CN210922513U - Monitoring device in growth process of single crystal diamond - Google Patents
Monitoring device in growth process of single crystal diamond Download PDFInfo
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- CN210922513U CN210922513U CN201922288087.8U CN201922288087U CN210922513U CN 210922513 U CN210922513 U CN 210922513U CN 201922288087 U CN201922288087 U CN 201922288087U CN 210922513 U CN210922513 U CN 210922513U
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Abstract
The utility model provides a monitoring device in the growth process of single crystal diamond, which comprises a chemical vapor deposition device, a thickness monitoring device and a mobile platform; the chemical vapor deposition equipment is provided with a deposition chamber, a deposition platform and a visible window; the visible window is used for monitoring the diamond placed on the deposition platform, and the deposition platform is arranged in the deposition chamber; the thickness monitoring device comprises a thickness monitoring component and an objective lens, wherein the objective lens is used for monitoring the diamond placed on the deposition platform through a visible window; the thickness monitoring part is connected with the objective lens and the mobile platform and used for obtaining thickness and position data corresponding to each detection position on the surface of the single crystal diamond, and the objective lens is arranged on the mobile platform and faces the chemical vapor deposition equipment. The monitoring device can monitor the thickness of the single crystal diamond in real time through the mobile platform and the thickness monitoring equipment, once obvious change can be observed on the height of a local part, whether production is interrupted or not is further determined, and losses of water, electricity, gas, manpower and the like are reduced.
Description
Technical Field
The utility model relates to a single crystal diamond technical field especially relates to a monitoring devices in single crystal diamond growth process.
Background
When the carat-grade single crystal diamond is grown by adopting microwave Plasma chemical vapor deposition equipment, namely MPCVD (microwave Plasma chemical vapor deposition), the seed crystal needs to grow for a long time of about 10-15 days after being placed in the CVD equipment, and the problems of polycrystalline growth, black carbon inclusion and internal stress are easily caused at a certain time node due to the influence of various conditions such as technical process level, seed crystal quality, external environmental factors and the like in the growth process, so that the product yield is influenced, and the cost is increased. However, when the diamond is at a high temperature of about 1000 ℃, the existing observation means (mainly visual observation) cannot observe whether the polycrystal is generated, that is, once the initial growth quality is not good, the cost in all aspects of water, electricity, gas, manpower and the like is wasted in the next time.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a monitoring devices in single crystal diamond growth process to can't observe in real time among the solution prior art whether have the polycrystal or the formation such as inclusion, can't monitor single crystal diamond growth, thereby cause the extravagant problem of cost because of technology or other factors.
In order to achieve the above and other related objects, the present invention provides a monitoring device for single crystal diamond growth process, comprising a chemical vapor deposition device, a thickness monitoring device and a mobile platform;
the chemical vapor deposition equipment is provided with a deposition chamber, a deposition platform and a visible window; the visible window is used for monitoring the diamond placed on the deposition platform, and the deposition platform is arranged in the deposition chamber;
the thickness monitoring device comprises a thickness monitoring component and an objective lens, wherein the objective lens is used for monitoring the diamond placed on the deposition platform through the visual window; the thickness monitoring part is connected with the objective lens and the moving platform and used for obtaining thickness and position data corresponding to each detection position on the surface of the single crystal diamond, and the objective lens is arranged on the moving platform and faces the chemical vapor deposition equipment.
Preferably, the chemical vapor deposition apparatus is a microwave plasma chemical vapor deposition apparatus.
Preferably, the moving platform is an XY moving platform.
Preferably, the thickness monitoring part comprises a thickness monitoring unit and a controller, the thickness monitoring unit is connected with the objective lens and used for obtaining thickness calculation source data of each detection position on the surface of the single crystal diamond, and the controller is in communication connection with the mobile platform and the thickness monitoring unit.
More preferably, the thickness monitoring unit is a michelson interferometer.
More preferably, the controller includes:
the mobile control unit is connected with the mobile platform and is used for controlling the mobile platform to move and providing position data of each detection position on the surface of the single crystal diamond;
the thickness calculating unit is used for obtaining single crystal diamond thickness calculating source data of each detection position on the surface of the single crystal diamond from the thickness monitoring unit and calculating to obtain single crystal diamond thickness data of each detection position on the surface of the single crystal diamond;
and the information unit is used for matching and providing the thickness data of the single crystal diamond at each detection position of the surface of the single crystal diamond obtained from the thickness calculation unit and the position data of each detection position of the surface of the single crystal diamond obtained from the mobile control platform.
