CN108554334B - MPCVD synthesis equipment and synthesis temperature control method - Google Patents
MPCVD synthesis equipment and synthesis temperature control method Download PDFInfo
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- CN108554334B CN108554334B CN201810360787.0A CN201810360787A CN108554334B CN 108554334 B CN108554334 B CN 108554334B CN 201810360787 A CN201810360787 A CN 201810360787A CN 108554334 B CN108554334 B CN 108554334B
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B01J19/0033—Optimalisation processes, i.e. processes with adaptive control systems
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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Abstract
The invention relates to an MPCVD synthesis device and a synthesis temperature control method, wherein the synthesis device comprises a reaction cavity, a microwave output device for outputting electromagnetic waves to the reaction cavity, an air pressure control device for controlling the gas pressure in the reaction cavity and a temperature measurement device for measuring the surface temperature of a compound in the reaction cavity; the microwave control system further comprises a control center, and the microwave output device, the air pressure control device and the temperature measuring device are all in communication connection with the control center. The synthesis equipment can automatically adjust the power and the gas pressure of the reaction cavity when the temperature deviates, so that the power and the pressure are automatically matched, and the temperature is recovered to be within a specific interval range; in the process of synthesizing a single composition, the synthesis temperature of the composition can be effectively controlled, and the quality of a final product is improved; in the process of synthesizing a plurality of compositions, when a certain temperature deviates, the temperature can be fed back to the machine end for warning, corresponding adjustment can be made in time, and the synthesis quality and the yield of the compositions in the same batch can be improved.
Description
Technical Field
The invention relates to MPCVD synthesis equipment and a synthesis temperature control method, which are particularly suitable for synthesizing diamond.
Background
The MPCVD process can be used not only for the synthesis of diamond, but also for the preparation of many other materials. Diamond attracts attention because of its extremely excellent physicochemical properties. However, natural diamond reserves are limited, and thus various synthetic diamond methods such as a high temperature high pressure method (HPHT), a hot wire chemical vapor deposition method (HJCVD) have been developed. Wherein, the method for synthesizing diamond by Microwave plasma chemical vapor deposition (Microwave plasma chemical vapor deposition) can synthesize diamond with high quality and large area because no impurities are introduced.
The quality of diamond synthesized by MPCVD is related to many factors, including carbon source concentration, gas flow, temperature, substrate table height, microwave power, synthesis temperature. The synthesis temperature has a great relationship with the quality of the synthesized diamond, so that the automatic monitoring of the temperature of the diamond in the synthesis process is very critical.
The flow chart of the Microwave plasma chemical vapor deposition (Microwave plasma chemical vapor deposition) method for synthesizing diamond is shown in figure 1. Generally, an MPCVD synthesis apparatus for synthesizing diamond includes a microwave output device, a chamber structure for performing a chemical deposition reaction, and a temperature measuring device for monitoring a surface temperature of diamond in the chamber structure.
The conventional thermometric technique for synthesizing diamond by MPCVD is mainly shown in FIG. 2. The method can only provide real-time temperature measurement for one diamond seed crystal, generally takes a non-contact infrared thermometer as a temperature measuring device, adjusts the laser point position to a position to be measured through an observation window on a cavity structure, and monitors after fixation.
The existing temperature measurement technology has the following defects:
1) in the process of synthesizing the diamond, the non-contact temperature measuring device only obtains the temperature measuring result of a certain point, and the temperature distribution in a larger area cannot be known;
2) in the process of synthesizing a single diamond, although the non-contact temperature measuring device can obtain the temperature measuring result of a certain point, the non-contact temperature measuring device cannot feed back power and pressure in real time, so that the equipment does not have any feedback measure after the temperature rises in the synthesizing process, the temperature stability cannot be ensured, and the quality of the synthesized diamond is reduced.
