CN109678150A - Substrate, thermal evenness controlling device and the synthesis device of diamond synthesizing - Google Patents
Substrate, thermal evenness controlling device and the synthesis device of diamond synthesizing Download PDFInfo
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- CN109678150A CN109678150A CN201811556884.3A CN201811556884A CN109678150A CN 109678150 A CN109678150 A CN 109678150A CN 201811556884 A CN201811556884 A CN 201811556884A CN 109678150 A CN109678150 A CN 109678150A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/26—Preparation
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Abstract
The substrate of diamond synthesizing belongs to artificial crystal synthesis device technical field, comprising: substrate matrix has the contact surface for placing seed crystal；Thermal compensation unit, including multiple thermal compensation components being arranged on substrate matrix, thermal compensation component is used to carry out temperature adjusting to the temperature of the contact surface.Also provide thermal evenness controlling device, comprising: substrate；Temperature measures component, for measuring the real time temperature of seed crystal；Temperature controller measures the seed crystal real time temperature that component measures according to the temperature, controls corresponding thermal compensation component operation and carries out thermal compensation adjusting.Synthesis device, the reaction cavity which has using above-mentioned diamond synthesizing substrate；And/or the equipment has above-mentioned thermal evenness controlling device.The thermal compensation component having can be corresponding with each seed crystal, so that carrying out thermal compensation to each seed crystal is finally reached whole temperature uniformity to play the control action of local temperature, and then is obviously improved the yield of diamond.
Description
Technical field
The present invention relates to diamond synthesizing fields, and in particular to a kind of substrate of diamond synthesizing, temperature uniformity control
Device processed and synthesis system belong to artificial crystal synthesis device technical field.
Background technique
Diamond causes everybody concern due to having extremely excellent physicochemical properties.But natural diamond stores up
Measure limited, then people develop a variety of diamond synthesis methods, such as high temperature and high pressure method (HPHT), hot filament CVD
(HJCVD).Wherein MPCVD method (Microwave plasma chemical vapor
Deposition) diamond synthesis method can synthesize high quality, the diamond of large area forms due to the introducing of not no impurity
For proper method.
The quality of MPCVD method diamond synthesis is related with many factors, including carbon source concentration, gas flow size, temperature,
Substrate table height, microwave power, synthesis temperature.Wherein the control of temperature uniformity is particularly important during growth diamond, mesh
Preceding common cooling method is that substrate interior is passed through condensed fluid medium, takes away heat by media flow, was synthesized with control
Temperature in journey.However during carrying out more diamond syntrophisms, this mode can not continuous and effective guarantee seed crystal
Between seed crystal and the uniformity of same seed temperature.It is possible the reason is as follows that: 1. plasma be elliposoidal, this is to lead
The non-uniform principle defect of synthesis temperature between seed crystal is caused, 2. with the growth of diamond, the increase of seed crystal thickness, same
Seed crystal height can constantly be goed deep into inside plasma, and since temperature is stepped up at plasma ball center, this also leads to seed
Brilliant temperature constantly increases, 3. the contact surface of substrate and seed crystal, due to the mode of substrate surface processing, or processing aspect itself
Caused by gap cause contact surface to increasingly generate carbon black with the progress of reaction, influence to radiate, what 4. seed crystal itself had leads
Heat differential is different, and 5. since gas source and electric field strength are inconsistent, caused plasma species and Density Distribution are uneven, thus with
, there is the phenomenon that non-uniform temperature in the progress of reaction.
MPCVD method MPCVD (Microwave plasma chemical vapor
Deposition) process of diamond synthesis is as shown in Figure 5.CVD method synthesizes the device of more diamonds: seed crystal is arranged in substrate
On, during synthesis, diamond is constantly deposited on seed crystal (square indicates seed crystal in figure) surface, is grown into.
Substrate interior is passed through condensed fluid medium, takes away heat by media flow, to control seed crystal in synthesis process
Temperature.Laser point is adjusted to position to be measured by observation window by Non-contacting Infrared Thermometer, is carried out later real-time
Monitoring.
During batch diamond synthesis, non-contact temperature measuring device monitoring measures seed crystal upper surface temperature, with
The progress of reaction frequently can lead to individual monocrystalline and the too low or excessively high phenomenon of temperature occurred due to the combined influence of various factors,
But current technology scheme, it can not accomplish the control for individual seed temperatures, after there is the phenomenon, cooling weight can only be selected
New adjustment seed temperature uniformity, but the operation greatly increases time cost, while can not also solve the temperature of individual monocrystalline
Spend control problem；Or continue to produce, eventually reduce product yield.No matter which kind of operation is taken, and the technical solution is all
It will increase the cost of final products.
