CN110760816A - Diamond on-line detection growth device and growth defect treatment method - Google Patents

Diamond on-line detection growth device and growth defect treatment method Download PDF

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Publication number
CN110760816A
CN110760816A CN201911213947.XA CN201911213947A CN110760816A CN 110760816 A CN110760816 A CN 110760816A CN 201911213947 A CN201911213947 A CN 201911213947A CN 110760816 A CN110760816 A CN 110760816A
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diamond
growth
optical camera
reaction chamber
measuring device
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彭国令
黄翀
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Changsha New Material Industry Research Institute Co Ltd
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Changsha New Material Industry Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52Controlling or regulating the coating process
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01CMEASURING DISTANCES, LEVELS OR BEARINGS; SURVEYING; NAVIGATION; GYROSCOPIC INSTRUMENTS; PHOTOGRAMMETRY OR VIDEOGRAMMETRY
    • G01C11/00Photogrammetry or videogrammetry, e.g. stereogrammetry; Photographic surveying
    • G01C11/04Interpretation of pictures

Abstract

The invention provides a diamond on-line detection growth device and a growth defect treatment method, wherein the diamond on-line detection growth device comprises a reaction chamber, an optical camera measuring device, a gas storage and conveying system and a control device, the optical camera measuring device is arranged outside the reaction chamber, the optical camera measuring device shoots and reflects the growth condition of diamond in the chamber in real time through an observation window and feeds the growth condition back to a central processing unit of the control device, and the central processing unit controls whether a carbon source gas mixture and an etching gas mixture enter the reaction chamber according to a detection result, so that the growth process of diamond can be recorded in real time, growth defects can be treated in time, and the growth quality and yield of diamond are ensured.

Description

Diamond on-line detection growth device and growth defect treatment method
Technical Field
The invention relates to the technical field of crystal growth, in particular to a diamond on-line detection growth device and a growth defect treatment method.
Background
The diamond has excellent physical and chemical properties, so that the diamond can be competent for the fields of drill bits, semiconductors, nonmetal cutting and the like, and has excellent performance. However, the reserves of natural diamond are limited, so that various methods for synthesizing diamond, such as a high temperature and high pressure method, a hot filament chemical vapor deposition method, etc., have been developed, wherein the method for synthesizing diamond by Microwave Plasma Chemical Vapor Deposition (MPCVD) can synthesize high-quality and large-area diamond without introducing impurities, and thus is widely used.
The quality of diamond synthesized by the MPCVD (microwave plasma chemical vapor deposition) method is related to various factors, including carbon source concentration, gas flow rate proportion, substrate table height, microwave power, synthesis temperature and the like. In the process of synthesizing diamonds in batches, the stability of the synthesis process can be influenced by the change of any synthesis parameter, particularly, in the long-time equipment operation process, the process is a dynamic stable balance process, the synthesis parameter can be inevitably disturbed (temperature is gradually increased or the thickness of diamond seed crystals is gradually increased and the like) along with the growth of the diamonds, the change of the growth environment has great influence on the appearance of the surfaces of the diamonds, and further, edge polycrystal or middle non-single crystal diamond phases are generated, once the situation occurs, irreversible consequences can occur if the situation is not processed in time, namely, the growth quality is seriously reduced, and the product yield is influenced.
In the prior art, a method for directly monitoring defects in the diamond growth process is not available. The existing monitoring only monitors the temperature generally, and the online detection modes mainly comprise two modes: temperature measurement technology and local plasma testing technology. Only real-time temperature measurement of one diamond seed crystal or detection of plasma parameters in a certain area can be provided. The non-contact infrared thermometer adjusts the laser point position to the position to be measured through the observation window, and real-time monitoring is carried out after the laser point position is fixed.
