CN109678150B - Substrate for diamond synthesis, temperature uniformity control device and synthesis equipment - Google Patents
Substrate for diamond synthesis, temperature uniformity control device and synthesis equipment Download PDFInfo
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- CN109678150B CN109678150B CN201811556884.3A CN201811556884A CN109678150B CN 109678150 B CN109678150 B CN 109678150B CN 201811556884 A CN201811556884 A CN 201811556884A CN 109678150 B CN109678150 B CN 109678150B
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Abstract
The substrate for synthesizing diamond belongs to the field of artificial crystal synthesizing equipment technology, and includes: a substrate base having a contact surface on which a seed crystal is placed; and the thermal compensation unit comprises a plurality of thermal compensation components arranged on the substrate base body, and the thermal compensation components are used for carrying out temperature regulation on the temperature of the contact surface. There is also provided a temperature uniformity control apparatus comprising: a substrate; the temperature measuring assembly is used for measuring the real-time temperature of the seed crystal; and the temperature controller controls the corresponding thermal compensation component to work to carry out thermal compensation adjustment according to the real-time temperature of the seed crystal measured by the temperature measurement component. A synthesis apparatus having a reaction chamber using the substrate for diamond synthesis; and/or the equipment is provided with the temperature uniformity control device. The thermal compensation assembly can correspond to each seed crystal, so that thermal compensation is carried out on each seed crystal, the control effect of local temperature is achieved, the integral temperature uniformity is finally achieved, and the yield of the diamond is remarkably improved.
Description
Technical Field
The invention relates to the field of diamond synthesis, in particular to a substrate for diamond synthesis, a temperature uniformity control device and a synthesis system, and belongs to the technical field of artificial crystal synthesis equipment.
Background
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 due to no introduction of impurities, and is a more suitable method.
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 control of temperature uniformity in the process of growing diamond is very important, and the current common cooling mode is that a condensed fluid medium is introduced into the substrate, and heat is taken away through medium flow so as to control the temperature in the synthesis process. However, in the process of growing multiple diamonds together, the method cannot continuously and effectively ensure the temperature uniformity among the seed crystals and among the same seed crystal. The possible reasons are as follows: firstly, the plasma is in an ellipsoid shape, which is a principle defect of uneven synthesis temperature among seed crystals, secondly, the height of the same seed crystal can continuously extend into the plasma along with the increase of the thickness of the diamond, and the temperature of the seed crystal is continuously increased because the temperature of the center of a plasma ball is gradually increased.
The process of synthesizing diamond by microwave plasma chemical vapor deposition (mpcvd) (microwave plasma chemical vapor deposition) is shown in fig. 5. Device for synthesizing multiple diamonds by CVD method: the seed crystal is arranged on the substrate, and during the synthesis process, the diamond is continuously deposited on the surface of the seed crystal (the block in the figure represents the seed crystal) and gradually grows.
The condensed fluid medium is introduced into the substrate, and the heat is taken away through the medium flow so as to control the temperature of the seed crystal in the synthesis process. The non-contact infrared thermometer adjusts the laser point location to the position to be measured through the observation window, and then carries out real-time monitoring.
In the process of synthesizing diamond in batches, a non-contact temperature measuring device monitors and measures the temperature of the upper surface of seed crystals, and as the reaction proceeds, the phenomenon that the temperature of individual single crystals is too low or too high is often caused due to the comprehensive influence of various factors, but the current technical scheme can not control the temperature of individual seed crystals, and after the phenomenon occurs, only the temperature can be reduced to readjust the temperature uniformity of the seed crystals, but the operation greatly increases the time cost, and simultaneously the temperature control problem of individual single crystals can not be solved; or the production is continued, and the product yield is finally reduced. Whatever action is taken, this solution increases the cost of the final product.
Disclosure of Invention
During diamond synthesis, temperature stability is of paramount importance to the quality of the final product. Temperature uniformity control is a major difficulty in mass production of diamonds. The invention mainly aims at the problem that the temperature of individual seed crystals is not uniform in the synthesis process, provides a substrate for diamond synthesis, a temperature uniformity control device and synthesis equipment, realizes the control of local temperature, and achieves the purposes of improving the yield and reducing the cost.
The present invention provides a substrate for diamond synthesis for placing a seed crystal for diamond synthesis, comprising:
a substrate base having a contact surface on which a seed crystal is placed;
a thermal compensation unit including a plurality of thermal compensation members disposed on the substrate base,
the thermal compensation assembly is used for adjusting the temperature of the contact surface.
