CN110565164A - Method for preventing seed crystal from drifting in process of growing diamond by MPCVD and growing method - Google Patents
Method for preventing seed crystal from drifting in process of growing diamond by MPCVD and growing method Download PDFInfo
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- CN110565164A CN110565164A CN201910942587.0A CN201910942587A CN110565164A CN 110565164 A CN110565164 A CN 110565164A CN 201910942587 A CN201910942587 A CN 201910942587A CN 110565164 A CN110565164 A CN 110565164A
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the field of diamond manufacturing, in particular to a seed crystal drifting prevention method and a seed crystal drifting prevention method in an MPCVD diamond growth process. A method for preventing seed crystal from drifting in an MPCVD diamond growth process comprises the following steps: s10, processing the substrate, and grinding the upper surface of the substrate to roughen the upper surface of the substrate; s20, placing a seed crystal on the substrate, and heating the substrate with the seed crystal to a first temperature threshold value; s30, placing the substrate and the seed crystals after the heating treatment into an MPCVD device, and arranging the seed crystals in a close-packed manner; and S40, preparing to grow diamond. The method for preventing seed crystal from drifting in the process of growing diamond by MPCVD can achieve the following effects in the using process: 1. the seed crystal drift can be effectively avoided on the premise of not additionally processing the substrate. 2. The seed crystals are arranged in a close-packed mode, the interval is reduced, the seed crystals can be prevented from drifting, more seed crystals can be placed in a limited area, and the temperature uniformity of the seed crystals can be improved.
Description
Technical Field
the invention relates to the field of diamond manufacturing, in particular to a seed crystal drifting prevention method and a seed crystal drifting prevention method in an MPCVD diamond growth process.
background
Because diamond has extremely high hardness, thermal conductivity, insulativity, light transmittance, and excellent physical and chemical properties such as acid resistance, heat resistance, radiation resistance and the like, the diamond is widely applied to various fields such as industry, scientific research and the like.
Microwave Plasma Chemical Vapor Deposition (MPCVD) is currently the predominant method for diamond synthesis. The method is mainly characterized in that the electron density in the plasma is high, the concentration of generated atomic H is high, no electrode pollution exists, stable plasma can be generated under larger pressure, and the quality of the grown diamond is higher.
the MPCVD method is to deposit diamond on the surface of a seed crystal on a substrate table by plasma. The seed crystal is typically placed on a molybdenum plate within a molybdenum holder. To achieve mass production, a plurality of seed crystals (diamond single crystal wafer) are placed in an array on a substrate table. However, when a plurality of diamonds grow in the same batch, firstly, hydrogen needs to be introduced, the pressure and the microwave power are gradually increased after the plasma is started, the surface of the seed crystal is etched, and then, the diamond growth is realized by introducing process gases such as methane and the like. However, the seed crystal is easy to drift in the process of introducing hydrogen, starting to increase the air pressure and microwave power. Seed crystal drift not only changes the position of the seed crystal, causes uneven temperature among the seed crystals, but also influences the deposition quality of the diamond. If the seed drifts out of the range of the plasma cage, the diamond growth can be stopped.
The patent document with application number 201810163115.0 discloses a method for improving the stability of single crystal diamond prepared by MPCVD, wherein a substrate bearing a seed crystal is provided with a groove, and the purpose of the method is not to solve the problem that the seed crystal is easy to drift, but is also a technical means for solving the drift of the seed crystal in the field.
In the prior art, grooves are dug on the surface of a molybdenum sheet or a molybdenum sheet with holes is placed on the surface of the molybdenum sheet, and seed crystals are placed in the grooves or the holes to play a role in fixing. But has the following problems:
1. Seed crystals are placed in the grooves or holes of the molybdenum sheet, and diamond polycrystal or carbon black growing on the edge of the molybdenum sheet influences the growth quality of the diamond in the growing process; 2. the processing cost is high. The molybdenum sheet groove and the molybdenum sheet with the holes can be used only once basically; 3. the machining precision cannot be guaranteed. If the processing precision and the processing quality inside the groove or in the hole are inconsistent, the heat dissipation efficiency of the seed crystal is different, and the temperature uniformity of the seed crystal is influenced.
therefore, there is a need in the art for innovations and research in the invention for preventing seed crystal drift.
