CN111545922B - Processing method of silicon carbide crystal - Google Patents
Processing method of silicon carbide crystal Download PDFInfo
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- CN111545922B CN111545922B CN202010270072.3A CN202010270072A CN111545922B CN 111545922 B CN111545922 B CN 111545922B CN 202010270072 A CN202010270072 A CN 202010270072A CN 111545922 B CN111545922 B CN 111545922B
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a processing method of silicon carbide crystals, which comprises the following steps: (1) carrying out laser etching on the silicon carbide crystal ingot to form a crystal boundary with a required size; (2) after a film is adhered to the surface of the crystal, laser irradiation is carried out; (3) peeling the crystal adhered with the thin film from the silicon carbide crystal ingot; (4) separating the crystal from the film. The invention adopts laser etching and laser irradiation for two times of laser processing, so that more stress is generated in unit area, the crystal can be bent and folded more during stripping, the yield is not influenced, and the thin crystal can be obtained. The invention can realize the processing of the superhard silicon carbide crystal, has simple processing technology and high yield, and can be cut into silicon carbide micro crystals with any size and shape; and simultaneously realizes the thinning treatment of the crystal.
Description
Technical Field
The invention belongs to the technical field of crystal processing, and relates to a processing method of a silicon carbide crystal, in particular to a method for obtaining a crystal with a required size by stripping from a silicon carbide crystal ingot.
Background
The silicon carbide micro crystal is a third-generation wide-bandgap semiconductor material, has excellent properties of high thermal conductivity, high breakdown voltage, extremely high carrier mobility, high chemical stability and the like, can be manufactured into high-frequency and high-power electronic devices and optoelectronic devices which work under the conditions of high temperature and strong radiation, has great application value in the fields of national defense, high technology, industrial production, power supply and power transformation, and is regarded as a third-generation wide-bandgap semiconductor material with great development prospect.
The silicon carbide micro crystal is applied to devices and needs to be processed into crystals with a certain size, and the size of the crystals needed in some fields is micron level or nanometer level. Existing silicon carbide crystal processing techniques involve slicing an ingot into microcrystals of a desired size, such as CN 102514110B. Because the hardness of the silicon carbide crystal is high and is second to diamond, the silicon carbide crystal brings great difficulty to crystal processing, and particularly, the cutting speed is slow and the time is long.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a method for processing a silicon carbide microcrystal, which includes the steps of laser etching, film coating, and laser irradiation, and is capable of cutting a silicon carbide ingot into crystals of any size.
The technical scheme adopted by the invention is as follows:
according to one aspect of the present application, there is provided a method of processing a silicon carbide crystal, the method comprising the steps of:
(1) carrying out laser etching on the silicon carbide crystal ingot to form a boundary of crystals with required size;
(2) after a film is adhered to the surface of the crystal, laser irradiation is carried out;
(3) and peeling the crystal adhered with the thin film from the silicon carbide crystal ingot.
(4) Separating the crystal from the film.
The invention realizes that crystals with required size, especially micro crystals are stripped from the silicon carbide crystal ingot by the steps of laser etching, film coating and laser irradiation of the silicon carbide crystal ingot. Firstly, performing laser etching on the surface of a silicon carbide crystal ingot, and cutting a boundary pattern of a micro crystal with a certain depth and a required size according to the requirement; adhering a film on the surface of the crystal, and then carrying out laser irradiation; laser irradiation not only realizes deep grooving of primary laser and crystal formation defects of an ingot internal structure of secondary laser, but also realizes the denaturation of a thin film so as to be tightly bonded with the crystal, and the crystal and the denatured thin film are conveniently stripped from the ingot together; the peeling of the crystals is achieved by the adhesion of the thin film, and then by separating the micro-crystals from the thin film, crystals of the desired size are obtained. The method has simple processing technology and high yield, and can cut the silicon carbide crystal into silicon carbide crystals with any size.