Further, the thermal compensation component is arranged in the substrate base body and corresponds to the position of the contact surface.
Further, a plurality of contact surfaces are arranged in a horizontal and vertical strip shape,
further, wherein the thermal compensation component is an electric heater and/or an electric refrigerator. Further preferably, the thermal compensation component is an electric heater.
Further, the thermal compensation assembly further comprises a temperature measuring device, and the temperature measuring device is preferably a thermocouple.
The invention also provides a temperature uniformity control device in the diamond synthesis process, which is characterized by comprising the following components:
the substrate for diamond synthesis has a contact surface for placing a seed crystal;
the temperature measuring assembly is used for measuring the real-time temperature of the seed crystal;
and the temperature controller controls the corresponding thermal compensation component to work to carry out thermal compensation adjustment according to the real-time temperature of the seed crystal measured by the temperature measurement component.
Furthermore, the temperature measuring component is a thermocouple or a non-contact temperature measuring device.
Further preferably, the temperature measuring assembly is a non-contact temperature measuring device.
Further preferably, the non-contact temperature measuring device is a non-contact infrared thermometer.
The thermal compensation assembly is used for adjusting the temperature of the contact surface.
Further, the thermal compensation component is arranged in the substrate base body and corresponds to the position of the contact surface.
Further, the contact surfaces are arranged in a horizontal and vertical strip shape.
Further, wherein the thermal compensation component is an electric heater and/or an electric refrigerator.
Furthermore, the temperature uniformity control device also comprises a control center, wherein the control center is connected with the temperature measurement assembly and the thermal compensation assembly and is used for receiving the temperature measurement data of the temperature measurement assembly and controlling the thermal compensation assembly to perform thermal compensation according to the difference between the measured temperature data and the target temperature.
Further, the substrate is positioned on a substrate table.
Furthermore, the substrate table is provided with a heat conducting wire, and the substrate is positioned on the heat conducting wire. Further preferably, the heat conducting wires are molybdenum wires.
The substrate table is provided with a heat dissipation structure, the heat dissipation structure comprises a condensation cavity, a liquid inlet channel and a liquid outlet channel, the condensation cavity is arranged in the substrate table and close to the top end of the substrate table, and the condensation cavity is communicated with the liquid inlet channel and the liquid outlet channel.
As a further improvement of the technical proposal, the top of the condensation cavity is provided with a plurality of grooves for increasing the contact area of the condensation medium and the substrate table.
The invention also provides MPCVD synthesis equipment, which is characterized in that: the reaction chamber of the device uses the substrate for synthesizing diamond; and/or the equipment is provided with the temperature uniformity control device.
Action and effects of the invention
According to the substrate for diamond synthesis provided by the invention, the thermal compensation unit is arranged in the substrate, and the thermal compensation component of the thermal compensation unit can correspond to each seed crystal, so that the thermal compensation is carried out on each seed crystal, the control effect of local temperature is achieved, the integral temperature uniformity is finally achieved, and the yield of diamond is obviously improved.
Because the thermal compensation unit still has temperature measurement device, through temperature measuring device, give temperature controller with real-time temperature measurement data transfer, automatic control heat adjusting device's heating or refrigeration effect, and then carry out automatic control to the seed crystal temperature that the temperature is low or is low excessively, realize the temperature inequality of automatic control small-range, reach temperature homogeneity purpose.
Drawings
FIG. 1 is a schematic view of the structure of a substrate for diamond synthesis in an embodiment of the present invention;
FIG. 2 is a top view of FIG. 1 of FIG. 2;
FIG. 3 is a schematic structural view of an MPCVD synthesis apparatus in an embodiment of the present invention;
FIG. 4 is a flow chart of microwave plasma chemical vapor deposition MPCVD method for synthesizing diamond; and
FIG. 5 is a schematic structural diagram of an apparatus for synthesizing a plurality of diamonds by a CVD method. Illustration of the drawings:
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the following embodiments are specifically described for the substrate for diamond synthesis, the temperature uniformity control device and the synthesis system of the invention with reference to the attached drawings.
Example 1
Fig. 1 is a schematic view of the structure of a substrate for diamond synthesis in an embodiment of the present invention.
Fig. 2 is a top view of fig. 1 of fig. 2.