More preferably, the thickness monitoring unit is a michelson interferometer.
More preferably, the thickness monitoring part further comprises a thickness calculation unit for obtaining thickness calculation source data from the thickness monitoring unit and calculating to obtain the thickness of the single crystal diamond.
Further more preferably, the thickness monitoring part further comprises a control unit for controlling the movement of the moving platform, and the control unit is connected with the moving platform.
Still further more preferably, the control unit is connected to the thickness calculation unit for obtaining the single crystal diamond position from the control unit.
Still further more preferably, the thickness monitoring section further includes a three-dimensional topography simulation unit for obtaining a position of the single crystal diamond from the control unit, obtaining a thickness of the single crystal diamond from the thickness calculation unit, and performing three-dimensional simulation of the position and the thickness of the single crystal diamond to obtain a three-dimensional topography of the single crystal diamond.
Further more preferably, the controller further comprises a termination signal judging and sending module for determining whether to terminate the growth of the single crystal diamond according to the thickness and position data of each detected position on the surface of the single crystal diamond provided by the information unit and sending a termination signal.
Further more preferably, the information unit is further configured to perform three-dimensional simulation on the position data of each detected position on the surface of the single crystal diamond and the thickness data of the single crystal diamond at each detected position on the surface of the single crystal diamond, so as to obtain the three-dimensional morphology of the single crystal diamond.
The technical scheme has the following beneficial effects:
the utility model provides a monitoring devices among single crystal diamond growth process, for example michelson interferometer through moving platform and thickness monitoring equipment, can real-time supervision single crystal diamond thickness, except that marginal minority area, each regional growth rate of ideal single crystal diamond should keep unanimous, in case some regional growth rate of part is higher than or is less than whole speed, then it has the polycrystal to represent, defect such as inclusion generates, then can observe obvious change in height, and then can decide whether to interrupt production, reduce water, electricity, gas, the loss of each side such as manual work.
Drawings
Fig. 1 is a schematic structural diagram of a monitoring device in a single crystal diamond growth process according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a thickness monitoring component in a monitoring device in the growth process of single crystal diamond according to an embodiment of the present invention.
Fig. 3 is a schematic view of a single crystal diamond surface covered by a predetermined proportion of the surface of a single crystal diamond seed.
Reference numerals
1 chemical vapor deposition apparatus
11 deposition chamber
12 deposition platform
13 visual window
2 thickness monitoring device
21 thickness monitoring part
211 thickness monitoring unit
212 controller
2121 movement control unit
2122 thickness calculating unit
2123 information element
2124 termination signal determining and sending module
22 objective lens
3 moving platform
Detailed Description
In the description of the present invention, it should be noted that the structure, ratio, size, etc. shown in the attached drawings of the present specification are only used for matching with the content disclosed in the specification, so as to be known and read by the people familiar with the technology, and are not used for limiting the limit conditions that the present invention can be implemented, so that the present invention does not have the substantial technical significance, and the modification of any structure, the change of the ratio relationship or the adjustment of the size should still fall within the range that the technical content disclosed in the present invention can cover without affecting the function that the present invention can produce and the purpose that can be achieved. While the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like refer to orientations or positional relationships illustrated in the drawings, which are used for convenience in describing the invention and to simplify the description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
As shown in fig. 1, an embodiment of the present invention provides a monitoring device in a single crystal diamond growth process, including a chemical vapor deposition apparatus 1, a thickness monitoring apparatus 2, and a mobile platform 3;
the chemical vapor deposition equipment 1 is provided with a deposition chamber 11, a deposition platform 12 and a visible window 13; the visible window 13 is used for monitoring the diamond placed on the deposition platform 12, and the deposition platform 12 is arranged in the deposition chamber 11;
the thickness monitoring device 2 comprises a thickness monitoring part 21 and an objective lens 22, wherein the objective lens 22 is used for monitoring the diamond placed on the deposition platform 12 through the visual window 13; the thickness monitoring part 21 is connected with the objective lens 22 and the moving platform 3 and is used for obtaining thickness and position data corresponding to each detection position on the surface of the single crystal diamond, and the objective lens 22 is arranged on the moving platform 3 and faces the chemical vapor deposition equipment 1.
