CN110344021A - The equipment of the super Nano diamond of graphite heating chemical vapor deposition - Google Patents

The equipment of the super Nano diamond of graphite heating chemical vapor deposition Download PDF

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Publication number
CN110344021A
CN110344021A CN201810299894.7A CN201810299894A CN110344021A CN 110344021 A CN110344021 A CN 110344021A CN 201810299894 A CN201810299894 A CN 201810299894A CN 110344021 A CN110344021 A CN 110344021A
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China
Prior art keywords
graphite
sample stage
graphite block
heating
substrate
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丁明清
李莉莉
化称意
蔡军
冯进军
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CETC 12 Research Institute
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CETC 12 Research Institute
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Priority to CN201810299894.7A priority Critical patent/CN110344021A/en
Publication of CN110344021A publication Critical patent/CN110344021A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses provide a kind of equipment of super Nano diamond of graphite heating chemical vapor deposition, including sample stage component, gas handling system, graphite heating device assembly, the sample stage of sample stage component is for placing substrate to be deposited, gas handling system is for providing reaction gas, graphite heating device assembly includes graphite block and heating component, graphite block is located above the sample stage of the sample stage component, and and the opposite fire end of sample stage structure it is identical as substrate upper surface shape to be processed;Several deflector holes are offered on graphite block, deflector hole is used to reach the top of substrate to be deposited by the graphite block for the reaction gas of the gas handling system;Heating component is for heating graphite block.Present invention setting can in special-shaped deposition on substrate film thickness, texture is consistent with performance, super nanocrystalline diamond film of high quality as high intensity, wear-resisting protective film and functional film etc. can also manufacture the super nanocrystalline diamond components of polymorphic structure.

Description

The equipment of the super Nano diamond of graphite heating chemical vapor deposition
Technical field
The invention belongs to chemical vapour deposition diamond technical fields, and in particular to a kind of graphite heating chemical vapor deposition The equipment of super Nano diamond.
Background technique
Diamond is dielectric material most excellent in known materials, have low-k, low lossy microwave, high rigidity, The characteristics such as high thermal conductivity are in microwave vacuum device, infrared and laser device, mems device and solid electronic device Optimal dielectric material.At present experiment successfully by micron diamond (Micron crystal diamond, MCD, also referred to as Polycrystalline) it is used for short millimeter wave and Terahertz travelling-wave tubes delivery of energy window.Super nanocrystalline diamond (ultrananocrystalline Diamond, UNCD) it is another type of diamond, in 1993 by Argonne National Laboratory, U.S. Dieter Gruen Invention.The crystal grain of super nanocrystalline diamond can achieve nanoscale (3-5nm), much smaller than conventional nano diamond (NCD, crystalline substance Grain is from tens to several hundred microns).It has following advantages: 1. higher breaking strengths: >=1GPa compared with micron diamond, most High reachable 5GPa, 2. compactness are good, and surface roughness can reach 20-40nm.So that super nanocrystalline diamond is suitble to be made The thin-film material of high-mechanical property is widely used in the encapsulation and heat dissipation of sensor, micro-/nano electromechanical systems, solid electronic device, And the fields such as biomedicine.
As super nanocrystalline diamond is brilliant or nanocrystalline with micron, mainly pass through microwave plasma CVD (Microwave PCVD, MPCVD) and hot-wire chemical gas-phase deposition method (Hot Filament Chemical Vapor Deposition, HFCVD) it is grown.However, the substrate surface for growing diamond is flat state under normal conditions, Such as silicon wafer and metal substrate, so as to obtain on substrate each dot thickness uniformly, the diamond film of uniform quality.But in reality The surface of many parts or component is rendered as non-planar or polymorphic structure in.It is more for hot-filament chemical vapor deposition equipment Root heated filament constitutes a planar structure, mainly passes through radiant heating substrate.The distance between heated filament and substrate are usually 5 to 10 millis Rice exceeds the range, and the performance of diamond may rapid decrease.In microwave plasma CVD, substrate passes through Plasma is heated.Its surface each point temperature was both related with plasma, also related with substrate bottom heat transfer, for For special-shaped substrate, as a consequence it is hardly possible to be consistent surface each point temperature.Meanwhile even if substrate each point temperature is identical, due to The influence of shape plasma, the deposition rate on polymorphic structure surface can also differ greatly.So microwave etc. under normal conditions Ion body chemical vapor phase growing and hot-filament chemical vapor deposition equipment are not particularly suited for preparing diamond film on special-shaped substrate.