Summary of the invention
During diamond synthesizing, temperature stability is particularly important for the quality of final products.In batch production gold
During hard rock, the uniformity controlling of temperature is a big difficulty.Present invention is generally directed to occur individual seed crystal temperature in synthesis process
Non-uniform problem is spent, proposes the substrate, thermal evenness controlling device and synthesis device of a kind of diamond synthesizing, realization pair
The control of local temperature achievees the purpose that promote yield, reduces cost.
The present invention provides a kind of substrate of diamond synthesizing, for placing the seed crystal of diamond synthesizing, comprising:
Substrate matrix has the contact surface for placing seed crystal；
Thermal compensation unit, including multiple thermal compensation components being arranged on substrate matrix,
Wherein, thermal compensation component is used to carry out temperature adjusting to the temperature of contact surface.
Further, wherein thermal compensation component is arranged in substrate matrix and the position of corresponding contact surface.
Further, wherein the smooth vertical and horizontal bar shaped arrangement of multiple contact surfaces,
Further, wherein thermal compensation component is electric heater and/or electric refrigerator.It is further preferred that thermal compensation group
Part is electric heater.
Further, further include temperature measurement device in thermal compensation component, temperature measurement device be preferably thermocouple.
The present invention also provides the thermal evenness controlling devices during a kind of diamond synthesizing characterized by comprising
The substrate of above-mentioned diamond synthesizing has the contact surface for placing seed crystal；
Temperature measures component, for measuring the real time temperature of seed crystal；
Temperature controller measures the seed crystal real time temperature that component measures according to temperature, controls corresponding thermal compensation component work
Make to carry out thermal compensation adjusting.
Further, temperature measurement component is thermoelectricity occasionally non-contact temperature measuring device.
It is further preferred that temperature measure component non-contact temperature measuring device.
It is further preferred that non-contact temperature measuring device is Non-contacting Infrared Thermometer.
Thermal compensation component is used to carry out temperature adjusting to the temperature of contact surface.
Further, wherein thermal compensation component is arranged in substrate matrix and the position of corresponding contact surface.
Further, wherein the smooth vertical and horizontal bar shaped arrangement of multiple contact surfaces.
Further, wherein thermal compensation component is electric heater and/or electric refrigerator.
Further, thermal evenness controlling device further includes control centre, control centre and temperature measurement component and
Thermal compensation component connection, for receiving the temperature measuring data of temperature measurement component, and according to measurement temperature data and target temperature
The gap control thermal compensation component of degree carries out thermal compensation.
Further, substrate is located on Substrate table.
Further, be placed with heat conductive filament on Substrate table, substrate be located on heat conductive filament.It is further preferred that lead
Heated filament is molybdenum filament.
Substrate table is equipped with radiator structure, and radiator structure includes the condensation chamber being located in Substrate table, feed pathway and liquid out
Channel, condensation chamber are located at the position in Substrate table close to Substrate table top, and condensation chamber is connected to feed pathway, liquid outlet channel.
As a further improvement of the above technical scheme, several grooves are equipped at the top of condensation chamber for increasing cooling medium
With the contact area of Substrate table.
The present invention also provides a kind of MPCVD synthesis devices, it is characterised in that: the reaction cavity that the equipment has uses above-mentioned
Diamond synthesizing substrate；And/or the equipment has above-mentioned thermal evenness controlling device.
The effect and effect of invention
The substrate of the diamond synthesizing provided according to the present invention, because being provided with thermal compensation unit in substrate interior,
The thermal compensation component having can be corresponding with each seed crystal, so that thermal compensation is carried out to each seed crystal, to play office
The control action of domain temperature is finally reached whole temperature uniformity, and then is obviously improved the yield of diamond.