As shown in FIGS. 1 and 2, a substrate for diamond synthesis on which a seed crystal 4 for diamond synthesis is placed comprises a substrate base 2 and a thermal compensation unit comprising a plurality of thermal compensation members 5.
The substrate base body 2 has a contact surface 2 for placing a seed crystal on the upper part and a groove 2 provided on the bottom part, and has a cooling passage for circulating a cooling medium and a plurality of mounting holes provided in the base body.
The contact surface processing requirement is high, and the contact surface is a component which is directly contacted with the seed crystal to support, as shown in fig. 2, the contact surface can be processed on the upper surface of the whole substrate 2, or a plurality of contact surfaces are arranged in a horizontal, horizontal and vertical strip shape at intervals.
The position of the mounting hole is corresponding to the position of the contact surface, and the mounting hole can be mounted by arranging a filling block after grooving or designing the base body 2 into a split type (sealing after mounting).
And a thermal compensation unit comprising a plurality of thermal compensation components 5 disposed on the substrate base. In this embodiment, the thermal compensation assembly is used for detecting the temperature of the corresponding contact surface and adjusting the temperature, and includes a temperature sensing device and a thermal adjustment device, which are all disposed in the corresponding mounting holes.
Further, a thermal compensation component 5 is arranged in the substrate base body at a position corresponding to the contact surface.
Specifically, the thermal compensation component is an electric heater and/or an electric refrigerator: heating and raising the temperature of the local substrate base body by using an electric heater; the heat of the local substrate base body is rapidly conducted out by using an electric refrigerator, and the temperature of the substrate base body is rapidly reduced. The electric heater can use PTC ceramic heating body or thermal resistance wire, and the electric refrigerator can use semiconductor refrigeration piece, obviously under this high temperature condition, should use ceramic/metal packaged military or specially customized semiconductor refrigeration piece or use other electric refrigeration device after future technology advance.
The temperature measuring device is preferably a high temperature-resistant temperature sensing device such as a thermocouple due to high temperature.
Example 2
This example also provides a temperature uniformity control device based on the novel substrate, which includes the substrate, the temperature measurement unit, and the temperature controller in example 1, in addition to the substrate for diamond synthesis provided in example 1.
The substrate is positioned on the base plate table 1, the heat-conducting wires 3 are placed on the base plate table, and the substrate is positioned on the heat-conducting wires, preferably, the heat-conducting wires are molybdenum wires. The thermally conductive filaments separate the substrate base 2 from the substrate table 1, as shown in fig. 1.
The temperature measuring component is used for measuring the real-time temperature of the seed crystal, and the temperature measuring component is a non-contact temperature measuring device, preferably a non-contact infrared thermometer 90.
And the temperature controller controls the corresponding thermal compensation component to work to carry out thermal compensation adjustment according to the real-time temperature of the seed crystal measured by the temperature measurement component.
The substrate table is provided with a heat dissipation structure, the heat dissipation structure comprises a condensation cavity 11, a liquid inlet channel 12 and a liquid outlet channel 13, the condensation cavity is arranged in the substrate table and close to the top end of the substrate table, and the condensation cavity is communicated with the liquid inlet channel and the liquid outlet channel.
Furthermore, the top of the condensation cavity is provided with a plurality of grooves for increasing the contact area of the condensation medium and the substrate table.
Obviously, the above components are required to have certain high temperature resistance requirements due to the high temperature environment of diamond synthesis, wherein the substrate base 1 is in a round cake shape capable of resisting at least 900 ℃, alloy steel is preferably used, and the high temperature resistance requirement of the substrate table 1 is lower.
Further, the uniformity control device also comprises a control center 1, wherein the control center is connected with the temperature measurement assembly and the thermal compensation assembly through a signal processing center 20, and is used for receiving the temperature measurement data of the temperature measurement assembly and controlling the thermal compensation assembly to perform thermal compensation according to the difference between the measured temperature data and the target temperature.
Example 3
As shown in fig. 3, the embodiment provides an MPCVD synthesizing apparatus, which includes a control center 10, a signal processing center 20, a microwave power supply 30, a microwave generating device 40, a microwave transmission guiding device 50, a reflected microwave adjusting device (middle section) 60, a mode converter 70, a reflected microwave adjusting device (end section) 80, a non-contact infrared thermometer 90, and a reaction chamber 100.
The apparatus has a reaction chamber 100 in which the substrate for diamond synthesis in example 1 is used, and a specific substrate base 2 is set on a substrate stage 1.