In the process of synthesizing diamonds in batches and synthesizing single diamonds, a non-contact temperature measuring device can obtain a temperature measuring result of a certain point, and a plasma emission spectrometer can measure the plasma type, density, distribution information and the like of a certain area, but the temperature is only one of the influencing factors of diamond growth, the quality of the synthesized diamonds cannot be directly judged based on the monitoring result of the temperature, and the synthesized diamonds can only be taken out from a CVD cavity for characterization after the growth is completed, so that the growth quality is judged. The processing mode greatly wastes time and labor cost, and is not beneficial to industrial production.
Therefore, how to design an on-line detection growth device for the diamond can detect the defects in the growth process of the diamond in real time and take certain measures aiming at the defects to ensure the growth quality and the yield of the diamond.
Disclosure of Invention
In order to solve the problems, the invention provides a diamond on-line detection growth device and a growth defect processing method, wherein the real-time detection device for diamond growth reflects the growth condition of diamond in a cavity in real time through an optical camera measuring device and feeds back the result to a central processing unit, and the central processing unit controls whether a carbon source and etching gas enter a reaction cavity or not according to the detection result, so that the growth process of the diamond can be recorded in real time, growth defects can be timely processed, and the growth quality and the yield of the diamond can be ensured.
In order to achieve the above object, the present invention provides an online diamond growth detection apparatus, comprising:
the reaction chamber comprises a closed area suitable for containing diamond growth, and the outer side wall of the reaction chamber is provided with at least one observation window;
an optical camera measuring device including a measuring device body and an optical camera, the optical camera measuring device being installed at a position where a sample inside the reaction chamber can be observed through the observation window;
the gas storage and conveying system is connected with the vent holes in the reaction chamber through a gas conveying gas path, so that reaction gas or etching gas can enter the reaction chamber, and the gas storage and conveying system comprises a carbon source storage system and an etching gas storage system;
a control device comprising a central processing unit;
one mounting mode of the optical camera measuring device is that the optical camera measuring device is directly fixed outside the observation window; the other installation mode of the optical camera measuring device is that the optical camera measuring device is installed outside the reaction chamber through a fixing part, so that the optical camera can monitor the condition of a sample in the reaction chamber through an observation window;
the optical camera and the gas storage and delivery system are respectively and electrically connected with the central processing unit.
Preferably, the gas storage and delivery system further comprises an inert gas and hydrogen storage system, and optionally, other gas storage systems required by growth and doping can be further included.
Preferably, the gas storage and delivery system further comprises a gas mixing device for mixing the carbon source, the etching gas and the like with the inert gas, the hydrogen gas and other necessary gases as required.
Preferably, the optical camera measuring device is movably connected with a fixed part on the reaction chamber through a rotating shaft mechanism and can shoot the diamond in the reaction chamber through an observation window.
Preferably, the rotating shaft mechanism comprises an upper support, a lower support and a damping rotating shaft, the upper support is connected with the outer wall of the reaction chamber through a hinged support, the lower support is arranged on the measuring device body, and the damping rotating shaft is inserted between the upper support and the lower support.
Preferably, the opening diameter of the viewing window is less than 40 mm.
Preferably, the number of the optical camera measuring devices is at least one.
Preferably, the optical camera is a high-fidelity camera, the included angle between the shooting angle of the optical camera and the surface of the seed crystal is adjusted to be 50-70 degrees through the rotating shaft mechanism, so that the view of the plasma discharge and the diamond growth surface can be better captured, and the high-fidelity camera can record images and videos of the diamond growth surface for the purpose of researching the diamond growth process.
Preferably, the carbon source can be selected from one or more of methane, ethane, propane, butane, ethylene and acetylene.
Preferably, the carbon source is methane.
Preferably, the etching gas is oxygen.
Preferably, a pressure sensor for detecting the gas pressure in the reaction chamber, a concentration sensor for detecting the oxygen concentration, and a temperature sensor for detecting the temperature of the reaction chamber are further arranged in the reaction chamber.