Further, in the step (1), the depth of the laser etching is 0.1-1000 μm, and the width of the laser etching is 1-1000 μm; preferably, the depth of the laser etching is 20-200 μm, and the width of the laser etching is 30-50 μm. The depth of the laser etch is selected according to the thickness of the crystal of the desired size. The width of the laser etching is determined by the spot diameter of the laser, and is generally 1-3 spot diameters. The purpose of the laser etching is to obtain a pattern of crystals of a desired size, more precisely, the laser etching forms the boundaries of the crystals of the desired size, for example, in the embodiment of the present invention, the desired crystals are squares, the pattern of the desired crystals is obtained by laser etching, the width and depth of the etching form etched trenches, and the trenches surround the perimeter of the desired crystals. Because the inside of the depth of the laser etching generates great internal stress, the unit area generates greater stress, so that the crystal can be bent and folded more during peeling, and the yield is not influenced.
Further, the size of the crystal is micron-scale and/or nanometer-scale, and preferably, the number of the micro-crystal is at least two or more. In a preferred embodiment of the present invention, a plurality of crystals of a desired size are etched on the entire surface of the silicon carbide ingot, and when the plurality of crystals of a desired size are peeled off from the silicon carbide ingot, a thinning process of the silicon carbide ingot is also performed.
Further, in the step (1), the laser is at least one selected from a nanosecond laser and a femtosecond laser; preferably, the laser is a femtosecond laser. Preferably, the power of the laser is 10-1000W, and the laser etching time is 1-60 s. The x-y surface of the needed crystal is formed by the laser etching, and the irradiation intensity and time of the laser etching do not make special requirements as long as the depth required by the etching is met.
Further, in the step (2), the film is at least one selected from polydimethylsiloxane-containing films, polyethylene, polyisobutylene and butyl rubber films. The film has high thermal expansion coefficient, has good bonding effect on silicon carbide crystals, does not influence the crystal lattice structure of the crystals,
preferably, the film is adhered by one selected from the group consisting of coating and film bonding. Preferably, the thickness of the film is 0.1 to 200 μm. The coating liquid can be used for coating once and the polymer coating liquid can be used for coating for multiple times, the etched groove can be filled with the coating liquid or the polymer film, the film in the groove plays a certain buffering protection role after being denatured, and large internal stress can be generated after cooling, so that more uniform stress is generated when the crystal is adhered to the film for stripping.
Further, in the step (2), the laser is at least one selected from a nanosecond laser and a femtosecond laser; more preferably, the laser is a femtosecond laser. In the step (1), laser etching is performed to obtain an x-y surface of a required crystal, and the laser irradiation in the step (2) causes a defect to be formed at a certain position of the crystal; and by adopting two times of laser processing, more stress is generated in unit area, and the crystal can be bent and folded when being stripped, so that the yield is not influenced.
Preferably, the depth of the laser irradiation is the same as the depth of the laser etching. By regulating and controlling the power density and time of laser etching, the depth of laser irradiation is controlled to be the same as that of laser etching, so that the lower surface of the crystal obtained by stripping is almost flat, and the micro crystal with uniform thickness is obtained. The laser beam in the laser irradiation penetrates into the silicon carbide ingot to a desired depth, i.e., the depth of laser etching, so that a specific layer in the silicon carbide ingot is defective, thereby facilitating peeling. Preferably, the damage in the exfoliation layer of the silicon carbide ingot is caused to propagate less than 2 rayleigh lengths.
Further, in the step (3), after cooling, the crystal adhered with the film is stripped from the silicon carbide crystal ingot; preferably, the cooling is selected from at least one of liquid nitrogen cooling and cooling using a cryogenic box; more preferably, liquid nitrogen cooling is used. The effect of the cooling is to exacerbate the stress that causes the formation of crystal defects.