Because thermal compensation unit also has temperature measurement device, by temperature measuring device, by real time temperature measurement data
Send temperature controller to, to automatically control the heating or refrigeration effect of thermal conditioning device, and then it is too low for temperature or
Too low seed temperature carries out automatically controlling, and realizes and automatically controls small-scale temperature unevenness, reaches temperature uniformity purpose.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the substrate of diamond synthesizing in the embodiment of the present invention；
Fig. 2 is the top view of Fig. 1 of Fig. 2；
Fig. 3 is the structural schematic diagram of MPCVD synthesis device in the embodiment of the present invention；
Fig. 4 is the flow chart of MPCVD method MPCVD diamond synthesis；And
Fig. 5 is the apparatus structure schematic diagram that chemical vapour deposition technique CVD method synthesizes more diamonds.It illustrates:
Specific embodiment
It is real below in order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention
Example combination attached drawing is applied specifically to explain substrate, thermal evenness controlling device and the synthesis system work of diamond synthesizing of the invention
It states.
Embodiment 1
Fig. 1 is the structural schematic diagram of the substrate of diamond synthesizing in the embodiment of the present invention.
Fig. 2 is the top view of Fig. 1 of Fig. 2.
As shown in Figure 1, 2, the substrate of diamond synthesizing, for placing the seed crystal 4 of diamond synthesizing, including substrate base
The thermal compensation unit of body 2, multiple thermal compensation components 5 composition.
Substrate matrix 2, top have the contact surface 2 and groove arranged at the bottom 2 for placing seed crystal, have and are situated between for cooling
The logical cooling duct of mass flow and setting are in the intracorporal multiple mounting holes of base.
Contact surface processing request is higher, is that the component for carrying out support is directly contacted with seed crystal, as shown in Fig. 2, can be
Contact surface is all processed in the upper surface of entire matrix 2, is also possible to the smooth vertical and horizontal bar shaped of multiple contact surfaces and is alternatively arranged.
The position of mounting hole is corresponding with the position of contact surface, can be by the way that fill block is arranged after grooving to install or by matrix
2 are designed as split type (installing rear re-closed).
Thermal compensation unit, including multiple thermal compensation components 5 being arranged on substrate matrix.In the present embodiment, thermal compensation group
The temperature that part is used to detect corresponding contact surface is gone forward side by side trip temperature adjusting, including temperature sensor and thermal conditioning device,
It is arranged in corresponding mounting hole.
Further, the position in substrate matrix and corresponding to contact surface is arranged in thermal compensation component 5.
Specifically, thermal compensation component is electric heater and/or electric refrigerator: carrying out the lining to part by using electric heater
Base body carries out heat temperature raising；Quickly export the heat of local substrate matrix by using electric refrigerator, but its fast prompt drop
Temperature.PTC ceramics calandria or hot water radiation wire can be used in electric heater, and semiconductor chilling plate can be used in electric refrigerator,
Obviously under this high-temperature condition, should use ceramic/metal encapsulate military or particularly customized semiconductor chilling plate or
Other electric refrigeration devices are used after WeiLai Technology progress.
Temperature measurement device, since temperature is higher, the temperature sensing devices resistant to high temperature such as preferred thermoelectric is even.
Embodiment 2
The present embodiment is also provided on the basis of the diamond synthesizing substrate that embodiment 1 provides based on the novel substrate
A kind of thermal evenness controlling device comprising substrate, temperature measurement component and temperature controller in above-described embodiment 1.
Substrate, be located at Substrate table 1 on, Substrate table on be placed with heat conductive filament 3, substrate be located on heat conductive filament, it is preferred that
Heat conductive filament be molybdenum filament.The heat conductive filament keeps apart substrate matrix 2 and Substrate table 1, as shown in Figure 1.
Temperature measures component, and for measuring the real time temperature of seed crystal, temperature measures component non-contact temperature measuring device, preferably
, it is Non-contacting Infrared Thermometer 90 that temperature, which measures component,.
Temperature controller measures the seed crystal real time temperature that component measures according to temperature, controls corresponding thermal compensation component work
Make to carry out thermal compensation adjusting.
Wherein, Substrate table is equipped with radiator structure, and radiator structure includes the condensation chamber 11 being located in Substrate table, feed pathway
12 are located at the position in Substrate table close to Substrate table top with liquid outlet channel 13, condensation chamber, and condensation chamber and feed pathway, liquid is logical out
Road connection.
Further, several grooves are equipped at the top of condensation chamber with the contact area for increasing cooling medium and Substrate table.
Clearly as the hot environment of diamond synthesizing, above component requires certain high temperature resistant requirement,
In, substrate matrix 1 is to be resistant at least 900 DEG C of round pie, it is preferable to use steel alloy, and the high temperature resistant of Substrate table 1 requires low one
A bit.