Preferably, the real-time detection device for diamond growth further comprises a display screen for displaying the temperature, the gas pressure and the oxygen concentration in the reaction chamber.
Preferably, the material of the observation window is transparent.
The invention also provides a diamond growth defect treatment method of the diamond online detection growth device, which comprises the following steps:
s1, sending a diamond growth picture to a central processing unit by the optical camera measuring device, and judging that growth defects appear by the central processing unit;
s2, the control device controls the gas storage and delivery system to stop the carbon source gas mixture from entering the reaction chamber;
s3, the control device controls the gas storage and delivery system to access the etching gas mixture to the reaction chamber;
s4, the optical camera measuring device transmits the etching picture to the central processing unit in real time, whether etching is finished is judged, and if yes, the step S5 is executed; if not, go to step S3;
and S5, stopping introducing the etching gas mixture, opening the carbon source gas mixture, and continuing to grow the diamond.
Preferably, in step S1, the growth defect is a picture that is sent to the central processing unit by the optical camera measuring device, and an abnormal bright spot appears on the diamond growth surface.
It has been found that, surprisingly, during the synthesis of diamond, part of the diamond surface may have abnormal bright spots with higher brightness than other parts of the diamond, which may eventually form defects in the diamond, such as carbon black, during the subsequent synthesis process. There is no report on the bright spot in the prior art, and there is no processing method and process for the bright spot. According to the invention, etching gas is introduced in the synthesis process, and the defects on the diamond are removed in an etching mode, so that the high-quality diamond without or with fewer defects is synthesized for a long time.
Preferably, in the step S3, the concentration of the etching gas in the etching gas mixture is 4% to 8%.
Preferably, in the step S4, one mode of determining whether the etching is completed is that the abnormal bright point disappears. When the abnormal bright point disappears, the etching is finished.
Preferably, in step S4, another way to determine whether the etching is completed is to complete the etching when the etching reaches a predetermined time. If the preset time is too short, the defect of the abnormal bright point can not be completely etched, the inside of the diamond still has defects, and if the etching time is too long, the formed diamond layer can be etched after the bright point etching is finished, so that the production efficiency is reduced. The skilled person finds, through research, that the etching time is preferably 5-120min, and more preferably 10-30 min.
Preferably, the carbon source gas mixture is a mixed gas of methane and hydrogen.
Preferably, the etching gas mixture is a mixed gas of oxygen and hydrogen.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the diamond on-line detection growth device, the optical camera measuring device is arranged on the outer wall of the reaction chamber through the rotating shaft mechanism, the optical camera shoots the growth condition of the sub-crystals in the reaction chamber through the observation window of the reaction chamber, compared with the traditional shooting camera arranged in the reaction chamber, the cost and the failure rate of the whole device are increased due to the fact that the camera has higher requirements on the camera due to high temperature in the chamber and the existence of mixed gas, the high temperature resistance, corrosion resistance and the like are needed, and the requirement on the camera is reduced due to the fact that the camera is arranged outside the reaction chamber.
2. In the stage of starting the growth of the diamond, the carbon source gas mixture is conveyed into a diamond reaction chamber, in the growth process, an optical camera measuring device outputs a picture to a central processing unit in real time, the central processing unit judges whether an abnormal bright spot appears or not according to the picture, if the abnormal bright spot appears, the control device controls the carbon source gas mixture to stop conveying, under the condition that the growth environment of the diamond is not changed, the etching gas mixture is introduced, meanwhile, the optical camera measuring device 2 still outputs the picture to the central processing unit in real time, when the central processing unit recognizes that the abnormal bright spot disappears, the introduction of the etching gas is stopped, the carbon source gas mixture is continuously introduced, the diamond continues to grow, and the growth quality and the yield of the diamond are ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a diamond on-line detection growth device with a side photograph.
Fig. 2 is a flow chart of a diamond growth defect treatment method provided by the invention.