The monitoring device can monitor the thickness of the single crystal diamond in real time through a mobile platform and a thickness monitoring device such as a Michelson interferometer, once obvious change can be observed on the height of a local part, and then whether production is interrupted or not is determined, and losses of water, electricity, gas, manpower and the like are reduced.
The chemical vapor deposition equipment 1 is microwave plasma chemical vapor deposition equipment. Placing the single crystal diamond seed crystal in the deposition chamber 11 of the chemical vapor deposition device 1, exciting and decomposing the mixture of carbon-containing gas (such as methane) and hydrogen under the conditions of high temperature, pressure lower than standard atmospheric pressure and microwave to form plasma state carbon atoms, and depositing and alternately growing the single crystal diamond on the single crystal diamond seed crystal.
The mobile control platform 3 is an XY mobile platform. For example: and the Sims CSK precision positioning platform LMA series drives the objective lens 22 arranged on the mobile platform 3 to move.
In a preferred embodiment, the thickness monitoring unit 21 includes a thickness monitoring unit 211 and a controller 212, the thickness monitoring unit 211 is connected to the objective lens 22 for obtaining data of thickness calculation sources at each detection position of the surface of the single crystal diamond, and the controller 212 is connected to the moving platform 3 and the thickness monitoring unit 211 in a communication manner. The thickness monitoring unit 211 may be connected to the objective lens 22 through an optical fiber, and the thickness monitoring unit 211 emits an optical signal to the single crystal diamond through the objective lens 22 and transmits a feedback optical signal back to the thickness monitoring unit 211.
In a preferred embodiment, the thickness monitoring unit 211 is a michelson interferometer. The wavelength of the thickness monitoring unit 211 avoids the emission wavelength of the plasma, and the wavelength is more than or equal to 985 nm. The wavelength difference is preferably within. + -. 15nm (laser with good monochromaticity), for example, the wavelength is 1000nm, and the actual emission wavelength is within 985nm to 1015 nm.
In a preferred embodiment, as shown in fig. 2, the controller 212 includes:
the movement control unit 2121 is connected with the moving platform 3 and is used for controlling the movement of the moving platform 3 and providing position data of each detection position on the surface of the single crystal diamond;
the thickness calculating unit 2122 is used for obtaining single crystal diamond thickness calculation source data of each detection position on the surface of the single crystal diamond from the thickness monitoring unit 211 and calculating to obtain single crystal diamond thickness data of each detection position on the surface of the single crystal diamond;
and an information unit 2123 for matching and providing the thickness data of the single crystal diamond at each detected position on the surface of the single crystal diamond obtained from the thickness calculation unit 212 and the position data of each detected position on the surface of the single crystal diamond obtained from the mobile control platform 3.
The thickness calculating unit calculates the thickness according to the following calculation formula:
wherein, VM2The physical moving speed of a reflecting moving mirror in the Michelson interferometer;
n0is the refractive index of the single crystal diamond at normal temperature;
dn/dT: the coefficient of variation of the refractive index of the single crystal diamond with temperature;
△ T, the temperature difference between the temperature of the single crystal diamond and the room temperature;
t2: testing the time to reach the bottom interference fringe of the single crystal diamond by a Michelson interferometer;
t1: the michelson interferometer measures the time to reach the top interference fringe of the single crystal diamond.
In a preferred embodiment, as shown in fig. 2, the controller 212 further comprises a termination signal determining and sending module 2124 for determining whether to terminate the growth of the single crystal diamond according to the thickness and position data of each detected position of the surface of the single crystal diamond provided by the information unit 2123 and sending a termination signal.
When the monitored object is a single-crystal diamond, the growth of the single-crystal diamond is stopped when any one of the following conditions is met:
a1) when the thickness of the single crystal diamond is less than 1mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 50 mu m, and the growth of the single crystal diamond is stopped;
a2) when the thickness of the single crystal diamond is more than or equal to 1mm and less than 2mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 100 mu m, and the growth of the single crystal diamond is stopped;
a3) when the thickness of the single crystal diamond is less than or equal to 2mm and less than or equal to 3mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 150 mu m, and the growth of the single crystal diamond is stopped;
a4) when the thickness of the single crystal diamond is more than 3mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 200 mu m, and the growth of the single crystal diamond is stopped.
