heights of the several three-dimensional structures are 0.03-0.06 mm, and the lengths and widths of the several three-dimensional structures are greater than or equal to 0.2 mm and less than or equal to the The length and width of the water-soluble crystal particles.

A film material with controllable crystal plane orientation, wherein, it is prepared by the method for preparing a film material with controllable crystal plane orientation.

Beneficial effects: the present invention adsorbs the water-soluble crystal particles through the super-wetting of the three-dimensional super-wetting template array, and uses the surface energy difference between the processed area and the unprocessed area of the substrate surface to limit the diffusion of the water-soluble crystal particles, and obtains The thin film material with uniform crystal grain orientation and uniform size and controllable crystal plane orientation has fast film growth speed, simple preparation method, and the preparation process is not restricted by materials and substrates.

Description of drawings

1 is a schematic flowchart of a method for preparing a thin film material with controllable crystal plane orientation provided by an embodiment of the present invention;

FIG. 2 is a schematic structural diagram of a thin film material with controllable crystal plane orientation provided by an embodiment of the present invention.

Detailed ways

The present invention provides a method for preparing a thin film material with controllable crystal plane orientation. In order to make the purpose, technical solutions and advantages of the present invention clearer and clearer, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention.

The crystal plane orientation, composition, grain size and interface stress of the film will greatly affect the performance of the film. Films with different preferred orientations can show different properties, and can be applied to microelectronics technology, optoelectronics technology, MEMS technology, etc. according to different requirements. . How to prepare thin films with good performance to meet the requirements of integrated devices has become a key link restricting the application of thin films. At present, molecular beam epitaxy is mainly used to prepare thin films, but this method has a slow growth rate of thin films and requires strict matching of materials and substrates.

In order to solve the above problems, 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, and the method includes:

S1. The femtosecond laser is focused on the substrate, and a three-dimensional structure array is processed on the surface of the substrate by the femtosecond laser.

Femtosecond laser technology has unique advantages in cutting and drilling. Compared with traditional three-dimensional structure processing methods such as electron beam etching and wet etching, it can cold process a very flat section, and can controllably process any arbitrary shape. The three-dimensional structure of the shape. In this example, in order to prepare a thin film material with controllable crystal plane orientation without being constrained by materials and substrates, the shapes and sizes of several three-dimensional structures in the three-dimensional structure array are first determined according to the selected water-soluble crystal particles, and then femtosecond The laser is focused on the substrate, and a three-dimensional structure array is processed on the surface of the substrate by a femtosecond laser. In this embodiment, a three-dimensional structure array is processed on the surface of the substrate by a femtosecond laser, and the three-dimensional structure array is super wettable. The micro-nano patterns greatly enhance the surface wettability of the substrate.

In a specific embodiment, the substrate is any substrate material that can be processed by laser. In this embodiment, different substrates can be selected according to scientific research requirements or application scenarios of thin film materials. In a specific embodiment, the substrate is one of glass, sapphire, quartz and silicon wafer.

Considering that the processing conditions of the femtosecond laser on the substrate will affect the quality of the processed three-dimensional structure array, and then affect the prepared thin film material with controllable crystal plane orientation, the femtosecond laser is focused on the substrate in this embodiment. When the wavelength of the femtosecond laser is 535 nm, the power of the femtosecond laser is 3000-5000 mW, the scanning speed of the femtosecond laser on the substrate is 400 mm/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 535 nm and 5000 mW, respectively, scans the substrate 5 times at a scan speed of 400 mm/s.

In a specific embodiment, before the step of focusing the femtosecond laser light on the substrate in step S100, it includes:

S01, polishing the substrate;

S02, washing and drying the polished substrate.

Specifically, in this embodiment, before processing the substrate by using the femtosecond laser, the surface of the substrate is polished and pretreated to obtain a substrate with a polished surface, and then the substrate with a polished surface is washed and dried , remove the contaminants remaining on the surface of the substrate, and obtain a substrate with a smooth and bright surface.

In a specific embodiment, the preparation method of the film material with controllable crystal plane orientation further comprises:

S2. Focus the femtosecond laser on the three-dimensional structure array, and process the three-dimensional super-wetting template array on the surface of the substrate by using the femtosecond laser.