Such as the curved-surface structure of guided missile dome, using above-mentioned microwave plasma CVD or hot-wire chemical There are following problems in vapor deposition method.Firstly, on substrate surface each point non-uniform temperature, cause deposition rate and Buddha's warrior attendant The thickness of stone film is different.Second, the non-uniform temperature of each point on substrate surface, cause diamond film texture and mechanical, mechanics Etc. performances difference.Third, diamond film thickness difference often result in the rising of inside and outside stress with texture difference, lead to Buddha's warrior attendant The cracking of stone film and removing.Either the thickness difference of diamond film or the difference of texture and performance, for many applications Say it is all unacceptable, needless to say the cracking of diamond film and removing.
In conclusion existing MPCVD and HFCVD equipment special-shaped substrate surface deposit super nanocrystalline diamond when, There are the differences of the thickness of diamond film, texture and performance, lead to the various quality problems such as cracking and removing of diamond film.
Summary of the invention
In view of the above problems, the invention proposes the schemes to solve the above problems, provide a kind of thickness for realizing diamond Uniformly, the equipment of texture and the identical super Nano diamond of graphite heating chemical vapor deposition of performance.
According to one aspect of the present invention, a kind of equipment of super Nano diamond of graphite heating chemical vapor deposition is provided, Including sample stage component and gas handling system, the sample stage of the sample stage component is for placing substrate to be deposited, the air inlet system System is for providing reaction gas, further includes: graphite heating device assembly,
The graphite heating device assembly includes graphite block and heating component, and the graphite block is located at the sample stage component Above sample stage, and and the opposite fire end of sample stage structure it is identical as substrate upper surface shape to be deposited;The graphite block On offer several deflector holes, the deflector hole be used for the reaction gas for the gas handling system by the graphite block reach to The top of deposition substrate;For the heating component for heating the graphite block, the graphite heating device assembly is described for decomposing Reaction gas and substrate to be deposited is made to reach reaction temperature.
Optionally, in equipment of the present invention, the heating component of the graphite heating device assembly includes heat shielding cover, heating Coil and temperature measuring equipment, the heating coil setting is in heat shielding cover inner sidewall, around graphite block, for heating the graphite Block, the temperature measuring equipment are used to monitor the temperature of the graphite block.
Optionally, in equipment of the present invention, the heating coil is intermediate frequency or radio frequency heating coil.
Optionally, in equipment of the present invention, the graphite block is column graphite block, and the deflector hole is along column graphite block Axial setting.
Optionally, in equipment of the present invention, the graphite block is pyrolytic graphite block.
Optionally, in equipment of the present invention, the other end of the graphite block is identical as fire end shape, for compensating temperature Degree;Alternatively, the fire end of the graphite block is equipped with the cooling fin for compensation temperature.
Optionally, in equipment of the present invention, the supporting surface of the sample stage of the sample stage component and substrate bottom to be deposited The shape in face is identical.
Optionally, in equipment of the present invention, the reaction gas of the gas handling system is the reaction gas of no hydrogen.
Optionally, in equipment of the present invention, the equipment further includes vacuum system, the graphite heating device assembly, institute The spray equipment of the sample stage and the gas handling system of stating sample stage component is respectively positioned in the vacuum chamber of the vacuum system.
Optionally, in equipment of the present invention, the equipment further includes electrical power control cabinet,
The electrical power control cabinet for controlling graphite heating device assembly, sample stage component, gas handling system and vacuum system respectively The power supply of system and the operation of technical process.
Compared with prior art, effect of the invention is as follows:
A kind of equipment of super Nano diamond of graphite heating chemical vapor deposition provided by the invention, the equipment both can be Special-shaped deposition on substrate film thickness, texture is consistent with performance, high quality super nanocrystalline diamond film, as high-intensitive, wear-resisting Protective film and functional film etc. can also manufacture the super nanocrystalline diamond components of polymorphic structure;Make up MPCVD and HFCVD equipment deposits the deficiency of super nanocrystalline diamond in special-shaped substrate surface.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention, And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects of the present invention, feature and advantage can It is clearer and more comprehensible, the followings are specific embodiments of the present invention.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art To obtain other drawings based on these drawings.
Fig. 1 is the graphite heating chemical vapor deposition that first embodiment of the invention, second embodiment and 3rd embodiment provide The structural principle block diagram of the equipment of the super Nano diamond of product;
Fig. 2 is the cross-sectional view for the graphite block that first embodiment of the invention provides;
Fig. 3 is the structural schematic diagram for the graphite block that second embodiment of the invention provides.