The predetermined ratio from the center point of the surface of the single crystal diamond refers to the surface of the single crystal diamond covered by the surface of the single crystal diamond seed in a predetermined ratio having a center on the center axis of the surface of the single crystal diamond seed that passes through the center of the surface of the single crystal diamond covered by the predetermined ratio and is perpendicular to the surface of the single crystal diamond seed. The predetermined ratio may be empirically determined, for example, to be 70% from the center point of the surface of the single crystal diamond and the surface of the single crystal diamond seed is, for example, 8mm by 8mm square, such that the center of the surface of the single crystal diamond seed 70% covered by the surface of the single crystal diamond seed is on the center axis of the surface of the single crystal diamond seed and 5.6mm by 5.6mm square covered by the surface of the single crystal diamond seed, see the shaded portion in fig. 3.
In a preferred embodiment, when the object to be monitored is a plurality of single crystal diamonds, the single crystal diamond growth is terminated when the following conditions are satisfied: and stopping the growth of the single crystal diamond when the yield is lower than a preset proportion, wherein the yield is the number of the single crystal diamond grains/the total number of the single crystal diamond grains which do not accord with the growth condition of the single crystal diamond, and the single crystal diamond growth condition is judged to be not accord with when any one of the following conditions is met:
a1) when the thickness of the single crystal diamond is less than 1mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 50 mu m, and the growth of the single crystal diamond is stopped;
a2) when the thickness of the single crystal diamond is more than or equal to 1mm and less than 2mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 100 mu m, and the growth of the single crystal diamond is stopped;
a3) when the thickness of the single crystal diamond is less than or equal to 2mm and less than or equal to 3mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 150 mu m, and the growth of the single crystal diamond is stopped;
a4) when the thickness of the single crystal diamond is more than 3mm, the thickness difference between the highest point and the lowest point of the surface of the single crystal diamond with a preset proportion from the central point of the surface of the single crystal diamond is more than 200 mu m, and the growth of the single crystal diamond is stopped.
The predetermined proportion of yield below which can be empirically determined may be, for example, 50%.
In a preferred embodiment, as shown in fig. 2, the information unit 2123 is further configured to perform three-dimensional simulation on the position data of each detected position on the surface of the single crystal diamond and the thickness data of the single crystal diamond at each detected position on the surface of the single crystal diamond to obtain the three-dimensional topography of the single crystal diamond.
When in use, a single crystal diamond seed crystal is placed in a deposition chamber 11 of a chemical vapor deposition device 1, a mixture of carbon-containing gas (such as methane) and hydrogen is excited and decomposed at high temperature and under the pressure lower than the standard atmospheric pressure and under microwaves to form plasma carbon atoms, the plasma carbon atoms are deposited and alternately grown into the single crystal diamond on the single crystal diamond seed crystal, an objective lens 22 in a thickness monitoring device 2 can move through a moving platform 3 in the growth process, when the objective lens 22 is at a certain position, the single crystal diamond placed on a deposition platform 12 is monitored through a visible window 13, the objective lens 22 and a thickness monitoring part 21 can be connected through an optical fiber, single crystal diamond thickness calculation source data at each detection position on the surface of the single crystal diamond is obtained from a thickness monitoring unit 211, single crystal diamond thickness data at each detection position on the surface of the single crystal diamond is obtained through calculation, the size data of the single crystal diamond can, images may also be formed. The thickness and position data corresponding to each detection position on the surface of the single crystal diamond can be obtained through continuous and uninterrupted test in the growth process, and the information such as the growth rate, the surface growth state and the like of the single crystal diamond can be obtained through processing. The thickness of the single crystal diamond is monitored in real time, the growth rate of each region of the ideal single crystal diamond is kept consistent except for a few regions at the edge, once the growth rate of some local regions is higher or lower than the overall rate, the defects such as polycrystals, inclusions and the like are generated, obvious change can be observed in the height, further, whether production is interrupted or not can be determined, and loss of water, electricity, gas, manpower and the like is reduced.