3) In the process of simultaneously synthesizing a plurality of diamonds, the temperature of other diamonds cannot be measured simultaneously, namely the temperature uniformity of the diamonds is determined in real time, but in an actual synthesis experiment, the temperature of the diamonds is not uniform due to various reasons. The temperature uniformity of a plurality of diamonds cannot be determined, so that the synthesis quality, stability and yield of diamonds in the same batch are greatly influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides MPCVD synthesis equipment and a synthesis temperature control method, which aim to solve the problem that the surface temperature of diamond is difficult to keep stable in the MPCVD synthesis process.
In order to solve the technical problems, the technical scheme of the invention is as follows: an MPCVD synthesis device comprises a reaction cavity, a microwave output device used for outputting electromagnetic waves to the reaction cavity, a gas pressure control device used for controlling the gas pressure in the reaction cavity and a temperature measuring device used for measuring the surface temperature of a compound in the reaction cavity; the microwave control system further comprises a control center, and the microwave output device, the air pressure control device and the temperature measuring device are all in communication connection with the control center.
Further, the microwave transmission system is used for guiding the microwaves from the microwave output device to the reaction cavity. Alternative microwave transmission systems typically include components such as waveguides, circulators, water loads, screw impedance adjusters, shorting pistons, microwave switching antennas, and the like.
Further, the control center comprises one of a computer, a single chip microcomputer and a PLC, and further can be other devices with data processing functions.
By adopting the structural design, in the synthesis process, when the temperature is detected to deviate from the preset temperature interval by the temperature measuring device, the control center automatically adjusts the microwave output power of the equipment and/or the gas pressure of the reaction cavity, so that the temperature returns to the preset temperature interval, the stability of the surface temperature of the compound (such as diamond) in the synthesis process is ensured, and the quality of the compound is obviously improved.
Further, a method for optionally adjusting microwave output power and/or gas pressure of a reaction cavity comprises the steps that when the temperature is higher than a preset temperature range, a control center firstly sends a power adjusting instruction to a microwave generating device to reduce the output power, then sends a gas pressure adjusting instruction to a gas pressure control device to reduce the gas pressure of the reaction cavity until the surface temperature of a target product falls into the preset temperature range. When the temperature is lower than the preset temperature range, the control center firstly sends a power adjusting instruction to the air pressure adjusting device to increase the air pressure, and then sends an air pressure adjusting instruction to the microwave generating device to increase the air pressure until the surface temperature of the target product falls into the preset temperature range.
Further, the power adjustment instruction corresponds to the air pressure adjustment instruction, and the specific power adjustment range and the corresponding air pressure adjustment range can be set according to different reactions. Optionally, the microwave output power is reduced by 4-100W, and the air pressure is reduced by 0-5 mbar; the air pressure is increased by 0.5-5mbar, and the power is increased by 4-100W.
The reaction chamber is internally provided with a base platform, the temperature measuring device is arranged on the side wall of the reaction chamber and is a non-contact temperature measuring device, and the temperature measuring area of the non-contact temperature measuring device comprises the top surface of the base platform. Optionally, the non-contact temperature measuring device is an infrared thermometer.
The side wall of the reaction cavity is provided with an observation window for visually observing the top surface of the base station, and the non-contact temperature measuring device is arranged on the observation window.
An image acquisition mechanism, preferably a CCD (Charge-coupled Device) or a camera, for acquiring image information of the top surface of the base and the surface of the composite is provided in the observation window.
The temperature measuring device is a single-point remote temperature measuring device or a multipoint remote temperature measuring device. The single-point remote temperature measuring device is a remote temperature measuring device which can only measure the temperature of a certain point or a certain area at a certain time; the multipoint remote temperature measuring device is a remote temperature measuring device capable of measuring the temperature of a plurality of points or a plurality of areas at a certain moment.