In attached drawing, 1 be heating coil, 2 be graphite block, 2-1 is fire end, 3 is deflector hole, 4 is heat shielding cover, 5 is survey Warm device, 6 be substrate to be deposited, 7 be sample stage, 8 be substrate temperature measuring equipment, 9 be mass flowmenter, 10 be control valve, 11 It is gas shower device for mixed gas pipeline, 12,13 be vacuum chamber, 14 be vacuum gauge, 15 is automatic pressure controller, 16 It is electrical power control cabinet for vacuum pump system, 17.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
In order to solve the problems in the prior art, the present invention provides a kind of super nanometer Buddha's warrior attendant of graphite heating chemical vapor deposition The equipment of stone, as shown in Figure 1, including graphite heating device assembly, sample stage component, gas handling system, vacuum system, power supply control Cabinet, the sample stage of sample stage component is for placing substrate 6 to be deposited;The substrate to be deposited can be non-planar or polymorphic structure; Gas handling system is connected with gas source, for providing reaction gas;Reaction gas is the reaction gas of no hydrogen, to avoid hydrogen atom pair The etching of graphite, the reaction gas include CH4With the mixed gas such as Ar, He and Ar.
Graphite heating device assembly thermally decomposes it for heating reaction gas, and heating substrate to be deposited make it is to be deposited Substrate reaches reaction temperature;Graphite heating device assembly includes graphite block 2 and heating component, as shown in Fig. 2, graphite block 2 is located at sample 7 top of sample stage of sample platform component, and the structure of the fire end 2-1 opposite with sample stage 7 and 6 upper surface shape of substrate to be deposited It is identical, make the distance of every bit on the fire end of graphite block 2 to substrate surface to be deposited it is all equal (mean error less than 0.1 milli Rice), the fire end 2-1 surface temperature difference of graphite block 2 is relatively small, and mean error is maintained within 10 DEG C, it can be ensured that different Shape deposition on substrate film thickness, texture is consistent with performance, high quality super nanocrystalline diamond, and it is heavy to solve substrate surface to be deposited The problem of inconsistency of the super nanocrystalline diamond of product.Several deflector holes 3 being uniformly arranged, the deflector hole 3 are offered on graphite block 2 For through-hole, deflector hole 3 reaches the top of substrate to be deposited for the reaction gas for gas handling system by graphite block;Heating component For heating graphite block.Graphite block is heated by heating component first, then again by heating after graphite block make to Deposition substrate reaches reaction temperature and decomposition reaction gas.The temperature of heating component can be increased to thousands of degree, such as: by CH4 Resolve into H2And carbon black.
Sample stage component includes bracket, sample stage 7 and substrate temperature measuring equipment for installing and fixing substrate to be deposited 8, sample stage 7 is arranged on bracket, and sample stage 7 is equipped with temperature detection hole, and substrate temperature measuring equipment 8 is installed by temperature detection hole On sample stage 7, the temperature for the substrate to be deposited 6 placed on test sample platform.
Gas handling system includes being respectively used to measure the mass flowmenter 9 of various gases, control valve 10, mixed gas pipeline 11 and gas shower device 12.Graphite heating device assembly is located at 12 lower section of gas shower device of gas handling system.
The spray equipment of graphite heating device assembly, the sample stage of sample stage component and gas handling system is respectively positioned on vacuum system In vacuum chamber.The vacuum system includes vacuum chamber 13, vacuum gauge 14, automatic pressure controller 15, high-vacuum pump, forvacuum Pump and valve, high-vacuum pump and forepump constitute vacuum pump system 16, and high-vacuum pump is only used for system and takes out in advance, growth course In only use forepump.Automatic pressure controller 15 makes the total pressure of diamond growth be maintained at setting numerically.
Electrical power control cabinet 17 for controlling graphite heating device assembly, sample stage component, gas handling system and vacuum system respectively Power supply and technical process operation and control etc. other control.