The above embodiments are merely illustrative of the principles and effects of the present invention, and are not to be construed as limiting the invention. Modifications and variations can be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A monitoring device in the growth process of single crystal diamond is characterized by comprising chemical vapor deposition equipment (1), thickness monitoring equipment (2) and a moving platform (3);
the chemical vapor deposition equipment (1) is provided with a deposition chamber (11), a deposition platform (12) and a visible window (13); the visual window (13) is used for monitoring the diamond placed on the deposition platform (12), and the deposition platform (12) is arranged in the deposition chamber (11);
the thickness monitoring device (2) comprises a thickness monitoring part (21) and an objective lens (22), wherein the objective lens (22) is used for monitoring the diamond placed on the deposition platform (12) through the visual window (13); the thickness monitoring part (21) is connected with the objective lens (22) and the moving platform (3) and used for obtaining thickness and position data corresponding to each detection position on the surface of the single crystal diamond, and the objective lens (22) is arranged on the moving platform (3) and faces the chemical vapor deposition equipment (1).
2. A device for monitoring the growth of single crystal diamonds according to claim 1 wherein said chemical vapor deposition apparatus (1) is a microwave plasma chemical vapor deposition apparatus.
3. A device for monitoring the growth of a single crystal diamond according to claim 1, wherein the moving platform (3) is an XY moving platform.
4. A device for monitoring the growth of a single crystal diamond according to any one of claims 1 to 3, wherein the thickness monitoring unit (21) comprises a thickness monitoring unit (211) and a controller (212), the thickness monitoring unit (211) is connected with the objective lens (22) and is used for obtaining data from thickness calculation sources at each detection position of the surface of the single crystal diamond, and the controller (212) is in communication connection with the moving platform (3) and the thickness monitoring unit (211).
5. A device for monitoring the growth of a single crystal diamond according to claim 4, wherein said thickness monitoring unit (211) is a Michelson interferometer.
6. A device for monitoring the growth of single crystal diamond as in claim 4, wherein said controller (212) comprises:
the movement control unit (2121) is connected with the moving platform (3) and is used for controlling the movement of the moving platform (3) and providing position data of each detection position on the surface of the single crystal diamond;
the thickness calculating unit (2122) is used for obtaining single crystal diamond thickness calculating source data of each detection position on the surface of the single crystal diamond from the thickness monitoring unit (211) and calculating to obtain single crystal diamond thickness data of each detection position on the surface of the single crystal diamond;
and an information unit (2123) for matching and providing the thickness data of the single crystal diamond at each inspection site on the surface of the single crystal diamond obtained from the thickness calculation unit (2122) and the position data of each inspection site on the surface of the single crystal diamond obtained from the moving stage (3).
7. A device for monitoring the growth of single crystal diamond according to claim 6, wherein said controller (212) further comprises a termination signal judging and transmitting module (2124) for determining whether to terminate the growth of single crystal diamond according to the thickness and position data of each detected position of the surface of single crystal diamond provided by said information unit (2123) and transmitting a termination signal.
8. A device for monitoring the growth process of single crystal diamond according to claim 6, wherein the information unit (2123) is further configured to perform three-dimensional simulation of the position data of each detected position on the surface of the single crystal diamond and the thickness data of the single crystal diamond at each detected position on the surface of the single crystal diamond to obtain the three-dimensional appearance of the single crystal diamond.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112197728A (en) * | 2020-09-16 | 2021-01-08 | 北京清碳科技有限公司 | Monitoring device in growth process of single crystal diamond |
| CN116883394A (en) * | 2023-09-06 | 2023-10-13 | 山东融泽新材料有限公司 | Diamond quality detection method based on image data processing |
| 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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2019
- 2019-12-17 CN CN201922288087.8U patent/CN210922513U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112197728A (en) * | 2020-09-16 | 2021-01-08 | 北京清碳科技有限公司 | Monitoring device in growth process of single crystal diamond |
| CN116883394A (en) * | 2023-09-06 | 2023-10-13 | 山东融泽新材料有限公司 | Diamond quality detection method based on image data processing |
| CN116883394B (en) * | 2023-09-06 | 2023-11-17 | 山东融泽新材料有限公司 | Diamond quality detection method based on image data processing |
| 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 |
| CN117516633B (en) * | 2024-01-03 | 2024-03-19 | 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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Denomination of utility model: A monitoring device for the growth process of single crystal diamond Effective date of registration: 20230807 Granted publication date: 20200703 Pledgee: Agricultural Bank of China Limited Shanghai Songjiang Sub-branch Pledgor: CR GEMS SUPERABRASIVES CO.,LTD. Registration number: Y2023980051176 |