The temperature measuring device is a single-point remote temperature measuring device, and the single-point remote temperature measuring device can control a temperature measuring point to do circulating motion. Further, the cyclic motion may be a repetitive circular motion, or may be a linear or curvilinear reciprocating motion. Therefore, the temperature data of different parts of the surface of the compound in the reaction cavity or the surface of different compounds in the reaction cavity can be acquired, so that the temperature change conditions of different parts of the surface of the compound in the reaction cavity or different compounds in the reaction cavity in the synthesis process can be acquired, and data support can be provided for the research and improvement of the synthesis process of the compound and how to realize accurate temperature compensation.
Adopts a single-point remote temperature measuring device or a multi-point remote temperature measuring device with temperature measuring points capable of performing circulating motion, during the synthesis of a plurality of compositions (such as a plurality of diamonds), the surface temperature change of all the compositions can be monitored simultaneously, when the surface temperature of all the compositions exceeds the whole temperature or the surface temperature of some compositions exceeds the preset temperature interval, the control center can analyze the collected temperature data through the temperature measuring device, automatically adjust the microwave output power (correspondingly, sending a power adjusting instruction to the microwave output device) and/or the gas pressure of the reaction cavity (correspondingly, sending a gas pressure adjusting instruction to the gas pressure control device), return the temperature to a set temperature range, ensure the stability of the surface temperature of the composition in the synthesis process, and improve the synthesis quality and the yield of the composition of the same batch.
The display screen is in communication connection with the control center. The temperature change condition data can be visually displayed through the display screen, for example, when the temperature of different temperature measuring points in the reaction cavity is monitored, the temperature measuring device can transmit the collected temperature signals to the control center, and the control center analyzes and processes the temperature signals to obtain a temperature distribution condition diagram of the surface of the composition in the reaction cavity and output the temperature distribution condition diagram to the display screen, so that an operator can visually check the temperature change condition of each temperature measuring point in the synthesis process.
According to the method for controlling the synthesis temperature in the synthesis equipment, in the synthesis process, the temperature measuring device collects the surface temperature signal of the compound in the reaction cavity in real time and transmits the temperature signal to the control center, the control center analyzes and processes the temperature signal and compares the temperature signal with the preset temperature interval, and when the control center judges that the surface temperature of the compound is in the preset temperature interval, the synthesis equipment continues to operate normally; when the control center judges that the surface temperature of the composition deviates from the preset temperature interval, the control center sends a microwave power adjusting instruction to the microwave output device and/or sends a gas pressure adjusting instruction to the gas pressure control device, so that the surface temperature of the composition returns to the preset temperature interval.
Furthermore, in the control process of the synthesis temperature, the gas pressure and the microwave power can be adjusted simultaneously to be matched; when the surface temperature of the composition is detected to be overhigh (exceeding a preset temperature interval), the gas pressure and the microwave power are simultaneously reduced, and conversely, the gas pressure and the microwave power are simultaneously increased. Similarly, the microwave power or the gas pressure can be adjusted independently to control the synthesis temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the temperature measuring device continuously gives feedback to a control center when measuring the temperature, and automatically adjusts the power and the gas pressure of the reaction cavity when the temperature deviates, so that the power and the pressure are automatically matched, and the temperature is restored to be within a specific interval range;
2. the temperature measuring device can measure the temperature of a large area or a plurality of measuring points, and simultaneously provides a temperature distribution map in a temperature measuring area, thereby providing data support for the research and improvement of a synthetic process of a compound and how to realize accurate temperature compensation;
3. in the process of synthesizing a single composition, the synthesis temperature of the composition can be effectively controlled to be stabilized in a certain temperature range, so that the quality of a final product is improved;
4. in the process of synthesizing a plurality of compositions, when the integral temperature deviates from a preset temperature interval, the control center makes a judgment and automatically adjusts the microwave output power and the gas pressure in the reaction cavity, so that the temperature is restored to the preset temperature interval, and the product quality is effectively improved; when one temperature deviates, the temperature can be fed back to the machine end for warning prompt, corresponding adjustment can be made in time, and the synthesis quality and the yield of the same batch of compounds can be improved.