In one particular embodiment of the present invention, graphite block 2 is column graphite block, axis of the deflector hole along column graphite block To setting, further, graphite block 2 is pyrolytic graphite block, utilizes the high heat conductance of pyrolytic graphite, it is ensured that graphite heating end surfaces Temperature difference is kept in a certain range (less than 10 DEG C).The heating component of graphite heating device assembly includes heat shielding cover 4, heater wire Circle 1 and temperature measuring equipment 5, graphite block 2 are removably mounted in heat shielding cover 4, to be replaced according to the shape of substrate 6 to be deposited Graphite block 2;Heat shielding cover 4 is used for heat shield effect, and the setting of heating coil 1 should around graphite block in 4 inner sidewall of heat shielding cover Heating coil 1 can use spiral way or other modes, be located between 4 inside of heat shielding cover and graphite block 2, for heating State graphite block 2;Temperature measuring equipment 5 uses temperature thermocouple or other thermometric modes, the temperature for monitoring quantity graphite block 2.
Further: heating coil 1 is that intermediate frequency or radio frequency heating coil will be high using the eddy current effect of intermediate frequency or radio frequency Fine and close pyrolytic graphite block is heated to 2100 DEG C or so, and high efficiency heats graphite block, and reaction gas is made to be rapidly achieved thermal decomposition Temperature carries out the chemical vapor deposition of super nanocrystalline diamond, passes through the super Nano diamond of pyrolysis gas aggradation.
In another alternative embodiment of the invention, the supporting surface of sample stage 7 is identical as the shape of substrate bottom surface to be deposited, So as in close contact therewith, reach identical heat-conducting effect, keep substrate surface more uniform temperature to be deposited consistent, thus further Ensure to deposit that film thickness, texture is consistent with performance, super nanocrystalline diamond of high quality.
In another alternative embodiment of the invention, sample stage component can also use lift sample stage component, pass through The height of sample stage is adjusted to adjust graphite heating device assembly the distance between to substrate to be deposited.
The embodiment of the present invention propose equipment can not only process plane substrate to be deposited, can also process it is non-planar or Abnormity substrate to be deposited, and guarantee abnormity deposition on substrate texture to be deposited consistent with performance, high quality, relatively thin super receive The super nanocrystalline diamond components of rice diamond film or polymorphic structure.If preparing super nanocrystalline diamond components, It needs using the substrate to be deposited being easily removed, such as molybdenum and graphite substrate.
In the second embodiment of the present invention, the present invention provides a kind of super Nano diamond of graphite heating chemical vapor deposition Equipment, including graphite heating device assembly, sample stage component, gas handling system, vacuum system, electrical power control cabinet, sample stage component Sample stage 7 for placing substrate 6 to be deposited, which can be non-planar or polymorphic structure, gas handling system and gas Source is connected, and for providing reaction gas, reaction gas is the reaction gas of no hydrogen, to avoid hydrogen atom to the etching of graphite, The reaction gas includes CH4With the mixed gas such as Ar, He and Ar.
Graphite heating device assembly thermally decomposes it for heating reaction gas, and heating substrate to be deposited make it is to be deposited Substrate reaches reaction temperature, and graphite heating device assembly includes graphite block 2 and heating component, as shown in figure 3, graphite block 2 is located at sample 7 top of sample stage of sample platform component, and the structure of the fire end 2-1 opposite with sample stage 7 and 6 upper surface shape of substrate to be deposited It is identical, make the distance of every bit on the fire end of graphite block 2 to substrate surface to be deposited it is all equal (mean error less than 0.1 milli Rice), 2 fire end surface temperature difference of graphite block is relatively small, and mean error is maintained within 1O DEG C, it can be ensured that in special-shaped substrate Upper deposition film thickness, texture is consistent with performance, high quality super nanocrystalline diamond, solves that substrate surface deposition to be deposited is super to be received The problem of inconsistency of rice diamond;The other end of graphite block 2 is identical as fire end shape, if being used for substrate table to be deposited Face pattern rise and fall the excessive and temperature difference it is larger when (more than 10 DEG C), adjusted using temperature-compensating;It is offered on graphite block 2 several The deflector hole 3 being uniformly arranged, the deflector hole 3 are through-hole, and deflector hole 3 is used to pass through graphite block 2 for the reaction gas of gas handling system Reach the top of substrate 6 to be deposited;Heating component decomposes the reaction gas and substrate to be deposited for heating graphite block 2 Reach reaction temperature.Heating graphite block by heating component makes substrate to be deposited reach reaction temperature and decomposition reaction gas Temperature.
Sample stage component includes bracket, sample stage 7 and substrate temperature measuring equipment for installing and fixing substrate to be deposited 8, sample stage 7 is arranged on bracket, and sample stage 7 is equipped with temperature detection hole, and substrate temperature measuring equipment 8 is installed by temperature detection hole On sample stage 7, for monitoring the temperature for the substrate to be deposited placed on sample stage.