Considering that the surface of the three-dimensional structure array processed by the femtosecond laser is relatively 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, and the The three-dimensional structure array is further processed, and a three-dimensional super-wetting template array is processed on the surface of the substrate, wherein the power of the femtosecond laser focused on the three-dimensional structure array is smaller than the power of the femtosecond laser focused on the substrate The shape and size of each three-dimensional super-wetting template in the three-dimensional super-wetting template array are basically the same as the shape and size of each three-dimensional structure in the three-dimensional structure array, except that each three-dimensional super-wetting template is more than the surface of each three-dimensional structure. smooth. In a specific embodiment, when the femtosecond laser is collected on the three-dimensional structure array, the scanning speed of the femtosecond laser is 400 mm/s, the wavelength of the femtosecond laser is 535 nm, and the power of the femtosecond laser is 1500-3000 mW, The number of scans of the femtosecond laser is 1 to 2 times. For example, a femtosecond laser with a wavelength and power of 535 nm and 3000 mW, respectively, scans the three-dimensional structure array twice at a scan speed of 400 mm/s.

In a specific embodiment, the preparation method of the film material with controllable crystal plane orientation further comprises:

S3, dropping water-soluble crystal particles onto the three-dimensional super-wetting template array, and heating the substrate to obtain a film material with controllable crystal plane orientation; wherein, the three-dimensional structure array includes several three-dimensional structures structure, the size and shape of the several three-dimensional structures are determined by the size and shape of the water-soluble crystalline 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 dropped onto the three-dimensional super-wetting template array, and the super-wetting properties of the three-dimensional super-wetting template array are utilized. The water-soluble crystal particles are adsorbed, and then the substrate is heated. During the heating process, the excess water in the water-soluble crystal particles adsorbed on the surface of the three-dimensional super-wetting template array is evaporated, thereby preparing a controllable Crystalline oriented thin film material. The invention adsorbs the water-soluble crystal particles through the super-wetting of the three-dimensional super-wetting template array, and uses the surface energy difference between the processed area and the unprocessed area of the substrate surface to limit the diffusion of the water-soluble crystal particles. The orientation and size of the wet template array are limited to obtain a film material with controllable crystal plane orientation with uniform grain orientation and uniform size.

In a specific embodiment, the water-soluble crystal particles are crystal materials with uniform particle size. By using different water-soluble crystal particles, different types of film materials with controllable crystal plane orientation can be obtained. In a specific embodiment, the water-soluble crystal particles are one or more of micro-nano-scale metal organic framework materials, magnetic materials, oxides and sulfides.

Considering that the temperature during the heat treatment and the time of the heat treatment will affect the quality of the prepared film material with controllable crystal plane orientation, in a specific embodiment, the temperature of the heat treatment is 30°C to 80°C, The heating treatment time is 5-10 minutes, and under this heating condition, a high-quality film material with controllable crystal plane orientation can be prepared. For example, heat at 70°C for 5 min, or at 40°C for 10 min.

In a specific embodiment, the inclination angles of several three-dimensional structures in the three-dimensional structure array can be designed as required, and by designing several three-dimensional structures with different inclination angles, thin film materials with nanoparticles having different inclination angles can be prepared. In a specific embodiment, the inclination angle of several three-dimensional structures in the three-dimensional structure array is 0-30°.

In a specific embodiment, the shape of several three-dimensional structures in the three-dimensional structure array is determined by the shape of the water-soluble crystal particles, because the shape of each three-dimensional super-wetting template in the three-dimensional super-wetting template array is different from the shape of all three-dimensional super-wetting templates. The shape of each three-dimensional structure in the three-dimensional structure array is basically the same, that is, 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 particles is a cube, the shapes of several three-dimensional structures are cubes; when the shape of the water-soluble crystal particles is a sheet having a thickness, the shapes of several three-dimensional structures are rectangular parallelepipeds; When the shape of the water-soluble crystal particles is spherical, the shapes of several three-dimensional structures are hemispherical. In a specific embodiment, the shape of the three-dimensional structure is one or more of a hemisphere, a tetrahedron, an octahedron and a hexahedron.

In a specific embodiment, the size of several three-dimensional structures in the three-dimensional structure array is determined by the size of the water-soluble crystal particles, because the size of each three-dimensional super-wetting template in the three-dimensional super-wetting template array is the same as that of all three-dimensional super-wetting templates. The size of each three-dimensional structure in the three-dimensional structure array is basically the same, 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 heights of the three-dimensional structures are 0.03-0.06 mm, and the length and width of the three-dimensional structures are greater than or equal to 0.2 mm and less than or equal to the length and width of the water-soluble crystal particles.

In a specific embodiment, the present invention also provides a film material with controllable crystal plane orientation prepared by using the above-mentioned preparation method for a 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 plane orientation of the present invention is simple, the growth rate is fast, and the crystal grain orientation is consistent and the size is uniform without being restricted by the material and the substrate.