Drawings
FIG. 1 is a flow chart of a prior art chemical vapor deposition process for preparing diamond.
FIG. 2 is a schematic diagram of the temperature measurement of diamond synthesized by chemical vapor deposition.
FIG. 3 is a control schematic diagram of an MPCVD synthesis apparatus of the present invention.
FIG. 4 is a schematic diagram of the structure of the reaction chamber of an MPCVD synthesis apparatus of the present invention.
FIG. 5 is a flow chart of the synthesis temperature control of an MPCVD synthesis apparatus of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. For convenience of description, the words "upper", "lower", "left" and "right" in the following description are used only to indicate the correspondence between the upper, lower, left and right directions of the drawings themselves, and do not limit the structure.
As shown in fig. 3, an MPCVD synthesizing apparatus comprises a reaction chamber 1, a microwave output device 2 for outputting electromagnetic waves to the reaction chamber, a gas pressure control device 4 for controlling the gas pressure in the reaction chamber, and a temperature measuring device 3 for measuring the surface temperature of the composition in the reaction chamber; the microwave temperature measuring device is characterized by further comprising a control center 5 and a data acquisition device 7, the microwave output device 2, the air pressure control device 4 and the temperature measuring device 3 are all in communication connection with the data acquisition device 7, and the data acquisition device 7 is in communication connection with the control center 5.
As shown in fig. 4, a base 101 is disposed in the reaction chamber 1, an observation window 102 is disposed on a side wall of the reaction chamber, the observation window covering a top surface of the base in a visible range, the temperature measuring device 3 is disposed on the observation window, the temperature measuring device is a non-contact temperature measuring device, and a temperature measuring region of the non-contact temperature measuring device includes the top surface of the base.
And an image acquisition mechanism for acquiring image information of the top surface of the base and the surface of the compound is arranged in the observation window.
The temperature measuring device is a single-point remote temperature measuring device, and the single-point remote temperature measuring device can control a temperature measuring point to do circulating motion.
And a display screen 6 which is in communication connection with the control center.
As shown in fig. 5, in the synthesis of diamond, as an example, according to the method for controlling synthesis temperature in synthesis equipment, in the synthesis process, the temperature measuring device collects a temperature signal of the surface of the diamond in the reaction chamber in real time and transmits the temperature signal to the control center, the control center analyzes and processes the temperature signal and compares the temperature signal with a preset temperature interval, and when the control center judges that the surface temperature of the diamond is within the preset temperature interval, the synthesis equipment continues to operate as usual; when the control center judges that the surface temperature of the diamond deviates from the preset temperature range, the control center sends a microwave power adjusting instruction to the microwave output device and sends a gas pressure adjusting instruction to the gas pressure control device, so that the gas pressure and the power are automatically matched, and the surface temperature of the diamond returns to the preset temperature range.