disclosure of Invention
In view of the above-mentioned shortcomings in the prior art, the present invention aims to provide a method for preventing seed crystal drift during the growth of diamond by MPCVD, which can prevent seed crystal drift at the beginning of diamond growth and further prevent the growth effect from being influenced by the moving position during the diamond growth.
in order to achieve the purpose, the invention adopts the following technical scheme:
A method for preventing seed crystal from drifting in an MPCVD diamond growth process comprises the following steps:
s10, processing the substrate, and grinding the upper surface of the substrate to roughen the upper surface of the substrate;
s20, placing a seed crystal on the substrate, and heating the substrate with the seed crystal to a first temperature threshold value;
S30, placing the substrate and the seed crystals after the heating treatment into an MPCVD device, and arranging the seed crystals in a close-packed manner;
And S40, preparing to grow diamond.
Preferably, the substrate is a molybdenum sheet.
In the preferred method for preventing seed crystal drift in the MPCVD diamond growth process, in step S10, the polishing the substrate is specifically performed by polishing the substrate with coarse sandpaper to form a plurality of scratches crossing each other.
preferably, in step S10, after polishing the substrate, the substrate is rinsed with deionized water, and then the substrate is placed in acetone, then isopropanol solution for ultrasonic cleaning, and finally dried with nitrogen.
preferably, in the method for preventing seed crystal drift in the MPCVD diamond growth process, in step S20, the heating specifically comprises:
The substrate and seed crystal are placed on a hot plate and heated above the first temperature threshold.
preferably, in the method for preventing seed crystal drift in the MPCVD diamond growth process, in step S20, the heating specifically comprises:
And putting the substrate and the seed crystal into MPCVD equipment, vacuumizing, introducing hydrogen, starting a microwave source, raising the air pressure and the microwave source power after the plasma is started, keeping the temperature of the seed crystal and the substrate at the second temperature threshold for a first preset time.
In the preferred method for preventing seed crystal drift in the MPCVD diamond growth process, in the step S30, the close packing mode is to control the seed crystal spacing distance not to exceed a preset distance.
Preferably, in the MPCVD method for preventing seed crystal from drifting during diamond growth, the step S40 specifically includes:
S41, introducing hydrogen, and setting the hydrogen flow as a first flow rate threshold value;
S42, after the plasma is started, the air pressure and the plasma power are gradually increased, and after the temperature reaches a third temperature threshold, the hydrogen flow rate is restored to a second flow rate threshold;
s43, etching the surface of the seed crystal by using plasma;
And S44, after the etching is finished, keeping the hydrogen flow unchanged, introducing methane with the flow as a third flow rate threshold, raising the seed crystal temperature to a fourth temperature threshold, and starting diamond growth.
An MPCVD method for growing diamond uses the method for preventing seed crystal drift.
the MPCVD method for growing diamond preferably further comprises the steps of:
Stopping introducing methane after the diamond grows for the second preset time, and etching the grown sample by using plasma; after the etching is finished, the air pressure and the microwave source power are gradually reduced, and the sample is taken out.
Compared with the prior art, the method for preventing seed crystal from drifting and the method for preventing seed crystal from drifting in the process of growing diamond by MPCVD provided by the invention can achieve the following effects in the using process:
1. The seed crystal drift can be effectively avoided on the premise of not additionally processing the substrate.
2. The seed crystals are arranged in a close-packed mode, the interval is reduced, the seed crystals can be prevented from drifting, more seed crystals can be placed in a limited area, and the temperature uniformity of the seed crystals can be improved.
drawings
FIG. 1 is a flow chart of a method for preventing seed crystal from drifting in the process of MPCVD diamond growth provided by the invention.
MPCVD (Modifie Plasma Chemical Vapor Deposition)
Detailed Description
in order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
referring to fig. 1, the present invention provides a method for preventing seed crystal from drifting during MPCVD diamond growth, comprising the steps of:
S10, processing the substrate, and grinding the upper surface of the substrate to roughen the upper surface of the substrate;
S20, placing a seed crystal on the substrate, and heating the substrate with the seed crystal to a first temperature threshold value;
s30, placing the substrate and the seed crystals after the heating treatment into an MPCVD device, and arranging the seed crystals in a close-packed manner;
and S40, preparing to grow diamond.