Gas handling system includes being respectively used to measure the mass flowmenter 9 of various gases, control valve 10, mixed gas pipeline 11 and gas shower device 12.Graphite heating device assembly is located at 12 lower section of gas shower device of gas handling system.
The spray equipment of graphite heating device assembly, the sample stage of sample stage component and gas handling system is respectively positioned on vacuum system In vacuum chamber.The vacuum system includes vacuum chamber 13, vacuum gauge 14, automatic pressure controller 15, high-vacuum pump, forvacuum Pump and valve, high-vacuum pump and forepump constitute vacuum pump system 16, and high-vacuum pump is only used for system and takes out in advance, growth course In only use forepump.Automatic pressure controller 15 makes the total pressure of diamond growth be maintained at setting numerically.
Electrical power control cabinet 17 for controlling graphite heating device assembly, sample stage component, gas handling system and vacuum system respectively Power supply and technical process operation and control etc. other control.
In one particular embodiment of the present invention, graphite block 2 is column graphite block, axis of the deflector hole along column graphite block To setting, further, graphite block 2 is pyrolytic graphite block.The heating component of graphite heating device assembly includes heat shielding cover 4, adds Heat coil 1 and temperature measuring equipment 5, graphite block 2 are removably mounted in heat shielding cover 4, so as to according to the shape of substrate to be deposited Replace graphite block;Heat shielding cover 4 is used for heat shield effect, and heating coil 1 is arranged in 4 inner sidewall of heat shielding cover, heater wire ring Around graphite block, which can use spiral way or other modes, be located between 4 inside of heat shielding cover and graphite block 2, For heating graphite block;Temperature measuring equipment 5 uses temperature thermocouple, for monitoring the temperature of graphite block.
Further: heating coil 1 is that intermediate frequency or radio frequency heating coil will be high using the eddy current effect of radio frequency or intermediate frequency Fine and close pyrolytic graphite block is heated to 2100 DEG C or so, passes through the super Nano diamond of pyrolysis gas aggradation.
In another alternative embodiment of the invention, the supporting surface of sample stage 7 is identical as the shape of substrate bottom surface to be deposited, So as in close contact therewith, reach identical heat-conducting effect.
In another alternative embodiment of the invention, sample stage component can also use lift sample stage component, pass through The height of sample stage is adjusted to adjust graphite heating device assembly the distance between to substrate to be deposited.
The equipment that the embodiment of the present invention proposes may insure in non-planar or special-shaped deposition on substrate film thickness to be deposited, knit Structure is consistent with performance, high quality super nanocrystalline diamond.
In the third embodiment of the present invention, the present invention provides a kind of super Nano diamond of graphite heating chemical vapor deposition Equipment, as shown in Figure 1, include graphite heating device assembly, sample stage component, gas handling system, vacuum system, electrical power control cabinet, For the sample stage of sample stage component for placing substrate 6 to be deposited, which can be non-planar or polymorphic structure, into Gas system is connected with gas source, and for providing reaction gas, reaction gas is the reaction gas of no hydrogen, to avoid hydrogen atom to stone The etching of ink, which includes CH4With the mixed gas such as Ar, He and Ar.
Graphite heating device assembly thermally decomposes it for heating reaction gas, and heating substrate to be deposited make it is to be deposited Substrate reaches reaction temperature, and graphite heating device assembly includes graphite block 2 and heating component, and graphite block 2 is located at sample stage component The top of sample stage 7, and and the opposite fire end of sample stage 7 structure it is identical as 6 upper surface shape of substrate to be deposited, make graphite block The distance of every bit is all equal (mean error is less than 0.1 millimeter) on 2 fire end to substrate surface to be deposited, graphite block heating End surfaces temperature difference is relatively small, and mean error is maintained within 1O DEG C, it can be ensured that in special-shaped deposition on substrate film thickness, texture Consistent with performance, high quality super nanocrystalline diamond solves substrate surface to be deposited and deposits super nanocrystalline diamond not Consistency problem.The fire end of graphite block 2 is equipped with the cooling fin for compensation temperature, which is arranged in temperature higher position, (more than 10 DEG C) when if excessive for substrate surface pattern to be deposited fluctuating, the temperature difference is larger, adjusted using temperature-compensating Section;Several deflector holes 3 being uniformly arranged are offered on graphite block 2, which is through-hole, and deflector hole 3 is used for for gas handling system Reaction gas the top of substrate to be deposited is reached by graphite block;Heating component makes the reaction gas for heating graphite block Body decomposes and substrate to be deposited reaches reaction temperature.Heating graphite block by heating component makes substrate to be deposited reach reaction temperature The temperature of degree and decomposition reaction gas.