When a plurality of diamonds are synthesized simultaneously, the temperature measuring points can be controlled to do circulating motion so as to collect temperature data of different diamond surfaces, the monitoring of the surface temperature of each diamond is realized, when the control center finds that the surface temperature of a certain diamond deviates, the control center sends an alarm prompt through the display screen and sends a related adjusting instruction to the microwave output device and/or the air pressure control device, the temperature of the surface of the diamond is recovered to a preset temperature interval, the uniformity of the surface temperature of each diamond is ensured, and the synthesis quality and the yield of the diamonds in the same batch are improved.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (3)
1. A control method of synthesis temperature in MPCVD synthesis equipment is used for simultaneously synthesizing a plurality of diamonds and is characterized in that the MPCVD synthesis equipment comprises a reaction cavity, a microwave output device used for outputting electromagnetic waves to the reaction cavity, an air pressure control device used for controlling the gas pressure in the reaction cavity, a temperature measurement device used for measuring the surface temperature of the diamonds in the reaction cavity, a control center and a display screen in communication connection with the control center, wherein the microwave output device, the air pressure control device and the temperature measurement device are all in communication connection with the control center; a base station is arranged in the reaction cavity, the temperature measuring device is arranged on the side wall of the reaction cavity, the temperature measuring device is a non-contact temperature measuring device, and the temperature measuring area of the non-contact temperature measuring device comprises the top surface of the base station; the temperature measuring device is a single-point remote temperature measuring device, and the single-point remote temperature measuring device can control temperature measuring points to do circulating motion, collect temperature data of different diamond surfaces and realize monitoring of the surface temperature of each diamond;
in the synthesis process, the temperature measuring device collects surface temperature signals of different diamonds in the reaction cavity in real time and transmits the temperature signals to the control center, the control center analyzes and processes the temperature signals and compares the temperature signals with a preset temperature interval, and when the control center judges that the surface temperature of the diamonds is within the preset temperature interval, the synthesis equipment continues to operate normally; when the control center judges that the surface temperature of the diamond deviates from the preset temperature interval, the control center sends a microwave power adjusting instruction to the microwave output device and sends a gas pressure adjusting instruction to the gas pressure control device, so that the surface temperature of the diamond returns to the preset temperature interval; when the temperature is higher than a preset temperature interval, the control center firstly sends a microwave power adjusting instruction to the microwave generating device to reduce the output power, and then sends a gas pressure adjusting instruction to the gas pressure control device to reduce the gas pressure of the reaction cavity until the surface temperature of the target product falls into the preset temperature interval; when the temperature is lower than the preset temperature interval, the control center firstly sends a gas pressure regulating instruction to the gas pressure regulating device to increase the gas pressure, and then sends a microwave power regulating instruction to the microwave generating device to increase the output power until the surface temperature of the target product falls into the preset temperature interval; the microwave output power is reduced by 4-100W, and the air pressure is reduced by 0-5 mbar; the air pressure is increased by 0.5-5mbar, and the power is increased by 4-100 w;
the temperature measuring points of the temperature measuring device are controlled to do circulating motion, temperature data of different diamond surfaces are collected, monitoring of the surface temperature of each diamond is achieved, when the control center finds that the surface temperature of a certain diamond deviates, the control center sends out an alarm prompt through a display screen, and sends out related adjusting instructions to the microwave output device and the air pressure control device, so that the surface temperature of the diamond returns to a preset temperature interval.
2. The control method according to claim 1, wherein an observation window for visually observing the top surface of the base is provided on the sidewall of the reaction chamber, and the non-contact temperature measuring device is provided on the observation window.
3. The control method according to claim 2, wherein an image obtaining mechanism for obtaining image information of the top surface of the base and the surface of the diamond is provided in the observation window.
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| CN109666924A (en) * | 2018-12-20 | 2019-04-23 | 长沙新材料产业研究院有限公司 | A kind of circulator protection system and control method |
| CN110760816A (en) * | 2019-12-02 | 2020-02-07 | 长沙新材料产业研究院有限公司 | Diamond on-line detection growth device and growth defect treatment method |
| CN110917998A (en) * | 2019-12-02 | 2020-03-27 | 长沙新材料产业研究院有限公司 | Diamond growth on-line monitoring method and diamond synthesis equipment |
| CN112684829A (en) * | 2020-12-22 | 2021-04-20 | 同济大学 | Temperature detection control system and method for MPCVD device |
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Address after: 410205 7th floor, building B8, Lugu Enterprise Square, Yuelu District, Changsha City, Hunan Province Patentee after: Aerospace Science and Industry (Changsha) New Materials Research Institute Co.,Ltd. Address before: 410205 7th floor, building B8, Lugu Enterprise Square, Yuelu District, Changsha City, Hunan Province Patentee before: CHANGSHA ADVANCED MATERIALS INDUSTRIAL RESEARCH INSTITUTE Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |