CN111962156A - Method for repairing single crystal diamond crystal structure based on ultrashort pulse laser - Google Patents
Method for repairing single crystal diamond crystal structure based on ultrashort pulse laser Download PDFInfo
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- CN111962156A CN111962156A CN202010783645.2A CN202010783645A CN111962156A CN 111962156 A CN111962156 A CN 111962156A CN 202010783645 A CN202010783645 A CN 202010783645A CN 111962156 A CN111962156 A CN 111962156A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/04—After-treatment of single crystals or homogeneous polycrystalline material with defined structure using electric or magnetic fields or particle radiation
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Abstract
The invention discloses a method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser. The method adopts detection technologies such as X-ray diffraction, laser Raman spectroscopy and the like, and can rapidly and nondestructively judge the crystallization quality of the whole diamond and local diamond. The radiation annealing treatment is carried out on the area with poor crystal quality in the diamond through ultrashort pulse high-energy laser beams such as picoseconds and femtoseconds, and therefore the crystal structure of the diamond is repaired flexibly and efficiently. The method can quickly and pertinently promote the repair of the surface layer crystal lattice damage of the diamond and improve the crystal quality of the diamond by combining the characteristics of short action time, small heat influence range and high energy density of the ultrashort pulse laser and adjusting the process parameters and controlling the annealing atmosphere and the temperature and pressure conditions, is particularly suitable for doping the diamond film, can effectively improve the uniformity and the crystal quality of the diamond film and optimizes the process performance of the film.
Description
Technical Field
The invention relates to the technical field of diamond materials, in particular to a method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser.
Background
The diamond has excellent physical and chemical properties, such as wide forbidden band, high thermal conductivity, high breakdown voltage, small dielectric constant, high radiation hardness and the like, is obviously superior to other third-generation semiconductor materials, and is a key material for manufacturing chips in the future. Based on the development of diamond growth and doping technology, the diamond is expected to be put into use in more technical fields with high added values, such as power electronics, quantum communication and the like, but the performance and the service life of a manufactured device can be seriously influenced by the problem of crystal structure degradation in the growth and doping processes, so that a good crystal structure is an important premise for further realizing industrial application.
At present, the research aiming at the repair of the crystal structure of the single crystal diamond mainly comprises the integral thermal annealing treatment, which mainly comprises high-temperature high-pressure annealing and high-temperature low-pressure annealing, but the methods are difficult to be effectively adjusted according to the individual difference of the diamond, and the method can not be used for carrying out targeted repair on local areas of the diamond and has no selectivity and high efficiency. Therefore, it is very important to find a method for flexibly and efficiently annealing the surface layer of the diamond and repairing the crystal structure of the diamond.
Disclosure of Invention
The invention aims to provide a method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser, which aims to solve the problems that the existing method has no selectivity and high efficiency, only can treat the whole diamond and cannot carry out targeted repair on local areas of the diamond. As shown in fig. 1, the crystal quality of the whole or a local region of the diamond can be determined quickly and nondestructively by using detection techniques such as X-ray diffraction and laser raman spectroscopy. The radiation annealing treatment is carried out on the area with poor crystal quality in the diamond through ultrashort pulse high-energy laser beams such as picoseconds and femtoseconds, and therefore the crystal structure of the diamond is repaired flexibly and efficiently. The method can quickly and pertinently promote the repair of the surface layer crystal lattice damage of the diamond and improve the crystal quality of the diamond by combining the characteristics of short action time, small heat influence range and high energy density of the ultrashort pulse laser and adjusting the process parameters and controlling the annealing atmosphere and the temperature and pressure conditions, is particularly suitable for doping the diamond film, can effectively improve the uniformity and the crystal quality of the diamond film and optimizes the process performance of the film.
The technical scheme adopted by the invention is as follows: a method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser comprises the following steps:
(1) screening of diamonds
a. Firstly adopting H for a single crystal diamond sample2SO4/KNO3Carrying out hot cleaning on the diamond by using the mixed solution or aqua regia, and then carrying out ultrasonic cleaning by using acetone, absolute ethyl alcohol and deionized water in sequence, wherein the cleaning time is 5min each time;
b. and judging the integral crystallization quality of the diamond by adopting X-ray diffraction, and screening the diamond of which the half height width of an X-ray rocking curve is more than or equal to 150 arcsec.