The reference numbers are as follows:
1. a reaction chamber; 11. an observation window; 2. an optical camera measuring device; 3. a rotating shaft mechanism; 4. a hinged bracket; 5. and (5) seed crystal.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention will be further described with reference to the following figures:
example 1:
referring to fig. 1, the present embodiment provides an on-line diamond growth detection apparatus, which includes
The device comprises a reaction chamber 1, wherein the reaction chamber 1 comprises a closed area suitable for containing diamond growth, and the outer side wall of the reaction chamber 1 is provided with at least one observation window 11;
an optical camera measuring device 2 including a measuring device body and an optical camera, the optical camera measuring device 2 being installed at a position where a sample inside the reaction chamber 1 can be observed through the observation window 11;
the gas storage and conveying system is connected with the vent holes in the reaction chamber 1 through a gas conveying gas path, so that reaction gas or etching gas can enter the reaction chamber 1, and the gas storage and conveying system comprises a carbon source storage system and an etching gas storage system;
a control device comprising a central processing unit;
one way of mounting the optical camera measuring device 2 is to fix it directly outside the observation window 11; another way of installing the optical camera measuring device 2 is to install the optical camera measuring device outside the reaction chamber 1 through a fixing component, so that the optical camera can monitor the condition of the sample inside the reaction chamber 1 through the observation window 11;
the optical camera and the gas storage and delivery system are respectively and electrically connected with the central processing unit.
Compared with the traditional method of arranging the shooting camera in the reaction chamber 1, the method has the advantages that the camera is arranged outside the reaction chamber 1, the requirements on the camera are reduced, the cost is relatively low, the shooting environment of the camera is relatively superior, the failure rate of the camera is reduced, and the stability of the whole device and the accuracy of the shooting result are relatively improved.
In a preferred embodiment, the gas storage and delivery system further comprises an inert gas and hydrogen storage system, and optionally, other gas storage systems required for growth and doping.
In a preferred embodiment, the gas storage and delivery system further comprises a gas mixing device for mixing the carbon source, the etching gas, and the like with the inert gas, the hydrogen gas, and other necessary gases as needed.
As a preferred embodiment, referring to fig. 1, the optical camera measuring device 2 is movably connected with a fixed part on the reaction chamber 1 through a rotating shaft mechanism 3, and can photograph the diamond in the reaction chamber 1 through an observation window 11.
As a preferred embodiment, the rotating shaft mechanism 3 includes an upper support, a lower support and a damping rotating shaft, the upper support is connected with the outer wall of the reaction chamber 1 through a hinged support, the lower support is arranged on the measuring device body, the damping rotating shaft is inserted between the upper support and the lower support, and the arrangement of the damping rotating shaft can easily adjust the shooting angle of the optical camera, so as to better capture the picture of the diamond growth surface.
As a preferred embodiment, since the growth of diamond requires the emission of microwave into the reaction chamber 1, the diameter of the opening of the observation window 11 is reduced as much as possible in order to prevent the leakage of microwave in case of satisfying the photographing of the optical camera, and in this embodiment, the diameter of the observation window 11 is 40 mm.
As a preferred embodiment, there is at least one optical camera measuring device 2, and in this embodiment, there is one optical camera measuring device 3.
In a preferred embodiment, the optical camera is a high-fidelity camera, and the shooting angle of the optical camera is adjusted to be between 50 and 70 degrees from the surface of the seed crystal 5 through the rotating shaft mechanism 3 so as to better capture the view of the plasma discharge and the diamond growth surface, and the high-fidelity camera can record images and videos of the diamond growth surface for the purpose of researching the diamond growth process.
As a preferred embodiment, the carbon source is methane.
In a preferred embodiment, the etching gas is oxygen.
In a preferred embodiment, the reaction chamber 1 is further provided with a pressure sensor for detecting the gas pressure in the reaction chamber, a concentration sensor for detecting the oxygen concentration, and a temperature sensor for detecting the temperature of the reaction chamber.