Or further, in order to better control the temperature, the apparatus further has the temperature uniformity control device in embodiment 2, the signal processing center 20 is connected with the temperature measurement module and the thermal compensation module through wires, and the control center 10 receives the temperature measurement data of the temperature measurement module through the signal processing center 20 and controls the thermal compensation module to perform thermal compensation according to the difference between the measured temperature data and the target temperature.
The diamond synthesis apparatus of the present embodiment has the following functions:
the central control device is used for monitoring and feeding back the temperature of the whole reaction container. When the non-contact temperature measuring device monitors the temperature, compared with the set target temperature, and when the temperature is lower than the set target temperature, the microwave power supply 30 and the microwave generating device 40 are controlled to heat and raise the temperature; when the temperature is higher than the preset temperature, the microwave power supply 30 and the microwave generating device 40 are controlled to stop or reduce the heating power, and meanwhile, the cooling device starts to drive the cooling medium in the heat dissipation structure to circulate for cooling. For the single crystal with lower temperature (the temperature difference is more than 10 ℃), the single crystal is automatically fed back to the control center.
And (4) local temperature control. On the basis of feedback, gradually starting a thermal compensation component corresponding to the seed crystal with lower or higher temperature: when the temperature is higher, the corresponding electric refrigeration component is started to carry out refrigeration and cooling; when the temperature is lower, the corresponding electric heating device is started to heat and raise the temperature so as to achieve the purpose of local temperature compensation, and meanwhile, the temperature is measured through the temperature measuring device and then is transmitted to the temperature controller to be controlled, so that the temperature of the plurality of diamonds is kept consistent. In the operation process, the temperature measuring device outputs data to the signal processing center 20 and feeds back the data to the control center 10 in time, whether the data are in an effective temperature interval (set by a user) is automatically judged, if the data are in the temperature interval, the equipment continues to operate, and if the data deviate from the effective temperature interval, the data are fed back to the control center 10, the thermal compensation assembly is started, and then the temperature is recovered to the effective temperature interval. Effects and effects of the embodiments
According to the substrate for diamond synthesis provided by the embodiment, because the thermal compensation unit is arranged in the substrate, the thermal compensation component of the thermal compensation unit can correspond to each seed crystal, so that the thermal compensation is carried out on each seed crystal, the control effect of local temperature is achieved, the integral temperature uniformity is finally achieved, and the yield of diamond is obviously improved.
Because the thermal compensation unit still has temperature measurement device, through temperature measuring device, give temperature controller with real-time temperature measurement data transfer, automatically control the heating or the refrigeration effect of thermal control device, and then carry out automatic control to the seed crystal temperature that the temperature is low or low excessively, realize the uneven temperature of automatic control small-range, reach temperature homogeneity purpose.
The embodiment provides a new cooling mode, namely a cooling structure, and the cooling effect can be increased. The improvement of the cooling effect can improve the process temperature and increase the plasma density. As is well known, the rate of diamond synthesis is proportional to pressure and power. When the pressure and the power are increased, the plasma density is increased, the growth speed is increased, the synthesis time is shortened, and the synthesis cost is reduced.
Embodiments provide a thermal compensation assembly applied to a diamond composite substrate, capable of improving temperature uniformity. The temperature control plays a decisive role in the yield of diamond batch production. The thermal compensation assembly corresponds to the placing position of the seed crystal, can play a role in controlling local temperature, finally achieves integral temperature uniformity, and obviously improves the yield of diamond.
The automatic temperature control in the diamond synthesis process is realized. Through the temperature measurement device, data are transmitted to the temperature controller, then the heating and/or refrigerating effect of the thermal compensation assembly is automatically controlled by the temperature controller, and then the automatic control is carried out on the seed crystal temperature with too low or too high temperature, so that the purpose of automatically controlling the temperature uniformity is realized.