(2) Selection of diamond surface layer repair area
Scanning the selected diamond with laser Raman spectrometer to determine its thickness at 1332.5cm-1The distribution state of the first-order intrinsic Raman peak of nearby diamond is selected, and the intrinsic Raman peak of diamond is invisible or its half-height width is greater than or equal to 10cm-1And the location thereof is marked.
(3) Repair of diamond surface crystal structure
a. Placing the marked diamond on a cold and hot table of a vacuum cavity, and focusing the ultrashort pulse laser equipment on a diamond surface marking area;
b. and (3) performing radiation annealing on the selected area of the diamond surface by using ultrashort pulse laser, such as nanosecond, picosecond and femtosecond laser beams.
c. And after the radiation annealing treatment is finished, detecting the crystal quality of the whole surface layer and the local surface layer of the diamond by adopting X-ray diffraction and laser Raman spectroscopy.
Further, in the present invention, the repaired diamond can be produced naturally, or synthesized by high temperature and high pressure, vapor phase chemical deposition and other methods. The diamond can be intrinsic diamond, or a diamond film or block which is doped in a late stage by doping growth or adopting a high-energy ion beam, thermal diffusion and other modes.
Furthermore, in the invention, the pulse laser beam for repairing the crystal structure on the surface of the diamond has the pulse width of nanosecond, picosecond, femtosecond and the like, the wavelength range is 2600nm, and the pulse laser beam can be ultraviolet light, visible light or near infrared light.
Furthermore, the average output power of the annealing pulse laser is 10mW-40W, the shape of a light spot can be various shapes such as circle, linearity, strip or plane according to different annealing areas, and the laser intensity (0-100%) and the acting time (more than or equal to 1ns) can be controlled through an optical attenuation sheet and an optical shutter.
Further, in the process of repairing the crystal structure of the single crystal diamond by the ultra-light laser, the diamond can be in the atmosphere of air, vacuum (< 0.1Pa), inert gas (helium or argon, and the like), reducing gas (hydrogen, and the like), the cold and hot table is configured to provide a temperature environment of-196 ℃ (liquid nitrogen) -1200 ℃ in the annealing process, and the cold and hot table is configured to provide a pressure environment of 0.0001-5.5 GPa.
Further, after the radiation annealing treatment is finished, the crystal quality of the whole surface layer and the local surface layer of the diamond is evaluated again by adopting X-ray diffraction and laser Raman spectroscopy, and the repairing effect and the subsequent scheme are determined.
The invention has the beneficial effects that: the method can rapidly and nondestructively judge the crystallization quality of the whole and local areas of the diamond through detection technologies such as X-ray diffraction, laser Raman spectroscopy and the like, and can perform radiation annealing treatment on the areas with poor crystal quality in the diamond by combining ultrashort pulse high-energy laser beams such as nanosecond, picosecond, femtosecond and the like, so that the crystal structure of the diamond can be flexibly and efficiently repaired. The method can make up the defect that the existing method mainly aims at integral annealing and cannot carry out local repair and regulation. The method can quickly and pertinently promote the repair of the surface layer crystal lattice damage of the diamond and improve the crystal quality of the diamond by combining the characteristics of short action time, small heat influence range and high energy density of the ultrashort pulse laser and adjusting the process parameters and controlling the annealing atmosphere and the temperature and pressure conditions, is particularly suitable for doping the diamond film, can effectively improve the uniformity and the crystal quality of the diamond film and optimizes the process performance of the film.
Drawings
FIG. 1 is a flow chart of a method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser provided by the invention;
fig. 2 is a laser raman spectrum detection result of a diamond crystal structure before and after annealing in which an ultra-short pulse laser beam is used to anneal a diamond sample into which high-energy boron ions are injected under the process conditions of example 3.