Further, which further includes control centre 1, and control centre passes through signal processing center 20
Component is measured with temperature and thermal compensation component is connect, for receiving the temperature measuring data of temperature measurement component, and according to survey
Amount temperature data and the gap of target temperature control thermal compensation component carry out thermal compensation.
Embodiment 3
As shown in figure 3, the present embodiment provides a kind of MPCVD synthesis device, including control centre 10, signal processing center
20, microwave power supply 30, microwave generating apparatus 40, microwave transmission guide device 50, microwave reflection regulating device (middle section) 60, mode
Converter 70, microwave reflection regulating device (latter end) 80, Non-contacting Infrared Thermometer 90 and reaction cavity 100.
It is specific to serve as a contrast using the substrate of the diamond synthesizing in embodiment 1 in the reaction cavity 100 that the equipment has
Base body 2 is arranged on Substrate table 1.
Or it is further, in order to preferably carry out temperature control, which also has the temperature in above-described embodiment 2 equal
Even property control device, signal processing center 20 measures component with temperature and thermal compensation module wire is connect, and control centre 10 is logical
The temperature measuring data that signal processing center 20 receives temperature measurement component is crossed, and according to measurement temperature data and target temperature
Gap controls thermal compensation component and carries out thermal compensation.
The diamond synthesizing equipment of the present embodiment has function below:
Central controller carries out the monitoring of W-response vessel temp and feeds back.When non-contact temperature measuring device monitors temperature
When, compared with the target temperature of setting, when temperature is lower than, control microwave power supply 30, microwave generating apparatus 40 carry out heating and rise
Temperature；When temperature is higher than, control microwave power supply 30, microwave generating apparatus 40 stop or reduce heating power, while cooling dress
Cooling medium circulation in unlatching driving radiator structure is set to cool down.Monocrystalline (temperature difference is at 10 DEG C or more) lower for temperature,
It is automatically fed to control centre.
The control of local temperature.On the basis of feedback, gradually opening temperature is lower or higher seed crystal corresponding to vulcanize
It repays component: when temperature is higher, opening corresponding electric cooling assembly, carry out refrigeration cool-down；When the temperature is low, it opens corresponding
Electric heating device carries out heat temperature raising, to achieve the purpose that local temperature-compensating, while carrying out thermometric by temperature measurement device
It is then passed to temperature controller to be controlled, is finally consistent more diamond temperature.In the process of running, temperature
Whether measurement device outputs data to signal processing center 20, and timely feedbacks to control centre 10, judge automatically in effective
Temperature range in (user's setting), if equipment continues to run in temperature range, if deviate effective temperature section, instead
It feeds control centre 10, starts thermal compensation component, and then temperature is restored to effective temperature section.The effect and effect of embodiment
Fruit
According to the substrate for the diamond synthesizing that embodiment provides, because being provided with thermal compensation unit in substrate interior,
The thermal compensation component having can be corresponding with each seed crystal, so that thermal compensation is carried out to each seed crystal, to play office
The control action of domain temperature is finally reached whole temperature uniformity, and then is obviously improved the yield of diamond.
Because thermal compensation unit also has temperature measurement device, by temperature measuring device, by real time temperature measurement data
Send temperature controller to, to automatically control the heating or refrigeration effect of thermal conditioning device, and then it is too low for temperature or
Too low seed temperature carries out automatically controlling, and realizes and automatically controls small-scale temperature unevenness, reaches temperature uniformity purpose.
Embodiment proposes that a kind of new type of cooling passes through radiator structure, can increase cooling effect.Cooling effect
It is promoted, technological temperature can be improved, increase plasma density.It is well known that the synthesis rate of diamond and pressure, power at
Direct ratio.When pressure and when power ascension, plasma density increases, and the speed of growth increases, and reduces generated time, reduce synthesis at
This.
Embodiment proposes that a kind of thermal compensation component is applied on diamond synthesizing substrate, can be improved temperature uniformity.Temperature
The control of degree, for producing the yield of diamond in batches, temperature plays decisive role.The thermal compensation component corresponds to seed crystal
Placement position, the control action of local temperature can be played, whole temperature uniformity is finally reached, is obviously improved diamond
Yield.