In a preferred embodiment, the real-time detection device for diamond growth further comprises a display screen for displaying the temperature, the gas pressure and the oxygen concentration in the reaction chamber.
In a preferred embodiment, the viewing window 11 is made of a transparent material.
Example 2:
the invention also provides a diamond growth defect treatment method of embodiment 1, referring to fig. 2, comprising the steps of:
s1, sending the diamond growth picture to a central processing unit by the optical camera measuring device 2, and judging that the growth defect occurs by the central processing unit;
s2, the control device controls the gas storage and delivery system to stop the carbon source gas mixture from entering the reaction chamber 1;
s3, the control device controls the gas storage and delivery system to access the etching gas mixture to the reaction chamber 1;
s4, the optical camera measuring device 2 transmits the etching picture to the central processing unit in real time, whether etching is finished is judged, and if yes, the step S5 is executed; if not, go to step S3;
and S5, stopping introducing the etching gas mixture, opening the carbon source gas mixture, and continuing to grow the diamond.
In a preferred embodiment, in step S1, the growth defect is a picture that the optical camera measuring device 2 sends to the central processing unit, and an abnormal bright point appears on the diamond growth surface.
It has been found that, surprisingly, during the synthesis of diamond, part of the diamond surface may have abnormal bright spots with higher brightness than other parts of the diamond, which may eventually form defects in the diamond, such as carbon black, during the subsequent synthesis process. There is no report on the bright spot in the prior art, and there is no processing method and process for the bright spot. According to the invention, etching gas is introduced in the synthesis process, and the defects on the diamond are removed in an etching mode, so that the high-quality diamond without or with fewer defects is synthesized for a long time.
Specifically, when a protrusion (polycrystalline growth) appears at the edge or the center of the surface of the diamond during the growth process, the temperature is sharply increased due to the point discharge effect, which is reflected by the fact that the color becomes bright.
It should be noted that the plasma itself has a high power density and electric field strength, and when a tip occurs, a strong point of the electric field, i.e. a tip discharge effect, is easily formed at this position, and the energy is converted into heat energy, and the temperature is increased.
As a preferred embodiment, in the step S3, the concentration of the etching gas in the etching gas mixture is 4% to 8%.
As a preferred embodiment, in the step S4, one way of determining whether the etching is completed is that the abnormal bright point disappears, and when the abnormal bright point disappears, the etching is completed.
As a preferred embodiment, in step S4, another way to determine whether the etching is completed is that the etching is completed when the etching reaches a predetermined time. If the preset time is too short, the defect of the abnormal bright point can not be completely etched, the inside of the diamond still has defects, and if the etching time is too long, the formed diamond layer can be etched after the bright point etching is finished, so that the production efficiency is reduced. The skilled person finds, through research, that the etching time is preferably 5-120min, and more preferably 10-30 min.
In a preferred embodiment, the carbon source gas mixture is a mixture of methane and hydrogen.
In a preferred embodiment, the etching gas mixture is a mixture of oxygen and hydrogen.
In the stage of starting the growth of the diamond, the carbon source gas mixture is conveyed into a diamond reaction chamber 1, in the growth process, an optical camera measuring device 2 outputs a picture to a central processing unit in real time, the central processing unit judges whether an abnormal bright spot appears or not according to the picture, as long as the abnormal bright spot appears, the control device controls the carbon source gas mixture to stop conveying, under the condition that the growth environment of the diamond is not changed, the etching gas mixture is introduced, meanwhile, the optical camera measuring device 2 still outputs the picture to the central processing unit in real time, when the central processing unit recognizes that the abnormal bright spot disappears, the introduction of the etching gas is stopped, the carbon source gas mixture is continuously introduced, the diamond continues to grow, and the growth quality and the yield of the diamond are ensured.