In the figure, (A) before the high-energy ion implantation diamond annealing and (B) after the high-energy ion implantation diamond annealing.
Detailed Description
The invention is further illustrated by the following figures and examples.
As shown in figure 1, by detection technologies such as X-ray diffraction, laser Raman spectroscopy and the like, the method can rapidly and nondestructively judge the crystallization quality of the whole and local areas of the diamond, and can perform radiation annealing treatment on the corresponding areas with poor crystal quality in the diamond by combining ultrashort pulse high-energy laser beams, so that the crystal structure of the diamond can be flexibly and efficiently repaired.
Example 1
A method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser comprises the following steps:
(1) screening of diamonds
a. The domestic Ib type high-temperature high-pressure synthesized single crystal diamond sample with the size of 3mm multiplied by 0.5mm is adopted as H2SO4/KNO3Heat treating the mixed solution, successively adopting acetone, absolute ethyl alcohol and deionized water to make ultrasonic cleaning,repeatedly cleaning for 3 times, each time for 5 min;
b. and judging the integral crystallization quality of the diamond by adopting X-ray diffraction, and screening the high-temperature high-pressure synthetic diamond of which the half-height width of an X-ray rocking curve is more than or equal to 150 arcsec.
(2) Selection of diamond surface layer repair area
Scanning the selected high-temperature high-pressure synthetic diamond by using a laser Raman spectrometer to determine that the depth of the diamond is 1332.5cm-1The distribution state of the first-order intrinsic Raman peak of nearby diamond is selected, and the intrinsic Raman peak of diamond is invisible or its half-height width is greater than or equal to 10cm-1And the location thereof is marked.
(3) Repair of diamond surface crystal structure
a. Placing the marked high-temperature high-pressure synthetic diamond in a vacuum cavity, filling hydrogen into the cavity, wherein the gas pressure is 100Pa, and the temperature of a cold-hot table is 25 ℃.
b. The laser power is 20W, the pulse width is 200fs, the laser wavelength is 1030nm, the frequency is 200kHz, the light spot is a strip-shaped light spot with the width of 10 mu m and the length of 50 mu m, and the laser scanning step length is 0.1 mm/s.
c. Selecting a 50% optical attenuation sheet, setting an optical shutter to be 10 mu s, focusing laser equipment on a diamond surface marking area, and carrying out radiation annealing on the selected area of the diamond surface by adopting an ultrashort pulse laser beam.
d. And after the radiation annealing treatment is finished, detecting the crystal quality of the whole surface layer and the local area of the high-temperature and high-pressure synthetic diamond by adopting X-ray diffraction and laser Raman spectroscopy, and determining the change of an X-ray rocking curve and the intrinsic Raman peak of the diamond.
Example 2
A method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser comprises the following steps:
(1) screening of diamonds
a. Carrying out aqua regia heat treatment on a IIa type CVD synthetic single crystal diamond sample with the nitrogen-doped growth size of 10mm multiplied by 1mm, sequentially carrying out ultrasonic cleaning on the sample by acetone, absolute ethyl alcohol and deionized water, and repeatedly cleaning for 3 times, wherein the cleaning time is 5min each time;
b. and judging the integral crystallization quality of the diamond by adopting X-ray diffraction, and screening the high-temperature high-pressure synthetic diamond of which the half-height width of an X-ray rocking curve is more than or equal to 150 arcsec.
(2) Selection of diamond surface layer repair area
Scanning the selected nitrogen-doped grown CVD diamond by using a laser Raman spectrometer to determine the depth of the diamond to be 1332.5cm-1The distribution state of the first-order intrinsic Raman peak of nearby diamond is selected, and the intrinsic Raman peak of diamond is invisible or its half-height width is greater than or equal to 10cm-1And the location thereof is marked.