Preferably, in this embodiment, the substrate is a molybdenum sheet.
specifically, the substrate is polished to increase friction, and a tool for polishing the substrate is sand paper; the first temperature threshold is 200 ℃, and the preheating time is 10 minutes.
selecting 9 high-temperature and high-pressure single-crystal diamond sheets with the length, width and height of 3mm, 3mm and 1mm as seed crystals, polishing the two sides of all the seed crystals, and polishing the two sides of the molybdenum sheet on which the seed crystals are placed; the upper surface of the molybdenum sheet is polished by 400-mesh sand paper to roughen the upper surface of the molybdenum sheet, diamond seed crystals are placed on the molybdenum sheet, the polished roughened surface of the molybdenum sheet faces upwards and is in direct contact with the diamond seed crystals, and 9 seed crystals are densely arranged in 3 rows and 3 columns; the molybdenum wafer and the seed crystal are placed in an MPCVD apparatus for a diamond growth program. Through the double modes of molybdenum sheet polishing and seed crystal close packing, seed crystal drifting can be effectively prevented, and the effect is excellent.
Preferably, in this embodiment, in the step S10, the grinding the substrate is specifically to grind the substrate with coarse sandpaper to form a plurality of scratches crossing each other. Specifically, the grinding directions are mutually crossed, and can be mutually vertical or form a certain angle, so that the friction force can be effectively increased.
As a preferable scheme, in this embodiment, in step S10, after the substrate is polished, the substrate is rinsed with deionized water, and then the substrate is placed in acetone, then placed in an isopropanol solution for ultrasonic cleaning, and finally dried with nitrogen. Specifically, the ionized water is purified by a water purifier to reach the standard (reaching the national water standard) by using activated carbon as a filter layer and then is electrolyzed by a diaphragm to generate two kinds of active water; the ultrasonic cleaning is to utilize the direct and indirect action of the cavitation action, the acceleration action and the direct current action of ultrasonic waves in liquid on the liquid and dirt to disperse, emulsify and peel off a dirt layer so as to achieve the aim of cleaning; the cleanliness of the substrate processed in this way can meet the clean environment for diamond growth.
preferably, in this embodiment, in step S20, the heating specifically includes:
The substrate and seed crystal are placed on a hot plate and heated above the first temperature threshold.
Specifically, the substrate and the seed crystal are directly heated to the first temperature threshold by using a heating plate, preferably, the first temperature threshold is 200 ℃, and the heating time is about 10 minutes. The heating mode has the advantages of convenience and trouble saving.
Preferably, in this embodiment, in step S20, the heating specifically includes:
And putting the substrate and the seed crystal into MPCVD equipment, vacuumizing, introducing hydrogen, starting a microwave source, raising the air pressure and the microwave source power after the plasma is started, keeping the temperature of the seed crystal and the substrate at the second temperature threshold for a first preset time.
Specifically, the second temperature threshold is 300 ℃, and the first predetermined time is preferably 10 minutes. After 10 minutes, the pressure and power are gradually reduced, and the seed crystal and the molybdenum sheet are taken out and then taken out for use.
preferably, in this embodiment, in the step S30, the close packing mode is to control the seed crystal spacing distance not to exceed a predetermined distance. The predetermined distance is preferably 0.5 mm. And rearranging seed crystals on the upper surface of the molybdenum sheet, wherein the interval between the seed crystals is controlled within 0.5 mm.
preferably, in this embodiment, the step S40 specifically includes:
S41, introducing hydrogen, and setting the hydrogen flow as a first flow rate threshold value;
s42, after the plasma is started, the air pressure and the plasma power are gradually increased, and after the temperature reaches a third temperature threshold, the hydrogen flow rate is restored to a second flow rate threshold;
S43, etching the surface of the seed crystal by using plasma;
and S44, after the etching is finished, keeping the hydrogen flow unchanged, introducing methane with the flow as a third flow rate threshold, raising the seed crystal temperature to a fourth temperature threshold, and starting diamond growth.
specifically, the glow is a light-emitting phenomenon after plasma of gas such as hydrogen and the like; the first flow rate threshold value is preferably 50sccm, the flow rate of the rushing hydrogen in the initial stage is low, and the main effect is that the situation that the seed crystal moves because of the blowing of the hydrogen formed when the hydrogen enters the seed crystal can be prevented by reducing the flow rate. The third temperature threshold is preferably 850 deg.C, the second flow rate threshold is preferably 200sccm, the third flow rate threshold is preferably 16sccm, and the fourth temperature threshold is preferably 1000 deg.C.
Example 2
The invention also provides an MPCVD method for growing diamond, which comprises the method for preventing seed crystal drifting in the embodiment 1.