The foregoing is a detailed description of the invention, and specific examples are used herein to explain the principles and implementations of the invention, the above description being merely intended to facilitate an understanding of the principles and core concepts of the invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (10)

1. An on-line diamond growth detection device is characterized by comprising
The reaction chamber comprises a closed area suitable for containing diamond growth, and the outer side wall of the reaction chamber is provided with at least one observation window;
an optical camera measuring device including a measuring device body and an optical camera, the optical camera measuring device being installed at a position where a sample inside the reaction chamber can be observed through the observation window;
the gas storage and conveying system is connected with the vent holes in the reaction chamber through a gas conveying gas path, so that reaction gas or etching gas can enter the reaction chamber, and the gas storage and conveying system comprises a carbon source storage system and an etching gas storage system;
a control device comprising a central processing unit;
one mounting mode of the optical camera measuring device is that the optical camera measuring device is directly fixed outside the observation window; the other installation mode of the optical camera measuring device is that the optical camera measuring device is installed outside the reaction chamber through a fixing part, so that the optical camera can monitor the condition of a sample in the reaction chamber through an observation window;
the optical camera and the gas storage and delivery system are respectively and electrically connected with the central processing unit.
2. An on-line diamond detection and growth device as claimed in claim 1, wherein the gas storage and delivery system further comprises a gas mixing device for mixing carbon source, etching gas and the like with inert gas, hydrogen gas and other necessary gases as required.
3. The diamond on-line detection growth device according to claim 1, wherein the optical camera measuring device is movably connected with a fixed part on the reaction chamber through a rotating shaft mechanism and can shoot the diamond in the reaction chamber through an observation window.
4. The diamond on-line detection growth device according to claim 3, wherein the rotating shaft mechanism comprises an upper support, a lower support and a damping rotating shaft, the upper support is connected with the outer wall of the reaction chamber through a hinged support, the lower support is arranged on the measuring device body, and the damping rotating shaft is inserted between the upper support and the lower support.
5. A diamond on-line detection growth device as claimed in claim 1, wherein the optical camera is a high fidelity camera, and the included angle between the shooting angle of the optical camera and the surface of the seed crystal is adjusted to be 50-70 degrees through the rotating shaft mechanism.
6. An on-line diamond growth apparatus as claimed in claim 2, wherein the carbon source is selected from one or more of methane, ethane, propane, butane, ethylene and acetylene.
7. The diamond on-line detection growth device according to claim 6, wherein the carbon source is methane.
8. An on-line diamond growth apparatus as claimed in claim 2, wherein said etching gas is oxygen.
9. A diamond growth defect treatment method for the online detection and growth device for the diamond according to any one of claims 1 to 8, which is characterized by comprising the following steps:
s1, sending a diamond growth picture to a central processing unit by the optical camera measuring device, and judging that growth defects appear by the central processing unit;
s2, the control device controls the gas storage and delivery system to stop the carbon source gas mixture from entering the reaction chamber;
s3, the control device controls the gas storage and delivery system to access the etching gas mixture to the reaction chamber;
s4, the optical camera measuring device transmits the etching picture to the central processing unit in real time, whether etching is finished is judged, and if yes, the step S5 is executed; if not, go to step S3;
and S5, stopping introducing the etching gas mixture, opening the carbon source gas mixture, and continuing to grow the diamond.
10. The diamond growth defect treatment method according to claim 9, wherein in the step S3, the concentration of the etching gas in the etching gas mixture is 4% -8%.
CN201911213947.XA 2019-12-02 2019-12-02 Diamond on-line detection growth device and growth defect treatment method Pending CN110760816A (en)

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US20230349835A1 (en) * 2020-05-22 2023-11-02 Fraunhofer Usa, Inc. Systems and methods for synthesizing a diamond using machine learning
CN117516633A (en) * 2024-01-03 2024-02-06 承德晶浪材料科技有限责任公司 Remote monitoring method, device, equipment and medium suitable for diamond production

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