(3) Repair of diamond surface crystal structure
a. Placing the marked CVD diamond grown by nitrogen doping in a vacuum cavity, filling argon into the cavity, wherein the gas pressure is 1000Pa, and the temperature of the cold and hot table is-196 ℃ in liquid nitrogen.
b. The power of a laser is 30W, the pulse width is 10ps, the laser wavelength is 532nm, the frequency is 100kHz, a light spot is circular, the diameter is 10 mu m, and the laser scanning step length is 0.5 mm/s.
c. Selecting 75% optical attenuation sheets, setting an optical shutter to be 20 mu s, focusing laser equipment on a diamond surface marking area, and carrying out radiation annealing on the selected area of the diamond surface of the nitrogen-doped growth CVD by adopting ultrashort pulse laser beams.
d. And after the radiation annealing treatment is finished, detecting the crystal quality of the whole surface layer and the local area of the CVD diamond grown by nitrogen doping by adopting X-ray diffraction and laser Raman spectroscopy, and determining the change of an X-ray rocking curve and the intrinsic Raman peak of the diamond.
Example 3
A method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser comprises the following steps:
(1) screening of diamonds
a. The IIb type single crystal diamond sample with the size of 5mm multiplied by 0.2mm doped by high-energy boron ion implantation is adopted as H2SO4/KNO3Heat treating the mixed solution, and successively adoptingUltrasonic cleaning with acetone, anhydrous alcohol and deionized water, and repeatedly cleaning for 3 times, wherein the cleaning time is 5min each time;
b. and judging the crystallization quality of the ion-implanted boron-doped diamond by adopting X-ray diffraction, and screening a diamond sample with the X-ray rocking curve full width at half maximum of more than or equal to 150 arcsec.
(2) Selection of diamond surface layer repair area
Performing surface scanning on the selected ion-implanted boron-doped diamond by using a laser Raman spectrometer, and determining that the surface scanning is 1332.5cm-1The distribution state of the first-order intrinsic Raman peak of nearby diamond is selected, and the intrinsic Raman peak of diamond is invisible or its half-height width is greater than or equal to 10cm-1And the location thereof is marked.
(3) Repair of diamond surface crystal structure
a. And (3) implanting marked ions into the boron-doped diamond and placing the boron-doped diamond into a diamond pressure cavity configured in a vacuum cavity, wherein the cavity is in an atmospheric atmosphere, the pressure of the diamond pressure cavity is 3GPa, and the temperature of the cold and hot table is 800 ℃.
b. The laser power is 40W, the pulse width is 20ns, the laser wavelength is 355nm, the frequency is 50kHz, the light spot is rectangular, the length is 20 mu m, the width is 20 mu m, and the laser scanning step length is 1 mm/s.
c. Selecting a 50% optical attenuation sheet, setting an optical shutter to be 40 mu s, focusing laser equipment on a diamond surface marking area, and carrying out radiation annealing on the selected area of the diamond surface doped with boron by using ultra-short pulse laser beams.
d. And after the radiation annealing treatment is finished, detecting the crystal quality of the whole surface layer and the local area of the diamond doped with boron by ion implantation by adopting X-ray diffraction and laser Raman spectroscopy, and determining the change of an X-ray rocking curve and the intrinsic Raman peak of the diamond.
As shown in fig. 2, under the process conditions of this embodiment, the ultra-short pulse laser beam is used to perform annealing treatment on the diamond sample implanted with high-energy boron ions, and the diamond crystal structure completely destroyed by the high-energy boron ion beam before annealing is significantly repaired by annealing.
Claims (10)
1. A method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser is characterized by comprising the following steps:
(1) screening of diamonds
a. Cleaning the diamond by sequentially adopting different chemical reagents;
b. judging the integral crystallization quality of the diamond by adopting X-ray diffraction, and screening the diamond of which the half-height width of an X-ray rocking curve is more than or equal to 150 arcsec;
(2) selection of diamond surface layer repair area
Performing surface scanning on the selected diamond by using a laser Raman spectrometer to determine the distribution state of a first-order intrinsic Raman peak of the diamond on the surface, and selecting the intrinsic Raman peak of the diamond which is invisible or the half-height width of the intrinsic Raman peak of the diamond which is not less than 10cm-1And marking the location thereof;
(3) repair of diamond surface crystal structure
a. Placing the marked diamond on a cold and hot table of a vacuum cavity, and focusing the ultrashort pulse laser equipment on a diamond surface marking area;
b. adopting ultrashort pulse laser to perform radiation annealing on the selected area of the diamond surface;
c. and after the radiation annealing treatment is finished, detecting the crystal quality of the whole surface layer and the local surface layer of the diamond by adopting X-ray diffraction and laser Raman spectroscopy.
2. The method for repairing a single crystal diamond crystal structure based on ultrashort pulse laser as claimed in claim 1, wherein the pulse width of the ultrashort pulse laser is nanosecond, picosecond or femtosecond.
3. A method for repairing a single crystal diamond crystal structure based on an ultrashort pulse laser as recited in claim 1, wherein the average output power of the ultrashort pulse laser is 10 mW-40W.
4. The method for repairing a single crystal diamond crystal structure based on an ultrashort pulse laser as claimed in claim 1, wherein the spot shape of the ultrashort pulse laser is circular, linear, bar-shaped or planar.
5. The method for repairing a single crystal diamond structure based on ultrashort pulse laser as claimed in claim 1, wherein the wavelength of the ultrashort pulse laser is 210-2600nm, which can be ultraviolet, visible or near infrared light.
6. The method for repairing the crystal structure of a single crystal diamond based on an ultrashort pulse laser as claimed in claim 1, wherein in the step a for repairing the crystal structure on the surface of the diamond of (3), the temperature of the cold and hot table for placing the diamond is in the range of-196 ℃ to 1200 ℃.
7. The method for repairing the crystal structure of a single crystal diamond based on an ultrashort pulse laser as recited in claim 1, wherein in the step (3) for repairing the crystal structure on the surface of the diamond, the vacuum chamber for placing the diamond is vacuum atmosphere, inert gas atmosphere or reducing gas atmosphere.
8. The method for repairing the crystal structure of a single crystal diamond based on an ultrashort pulse laser as claimed in claim 1, wherein in the step (3) for repairing the crystal structure of the surface of the diamond, a diamond pressure chamber can be placed in a vacuum chamber for placing the diamond, and a pressure environment of 0.0001-5.5GPa can be provided.
9. The method for repairing single crystal diamond crystal structure based on ultrashort pulse laser as claimed in claim 1, wherein the repaired diamond can be produced naturally, or synthesized by high temperature and high pressure, gas phase chemical deposition method, and the diamond can be intrinsic diamond, or diamond film or block grown by doping or post-doped by high energy ion beam and thermal diffusion method.
10. The method for repairing single crystal diamond crystal structure based on ultrashort pulse laser as claimed in claim 1, wherein the side length of the repaired diamond is 0.1-100mm, the thickness is 0.000001-10mm, and the repaired crystal face is generally a polished polygonal plane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114836836A (en) * | 2022-06-23 | 2022-08-02 | 济南大学 | Local rapid blackening method for lithium niobate wafer/lithium tantalate wafer |
| CN114836829A (en) * | 2022-04-27 | 2022-08-02 | 河南天璇半导体科技有限责任公司 | Method for producing single crystal diamond by MPCVD method |
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| CN106835069A (en) * | 2016-12-21 | 2017-06-13 | 武汉大学 | Semiconductor diamond film doping post-processing approach and device based on femtosecond laser |
| CN110281142A (en) * | 2019-06-20 | 2019-09-27 | 山东大学 | Diamond seed preparation method, diamond seed and monocrystalline |
| CN110938864A (en) * | 2019-11-08 | 2020-03-31 | 武汉大学 | Method for efficiently regulating and controlling dislocation density of CVD single crystal diamond local area |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114836829A (en) * | 2022-04-27 | 2022-08-02 | 河南天璇半导体科技有限责任公司 | Method for producing single crystal diamond by MPCVD method |
| CN114836836A (en) * | 2022-06-23 | 2022-08-02 | 济南大学 | Local rapid blackening method for lithium niobate wafer/lithium tantalate wafer |
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Application publication date: 20201120 |