Preferably, the present embodiment further includes: stopping introducing methane after the diamond grows for the second preset time, and etching the grown sample by using plasma; after the etching is finished, the air pressure and the microwave source power are gradually reduced, and the sample is taken out.
Specifically, the second predetermined time is preferably 24 hours.
And etching the surface of the seed crystal by using hydrogen plasma, keeping the hydrogen flow unchanged after the etching is finished, introducing methane in addition, raising the temperature of the seed crystal to the temperature, starting diamond growth, stopping introducing methane after the diamond grows for 24 hours, and etching the grown sample by using the hydrogen plasma. After the etching is finished, the air pressure and the microwave source power are gradually reduced, and the sample is taken out. In the process, the diamond seed crystal does not drift and the like.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (10)
1. a method for preventing seed crystal from drifting in an MPCVD diamond growth process is characterized by comprising the following steps:
S10, processing the substrate, and grinding the upper surface of the substrate to roughen the upper surface of the substrate;
s20, placing a seed crystal on the substrate, and heating the substrate with the seed crystal to a first temperature threshold value;
S30, placing the substrate and the seed crystals after the heating treatment into an MPCVD device, and arranging the seed crystals in a close-packed manner;
and S40, preparing to grow diamond.
2. A method for preventing seed crystal drift during MPCVD diamond growth according to claim 1, wherein the substrate is a molybdenum sheet.
3. A method for preventing seed crystal drift during MPCVD diamond growth according to claim 1, wherein in the step S10, the grinding of the substrate is performed by grinding the substrate with coarse sandpaper to form a plurality of scratches crossing each other.
4. A method for preventing seed crystal from drifting in an MPCVD diamond growth process according to claim 3, wherein in step S10, after the substrate is polished, the substrate is rinsed with deionized water, then the substrate is placed in acetone, then placed in isopropanol solution for ultrasonic cleaning, and finally dried with nitrogen.
5. A method for preventing seed crystal drift in an MPCVD diamond growth process according to claim 1, wherein in the step S20, the heating is specifically:
The substrate and seed crystal are placed on a hot plate and heated above the first temperature threshold.
6. A method for preventing seed crystal drifting in an MPCVD diamond growth process according to claim 5, wherein in step S20, the heating is specifically:
And putting the substrate and the seed crystal into MPCVD equipment, vacuumizing, introducing hydrogen, starting a microwave source, raising the air pressure and the microwave source power after the plasma is started, keeping the temperature of the seed crystal and the substrate at the second temperature threshold for a first preset time.
7. a method for preventing seed crystal drift during MPCVD diamond growth according to claim 1, wherein in step S30, the close packing is such that the seed crystal spacing distance is controlled not to exceed a predetermined distance.
8. a method for preventing seed crystal drift in an MPCVD diamond growth process according to claim 1, wherein the step S40 specifically is:
S41, introducing hydrogen, and setting the hydrogen flow as a first flow rate threshold value;
S42, after the plasma is started, the air pressure and the plasma power are gradually increased, and after the temperature reaches a third temperature threshold, the hydrogen flow rate is restored to a second flow rate threshold;
S43, etching the surface of the seed crystal by using plasma;
and S44, after the etching is finished, keeping the hydrogen flow unchanged, introducing methane with the flow as a third flow rate threshold, raising the seed crystal temperature to a fourth temperature threshold, and starting diamond growth.
9. A method of MPCVD diamond growth using the seed crystal drift prevention method of any of claims 1-8.
10. The MPCVD method of growing diamond according to claim 9, further comprising the step of:
Stopping introducing methane after the diamond grows for the second preset time, and etching the grown sample by using plasma; after the etching is finished, the air pressure and the microwave source power are gradually reduced, and the sample is taken out.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112391680A (en) * | 2020-11-16 | 2021-02-23 | 物生生物科技(北京)有限公司 | Splicing growth process for large-size single crystal diamond |
| CN114016130A (en) * | 2021-11-10 | 2022-02-08 | 哈尔滨工业大学 | Method for welding single crystal diamond seed crystal and sample holder |
| CN114059159A (en) * | 2021-11-18 | 2022-02-18 | 北京大学东莞光电研究院 | Diamond growth method |
| CN115074823A (en) * | 2022-04-27 | 2022-09-20 | 华灿光电(苏州）有限公司 | Epitaxial tray for improving yield of epitaxial wafer forming and using method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20191213 |