The present invention will be further explained below through specific embodiments.

Example 1

(1) Focus the femtosecond laser with wavelength and power of 535nm and 5000mW respectively on the silicon wafer, scan the silicon wafer 5 times at a scanning speed of 400mm/s, peel off the surface of the silicon wafer layer by layer, and process it on the surface of the silicon wafer A three-dimensional structure array is obtained; wherein, the inclination angle of several three-dimensional structures in the three-dimensional structure array is 3°, the shape of several three-dimensional structures is cuboid, the length of several three-dimensional structures is 5mm, the width is 0.4mm, and the depth is 0.06mm;

(2) Focus the femtosecond laser with wavelength and power of 535 nm and 3000 mW respectively on the three-dimensional structure array, scan the three-dimensional structure array twice at a scanning speed of 400 mm/s, and process a three-dimensional super-wetting template on the surface of the substrate array;

(3) drop water-soluble crystal particles onto the three-dimensional super-wetting template array, place the substrate on a heating stage, and heat the substrate at 60° C. for 10 min to obtain a film material with controllable crystal plane orientation .

Example 2

(1) Focus the femtosecond laser with wavelength and power of 535nm and 5000mW respectively on the silicon wafer, scan the silicon wafer 5 times at a scanning speed of 400mm/s, peel off the surface of the silicon wafer layer by layer, and process it on the surface of the silicon wafer A three-dimensional structure array is obtained; wherein, the three-dimensional structure array includes several first three-dimensional structures and several second three-dimensional structures arranged alternately in columns, the shape of several first three-dimensional structures is cuboid, the length of several first three-dimensional structures is 5 mm, and the width of several first three-dimensional structures is 5 mm. 0.4mm, the depth is 0.06mm, the shape of several second three-dimensional structures is hemispherical, and the radius of several second three-dimensional structures is 1mm;

(2) Focus the femtosecond laser with wavelength and power of 535 nm and 3000 mW respectively on the three-dimensional structure array, scan the three-dimensional structure array twice at a scanning speed of 400 mm/s, and process a three-dimensional super-wetting template on the surface of the substrate array;

(3) drop water-soluble crystal particles onto the three-dimensional super-wetting template array, place the substrate on a heating stage, and heat the substrate at 60° C. for 10 min to obtain a film material with controllable crystal plane orientation .

In summary, the present invention discloses a thin film material with controllable crystal plane orientation and a preparation method thereof, comprising: focusing a femtosecond laser on a substrate, and processing a three-dimensional structure on the surface of the substrate by the femtosecond laser array; femtosecond laser is focused on the three-dimensional structure array, and a three-dimensional super-wetting template array is processed on the surface of the substrate by the femtosecond laser; water-soluble crystal particles are dropped onto the three-dimensional super-wetting template array and heating the substrate to obtain a film material with controllable crystal plane orientation; wherein, the three-dimensional structure array includes several three-dimensional structures, and the size and shape of the several three-dimensional structures are determined by the water-soluble crystal particles size and shape are determined. The invention absorbs the water-soluble crystal particles through the super-wetting of the three-dimensional super-wetting template array, and uses the surface energy difference between the processed area and the unprocessed area of the substrate surface to limit the diffusion of the water-soluble crystal particles to obtain the crystal grain orientation. Consistent and uniform size and size of the film material with controllable crystal plane orientation, the film growth rate is fast, the preparation method is simple, and the preparation process is not restricted by the material and the substrate.

It should be understood that the application of the present invention is not limited to the above examples. For those of ordinary skill in the art, improvements or transformations can be made according to the above descriptions, and all these improvements and transformations should belong to the protection scope of the appended claims of the present invention.

Claims (7)

1. A preparation method of a thin film material with controllable crystal face orientation is characterized by comprising the following steps:

gathering 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 number of three-dimensional structures having sizes and shapes determined by the sizes and shapes of the water-soluble crystal particles; the femtosecond laser focused on the substrate satisfies: the scanning speed is 400mm/s, the wavelength is 535nm, the power is 3000-5000 mW, and the scanning times are 3-6; the femtosecond laser gathered 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.

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 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.

4. 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.

5. 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.

6. The method of claim 1, wherein the plurality of three-dimensional structures have one or more of hemispherical, tetrahedral, octahedral, and hexadecahedral shapes.

7. The method for preparing a thin film material with controllable crystal plane orientation according to claim 6, 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.

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