In a word, the device and the synthesis equipment can stably operate in the synthesis process and the system of multiple diamonds, save a large amount of time for stopping the machine and readjusting the temperature, obviously improve the yield of the synthesized diamonds and reduce the cost.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (9)
1. A temperature uniformity control device in a diamond synthesis process is characterized by comprising:
a substrate for diamond synthesis for placing a seed crystal for diamond synthesis, the substrate having a contact surface for placing the seed crystal;
the temperature measuring assembly is used for measuring the real-time temperature of the seed crystal;
the temperature controller controls the corresponding thermal compensation component to work for thermal compensation adjustment according to the real-time temperature of the seed crystal measured by the temperature measuring component,
wherein, the substrate is used for placing seed crystals for diamond synthesis, and comprises:
a substrate base having a contact surface on which a seed crystal is placed;
a thermal compensation unit including a plurality of thermal compensation members disposed on the substrate base,
the thermal compensation component is used for adjusting the temperature of the contact surface,
the substrate is positioned on a base plate table, a heat dissipation structure is arranged on the base plate table,
the heat dissipation structure comprises a condensation cavity, a liquid inlet channel and a liquid outlet channel which are arranged in the substrate table,
the condensation cavity is located at a position, close to the top end of the substrate table, in the substrate table and communicated with the liquid inlet channel and the liquid outlet channel.
2. The apparatus for controlling temperature uniformity in a diamond synthesis process according to claim 1, wherein:
wherein, the temperature measuring component is a non-contact temperature measuring device;
and/or the temperature measuring component is a non-contact infrared thermometer.
3. The apparatus for controlling temperature uniformity in a diamond synthesis process according to claim 1, further comprising:
and the control center is connected with the temperature measuring assembly and the thermal compensation assembly and is used for receiving the temperature measuring data of the temperature measuring assembly and controlling the thermal compensation assembly to perform thermal compensation according to the difference between the measured temperature data and the target temperature.
4. The apparatus for controlling temperature uniformity in a diamond synthesis process according to claim 1, wherein:
wherein, the heat-conducting wires are arranged on the base plate table, and the substrate is positioned on the heat-conducting wires;
and/or the heat conducting wires are molybdenum wires.
5. The apparatus for controlling temperature uniformity in a diamond synthesis process according to claim 1, wherein:
wherein, the top of the condensation cavity is provided with a plurality of grooves for increasing the contact area of the condensation medium and the substrate table.
6. The temperature uniformity control apparatus of claim 1, wherein:
wherein the thermal compensation component is arranged in the substrate base body and corresponds to the position of the contact surface;
and/or a plurality of contact surfaces are arranged in a horizontal and vertical strip shape.
7. The temperature uniformity control apparatus of claim 1, wherein:
wherein the thermal compensation component is an electric heater and/or an electric refrigerator;
and/or, the thermal compensation component is an electric heater.
8. The temperature uniformity control apparatus of claim 1, wherein:
wherein, the thermal compensation component also comprises a temperature measuring device;
and/or the temperature measuring device is a thermocouple.
9. An MPCVD synthesis device, characterized in that:
the apparatus has a temperature uniformity control device as claimed in any one of claims 1 to 8.
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| CN112684829A (en) * | 2020-12-22 | 2021-04-20 | 同济大学 | Temperature detection control system and method for MPCVD device |
| CN112779599B (en) * | 2020-12-23 | 2022-11-18 | 济南金刚石科技有限公司 | Chemical vapor deposition method and device for submicron diamond film |
| CN113515151B (en) * | 2021-04-14 | 2022-04-08 | 上海征世科技股份有限公司 | Temperature control device and control method for MPCVD equipment |
| CN113584577A (en) * | 2021-08-04 | 2021-11-02 | 中电化合物半导体有限公司 | Silicon carbide crystallization interface control structure, growth equipment and preparation method |
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| UA81614C2 (en) * | 2001-11-07 | 2008-01-25 | Карнеги Инститьюшн Ов Вашингтон | Device for producing of diamonts, unit for sample holding (variants) and method for producing of diamonds (variants) |
| US9279190B2 (en) * | 2013-11-12 | 2016-03-08 | Shanghai Jiao Tong University | Method for preparing diamond carbon membrane on surface of stainless steel |
| US9469918B2 (en) * | 2014-01-24 | 2016-10-18 | Ii-Vi Incorporated | Substrate including a diamond layer and a composite layer of diamond and silicon carbide, and, optionally, silicon |
| CN104775154B (en) * | 2015-04-25 | 2017-06-27 | 哈尔滨工业大学 | A kind of method of control surface temperature during isoepitaxial growth single-crystal diamond |
| CN107021480B (en) * | 2017-04-26 | 2019-01-08 | 金华职业技术学院 | A kind of reactor preparing diamond for deposition |
| CN107628607A (en) * | 2017-11-01 | 2018-01-26 | 成都格莱飞科技股份有限公司 | A kind of growth apparatus of graphene |
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