Furthermore, in the step (4), the film on the surface of the micro crystal is removed by adopting a chemical solvent corrosion method, the micro crystal is separated from the film, and oxygen can be introduced for combustion at the temperature of less than 1500 ℃ before the chemical corrosion. The chemical corrosion can clean the polymer on the crystal surface, and can also remove most of the polymer on the crystal surface by high-temperature oxygen combustion and then remove the polymer more cleanly by chemical corrosion. Or separating the micro crystal from the film by a crystal grain selector, and rapidly removing the crystal bonded on the surface of the film by the crystal grain selector.
According to another aspect of the invention, the application of the processing method of the silicon carbide crystal in manufacturing the silicon carbide microcrystal is provided. The processing method of the invention can obtain silicon carbide micro-crystals with required size and shape.
Further, the shape of the silicon carbide nanocrystal is selected from at least one of a polygon, a circle, an ellipse, and a profile. The polygon is selected from one of a triangle, a square, a regular pentagon, and the like. The profile may include various irregular shapes consisting of curves and lines. More preferably, the silicon carbide nanocrystals have a square shape.
Further, the thickness of the silicon carbide micro crystal is 0.1-1000 μm; preferably, the thickness of the silicon carbide micro-crystal is 20 to 200 μm. The thickness of the silicon carbide micro crystal obtained by the method has a wider range, because the laser etching and the laser irradiation are adopted for twice laser processing, more stress is generated in the unit area of the crystal, so that the required crystal can be bent and folded more when being stripped, and the silicon carbide micro crystal with different thicknesses can be obtained, thereby obtaining the very thin silicon carbide micro crystal.
The invention has the beneficial effects that:
(1) according to the invention, through the steps of laser etching, film coating and laser irradiation of the silicon carbide crystal ingot, the crystal with the required size is stripped from the silicon carbide crystal ingot. The invention adopts laser etching and laser irradiation for two times of laser processing, so that more stress is generated in unit area, the crystal can be bent and folded more during stripping, the yield is not influenced, and the thin silicon carbide micro crystal can be obtained. The invention can not only obtain the crystal with required size, but also realize the thinning treatment of the crystal.
(2) The invention can realize the processing of the superhard silicon carbide micro crystal, has simple processing technology and high yield, and can be cut into the silicon carbide micro crystal with any size. The method can obtain the micro-crystals with various shapes, has wide thickness range of the micro-crystals and can meet the requirements of various fields on the size of the micro-crystals.
Drawings
FIG. 1 is a laser etched pattern in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a laser irradiation configuration in an embodiment of the present invention;
FIG. 3 is a laser etched pattern in another embodiment of the present invention;
FIG. 4 is a laser etched pattern in accordance with yet another embodiment of the present invention;
in the figure, the position of the upper end of the main shaft,
1. a silicon carbide ingot; 2. a micro-crystal; 3. a film; 4. a laser device.
Detailed Description
The present invention is described in detail with reference to specific examples, which are provided to facilitate the understanding of the technical solutions of the present invention by those skilled in the art, and the implementation or use of the present invention is not limited by the description of the present invention.
In the present invention, reagents and equipment used are commercially available or commonly used in the art, if not specified.
The methods in the examples are conventional in the art unless otherwise specified.
The method of the present invention can be used in two applications, a "thinning process" which can separate very thin layers from the ingot, crystal or wafer surface, advantageously, the unwanted material can be very intact and the desired multiple crystals can be obtained. Another type is "crystal fabrication," and in particular, micro-crystal fabrication, in which multiple micro-crystals are cut simultaneously from the surface of a silicon carbide ingot.
Example 1
A processing method of silicon carbide specifically comprises the following steps:
(1) laser etching
Laser etching is carried out on the surface of a silicon carbide crystal ingot by using a laser device, preferably a femtosecond laser, the etched groove forms the boundary of a micro crystal with a required size, the laser power is 10-1000W, the laser etching time is 1-60 s by regulating and controlling the laser etching power and time, the laser etching depth is 0.2mm, the laser etching width is 0.1mm, and the etched pattern is shown in figure 1, namely, the surface of the silicon carbide crystal ingot 1 is cut into a plurality of square micro crystals 2 with the side length of 0.3 mm;
the surface of the silicon carbide crystal ingot can be etched by using a laser etching machine, for example, the method comprises the following specific operation steps: fixing a silicon carbide crystal ingot to be processed on a workbench of a laser etching machine, then adjusting a light path system of the laser etching machine, adjusting the position of a laser focus, and setting a cutting path of a polarizer on a computer of the laser etching machine to enable the surface of the silicon carbide crystal ingot on the workbench and a laser scanning line to generate relative motion; and rapidly cutting the surface of the silicon carbide crystal ingot by the polarizer at a preset deflection angle and a preset power density, and changing the cutting direction by using the workbench for a plurality of times until the satisfactory effect is achieved.
(2) After coating, laser irradiation is carried out
And spraying polydimethylsiloxane coating liquid on the surface of the silicon carbide crystal ingot 1, drying to form a polydimethylsiloxane film with the thickness of 50 mu m, and then carrying out laser irradiation on the surface of the silicon carbide crystal ingot 1, wherein the structural schematic diagram of the laser irradiation is shown in figure 2. The surface 1 of the silicon carbide ingot may be laser-irradiated using the laser device 4, so that defects are generated inside the micro-crystals 2. The depth of laser irradiation is regulated and controlled to be the same as the depth of laser etching by regulating the power density of the laser irradiation. The laser beam in the laser irradiation invades into the silicon carbide ingot to a required depth, so that the silicon carbide ingot generates defects on a layer at a specific depth, and the damage in the stripping layer of the silicon carbide ingot is expanded by less than 2 times of Rayleigh length.
The laser etching machine or the laser machine can be used for carrying out laser irradiation on the surface of the silicon carbide crystal ingot 1, namely the surfaces of the plurality of micro crystals 2, the laser irradiation realizes that the crystals in the silicon carbide crystal ingot 1 generate defects so as to be convenient for the micro crystals 2 to be stripped from the silicon carbide crystal ingot 1, and the laser irradiation realizes the denaturation of the film 3 so as to enable the connection between the film 3 and the crystals to be tighter, so that when the film 3 is stripped, the micro crystals 2 can be completely and firmly bonded on the film 3, and all the micro crystals 2 can be completely stripped from the silicon carbide crystal ingot 1 at one time.
(3) Cooling and stripping
And rapidly cooling the micro crystal adhered with the film by using liquid nitrogen, and then stripping the micro crystal from the silicon carbide crystal ingot 1, wherein the rapid cooling realizes the internal crystal stress deformation of the silicon carbide crystal ingot 1, and the stripping force of the film 3 realizes the stripping of the required crystal from the silicon carbide crystal ingot 1.
(4) Chemical etching
The micro-crystal to which the thin film is adhered is immersed in a strong acid such as hydrochloric acid, sulfuric acid, hydrofluoric acid or the like to remove the thin film on the crystal, and then subjected to a washing treatment with distilled water to obtain a plurality of micro-crystals having a length of 0.3mm, a width of 0.3mm, and a thickness of 0.2 mm.
Example 2
A processing method of silicon carbide specifically comprises the following steps:
(1) laser etching
Performing laser etching on the surface of a silicon carbide crystal ingot by using a femtosecond laser to form a boundary of a micro crystal with a required size, controlling the depth of the laser etching to be 0.1mm and the width of the laser etching to be 0.05mm, and cutting the surface of the silicon carbide crystal ingot 1 into a plurality of circular micro crystals 2 with the diameter of 0.2mm as shown in figure 3;
the surface of the silicon carbide crystal ingot 1 can be etched by using a laser etching machine, and the etched boundary, the etched depth and the etched width are controlled by regulating and controlling the power density, the polarized light angle, the time and the like of the laser etching machine.
(2) After coating, laser irradiation is carried out
Adhering a layer of polyethylene film with the thickness of 200 mu m on the surface of a silicon carbide crystal ingot, then carrying out laser irradiation by using a femtosecond laser, and controlling the depth of the laser irradiation to be the same as the depth of laser etching by adjusting the power density and time of the laser irradiation. The laser beam in the laser irradiation invades into the silicon carbide crystal ingot to a required depth, so that the silicon carbide crystal ingot generates defects on a layer where the silicon carbide crystal ingot is located at a specific depth, and the damage in the stripping layer of the silicon carbide crystal ingot is expanded by less than 2 times of Rayleigh length.
The laser irradiation realizes crystal generation defects inside the silicon carbide ingot 1 so that the micro-crystals 2 can be peeled off from the silicon carbide ingot 1, and the laser irradiation realizes the denaturation of the film so that the film is connected with the crystals more tightly, so that when the film is peeled off, the micro-crystals 2 can be completely and firmly bonded on the film, and all the micro-crystals 2 can be completely peeled off from the silicon carbide ingot 1 at one time.
(3) Cooling and stripping
The micro-crystal 2 to which the thin film is adhered is rapidly cooled using liquid nitrogen and then peeled off from the silicon carbide ingot 1. The rapid cooling realizes the internal crystal stress deformation of the silicon carbide crystal ingot 1, and the stripping of the micro crystal 2 is realized through the adhesion of a film.
(4) Separation of
The micro-crystals 2 were peeled off from the film by using a crystal grain picker to obtain a plurality of micro-crystals 2 having a diameter of 0.2mm and a thickness of 0.1 mm.
Example 3
A processing method of silicon carbide specifically comprises the following steps:
(1) laser etching
Performing laser etching on the surface of the silicon carbide crystal ingot 1 by using a femtosecond laser to form boundaries of a plurality of crystals with required sizes, controlling the depth of the laser etching to be 0.05mm and the width of the laser etching to be 0.05mm, and cutting the surface of the silicon carbide crystal ingot 1 into micro crystals 2 with different shapes and sizes as shown in figure 4 by using the etched pattern;
the surface of the silicon carbide crystal ingot 1 can be etched by using a laser etching machine, and the shape of the etched groove and the etching depth and width can be controlled by regulating the power density, the polarization angle and the like of the laser etching machine.
(2) After coating, laser irradiation is carried out
Coating butyl rubber coating liquid on the surface of the silicon carbide crystal ingot 1 for multiple times, drying to form a butyl rubber film with the thickness of 100 mu m, then carrying out laser irradiation by using a femtosecond laser, and regulating and controlling the depth of the laser irradiation to be the same as the depth of laser etching by regulating the power density of the laser irradiation. The laser beam in the laser irradiation invades into the silicon carbide ingot to a required depth, so that the silicon carbide ingot generates defects on a layer at a specific depth, and the damage in the stripping layer of the silicon carbide ingot is expanded by less than 2 times of Rayleigh length.
Laser irradiation of the surface of the plurality of micro-crystals 2 (i.e., the ingot surface) may be performed using a laser etcher or a laser machine, the laser irradiation causes defects in crystals inside the silicon carbide ingot 1 to facilitate peeling of the micro-crystals 2 from the silicon carbide ingot 1, and the laser irradiation causes denaturation of the thin film to enable the thin film to be more tightly attached to the crystals, so that when the thin film is peeled, the desired crystals can be completely and firmly bonded to the thin film, so that all the crystals can be completely peeled from the silicon carbide ingot at one time.
(3) Cooling and stripping
The micro-crystal 2 to which the thin film is adhered is rapidly cooled using liquid nitrogen and then peeled off from the silicon carbide ingot 1. The rapid cooling realizes the stress deformation of the crystal inside the silicon carbide crystal ingot 1, and the peeling of the micro crystal 2 is realized through the adhesion of the polymer.
(4) Chemical etching
The micro-crystal 2 to which the thin film is adhered is immersed in a strong acid such as hydrochloric acid, sulfuric acid, hydrofluoric acid, or the like to remove the thin film on the crystal, and then subjected to a washing treatment with distilled water to obtain a plurality of micro-crystals 2 having different shapes.
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (15)
1. A method of processing a silicon carbide crystal, the method comprising the steps of:
(1) carrying out laser etching on the silicon carbide crystal ingot to form a crystal boundary with a required size;
(2) after a film is adhered to the surface of the crystal, laser irradiation is carried out;
(3) peeling the crystal adhered with the thin film from the silicon carbide crystal ingot;
(4) separating the crystal from the thin film;
the film in the step (2) adopts a polymer with high thermal expansion coefficient, the polymer is selected from at least one of polydimethylsiloxane, polyethylene, polyisobutylene and butyl rubber film, the adhesion of the film is selected from one of coating and film bonding, and the thickness of the film is 0.1-200 mu m;
and an etched groove is formed between the adjacent crystals, and coating liquid or a polymer film can be filled in the etched groove.
2. The method for processing the silicon carbide crystal according to claim 1, wherein in the step (1), the depth of the laser etching is 0.1-1000 μm, and the width of the laser etching is 1-1000 μm.
3. The method for processing the silicon carbide crystal according to claim 2, wherein the depth of the laser etching is 20 to 200 μm, and the width of the laser etching is 30 to 50 μm.
4. The method for processing a silicon carbide crystal according to claim 1, wherein in step (1), the laser is at least one selected from the group consisting of a nanosecond laser and a femtosecond laser.
5. The method of processing a silicon carbide crystal according to claim 4, wherein the silicon carbide crystal is grown in the growth reactor,
the laser is femtosecond laser;
the power of the laser is 10-1000W, and the laser etching time is 1-60 s.
6. The method for processing a silicon carbide crystal according to claim 1, wherein in step (2), the laser is at least one selected from the group consisting of a nanosecond laser and a femtosecond laser.
7. The method of processing a silicon carbide crystal according to claim 6,
the laser is femtosecond laser;
the depth of the laser irradiation is the same as the depth of the laser etching.
8. The method of processing a silicon carbide crystal according to claim 1 wherein in step (3), after cooling, the crystal with the film adhered thereto is peeled from the silicon carbide ingot.
9. The method of processing a silicon carbide crystal according to claim 8, wherein the silicon carbide crystal is a silicon carbide crystal,
the cooling is selected from at least one of liquid nitrogen cooling and cooling using a cryogenic tank.
10. The method for processing a silicon carbide crystal according to claim 1, wherein in step (4), the thin film on the surface of the crystal is removed by chemical solvent etching to separate the crystal from the thin film;
and/or separating the crystals from the film using a grain picker.
11. Use of the method for processing a silicon carbide crystal according to any one of claims 1 to 10 for producing a silicon carbide nanocrystal.
12. The use according to claim 11, wherein the silicon carbide nanocrystals have a shape selected from at least one of a polygon, a circle, an ellipse, and a profile.
13. Use according to claim 12, wherein the silicon carbide nanocrystals are square in shape.
14. The use according to claim 11, wherein the silicon carbide nanocrystals have a thickness of 0.1 to 1000 μm.
15. The use according to claim 14,
the thickness of the silicon carbide micro crystal is 20-200 mu m.
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| CN113897683B (en) * | 2021-12-08 | 2022-03-29 | 浙江大学杭州国际科创中心 | Stripping method and stripping device for n-type silicon carbide single crystal wafer |
| CN114150382B (en) * | 2021-12-08 | 2022-11-22 | 浙江大学杭州国际科创中心 | Method and device for stripping n-type silicon carbide single crystal wafer based on photoetching |
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