Realize A.T.C during diamond synthesizing.By temperature measurement device, temperature is transferred data to
Then controller is automatically controlled the heating and/or refrigeration effect of thermal compensation component by temperature controller, and then too low for temperature
Or excessively high seed temperature carries out automatically controlling, and realizes A.T.C uniformity purpose.
In short, the stable operation of the device and synthesis device energy more than enough diamond synthesizing process and system, saving stop
Machine readjusts the plenty of time of temperature, and has been obviously improved the yield of diamond synthesis, reduces cost.
Above embodiment is preferred case of the invention, the protection scope being not intended to limit the invention.
Claims (10)
1. a kind of substrate of diamond synthesizing, for placing the seed crystal of diamond synthesizing, comprising:
Substrate matrix has the contact surface for placing seed crystal；
Thermal compensation unit, including multiple thermal compensation components being arranged on substrate matrix,
Wherein, the thermal compensation component is used to carry out temperature adjusting to the temperature of the contact surface.
2. the substrate of diamond synthesizing according to claim 1, it is characterised in that:
Wherein, the position in the substrate matrix and corresponding to the contact surface is arranged in the thermal compensation component；
And/or the bar shaped arrangement that multiple contact surfaces are smooth vertical and horizontal.
3. the substrate of diamond synthesizing according to claim 1, it is characterised in that:
Wherein, the thermal compensation component is electric heater and/or electric refrigerator；
And/or the thermal compensation component is electric heater.
4. the substrate of diamond synthesizing according to claim 1, it is characterised in that:
It wherein, further include temperature measurement device in the thermal compensation component；
And/or the temperature measurement device is thermocouple.
5. the thermal evenness controlling device during a kind of diamond synthesizing characterized by comprising
Substrate described in any one of claim 1-4 has the contact surface for placing seed crystal；
Temperature measures component, for measuring the real time temperature of seed crystal；
Temperature controller measures the seed crystal real time temperature that component measures according to the temperature, controls corresponding thermal compensation component work
Make to carry out thermal compensation adjusting.
6. the thermal evenness controlling device during diamond synthesizing according to claim 5, it is characterised in that:
Wherein, the temperature measures component non-contact temperature measuring device；
And/or the temperature measurement component is Non-contacting Infrared Thermometer.
7. the thermal evenness controlling device during diamond synthesizing according to claim 5, which is characterized in that also wrap
It includes:
Control centre, control centre measures component with temperature and thermal compensation component is connect, for receiving the temperature measurement group
The temperature measuring data of part, and the thermal compensation component is controlled according to the gap of measurement temperature data and target temperature and is vulcanized
It repays.
8. the thermal evenness controlling device during diamond synthesizing according to claim 5, it is characterised in that:
Wherein, the substrate is located on Substrate table；
Heat conductive filament is placed on the Substrate table, the substrate is located on heat conductive filament；
And/or the heat conductive filament is molybdenum filament.
9. the thermal evenness controlling device during diamond synthesizing according to claim 8, it is characterised in that:
Wherein, the Substrate table is equipped with radiator structure,
The radiator structure includes the condensation chamber being located in the Substrate table, feed pathway and liquid outlet channel,
The condensation chamber is located at the position in the Substrate table close to Substrate table top, and the condensation chamber and feed pathway go out liquid
Channel connection；
And/or several grooves are equipped at the top of the condensation chamber with the contact area for increasing cooling medium and Substrate table.
10. a kind of MPCVD synthesis device, it is characterised in that:
The reaction cavity that the equipment has using diamond synthesizing described in any one of claim 1-4 substrate；
And/or the equipment has thermal evenness controlling device described in any one of claim 5-9.
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| CN201811556884.3A CN109678150B (en) | 2018-12-19 | 2018-12-19 | Substrate for diamond synthesis, temperature uniformity control device and synthesis equipment |
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| CN201811556884.3A CN109678150B (en) | 2018-12-19 | 2018-12-19 | Substrate for diamond synthesis, temperature uniformity control device and synthesis equipment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN112779599A (en) * | 2020-12-23 | 2021-05-11 | 济南金刚石科技有限公司 | Chemical vapor deposition method and device for submicron diamond film |
| CN113515151A (en) * | 2021-04-14 | 2021-10-19 | 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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Address after: 410205 East of the first floor, 2nd floor, 7th floor, 8th floor, Building B8, Luguyuyuan, No. 27 Wenxuan Road, Changsha High-tech Development Zone, Changsha, 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. |