Sample stage component includes bracket, sample stage 7 and substrate temperature measuring equipment for installing and fixing substrate to be deposited 8, sample stage 7 is arranged on bracket, and sample stage 7 is equipped with temperature detection hole, and substrate temperature measuring equipment 8 is installed by temperature detection hole On sample stage 7, for monitoring the temperature for the substrate to be deposited placed on sample stage.
Gas handling system includes being respectively used to measure the mass flowmenter 9 of various gases, control valve 10, mixed gas pipeline 11 and gas shower device 12.Graphite heating device assembly is located at 12 lower section of gas shower device of gas handling system.
The spray equipment of graphite heating device assembly, the sample stage of sample stage component and gas handling system is respectively positioned on vacuum system In vacuum chamber.The vacuum system includes vacuum chamber 13, vacuum gauge 14, automatic pressure controller 15, high-vacuum pump, forvacuum Pump and valve, high-vacuum pump and forepump constitute vacuum pump system 16, and high-vacuum pump is only used for system and takes out in advance, growth course In only use forepump.Automatic pressure controller 15 makes the total pressure of diamond growth be maintained at setting numerically.
Electrical power control cabinet 17 for controlling graphite heating device assembly, sample stage component, gas handling system and vacuum system respectively Power supply and technical process operation and control etc. other control.
In one particular embodiment of the present invention, graphite block 2 is column graphite block, axis of the deflector hole along column graphite block To setting, further, graphite block 2 is pyrolytic graphite block.The heating component of graphite heating device assembly includes heat shielding cover 4, adds Heat coil 1 and temperature measuring equipment 5, graphite block 2 are removably mounted in heat shielding cover 4, so as to according to the shape of substrate to be deposited Replace graphite block;Heat shielding cover 4 is used for heat shield effect, and heating coil 1 is arranged in 4 inner sidewall of heat shielding cover, heater wire ring Around graphite block, which can use spiral way or other modes, be located between 4 inside of heat shielding cover and graphite block 2, For heating graphite block;Temperature measuring equipment 5 uses temperature thermocouple, for monitoring the temperature of graphite block.
Further: heating coil 1 is that intermediate frequency or radio frequency heating coil will be high using the eddy current effect of radio frequency or intermediate frequency Fine and close pyrolytic graphite block is heated to 2100 DEG C or so, passes through the super Nano diamond of pyrolysis gas aggradation.
In another alternative embodiment of the invention, the supporting surface of sample stage 7 is identical as the shape of substrate bottom surface to be deposited, So as in close contact therewith, reach identical heat-conducting effect.
In another alternative embodiment of the invention, sample stage component can also use lift sample stage component, pass through The height of sample stage is adjusted to adjust graphite heating device assembly the distance between to substrate to be deposited.
The equipment that the embodiment of the present invention proposes may insure in non-planar or special-shaped deposition on substrate film thickness to be deposited, knit Structure is consistent with performance, high quality super nanocrystalline diamond.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies Within, then the present invention is also intended to include these modifications and variations.

Claims (10)

1. a kind of equipment of the super Nano diamond of graphite heating chemical vapor deposition, including sample stage component and gas handling system, institute The sample stage of sample stage component is stated for placing substrate to be deposited, for providing reaction gas, feature exists the gas handling system In, further includes: graphite heating device assembly,
The graphite heating device assembly includes graphite block and heating component, and the graphite block is located at the sample of the sample stage component Above platform, and and the opposite fire end of sample stage structure it is identical as substrate upper surface shape to be deposited;It is opened on the graphite block Equipped with several deflector holes, the deflector hole is used to pass through graphite block arrival for the reaction gas of the gas handling system to be deposited Substrate;The heating component for heating the graphite block, the graphite heating device assembly for decompose the reaction gas and Substrate to be deposited is set to reach reaction temperature.
2. equipment according to claim 1, which is characterized in that the heating component of the graphite heating device assembly includes heat shielding Cover, heating coil and temperature measuring equipment are covered, the heating coil is arranged in heat shielding cover inner sidewall, for heating the graphite block, The temperature measuring equipment is used to monitor the temperature of the graphite block.
3. equipment according to claim 2, which is characterized in that the heating coil is intermediate frequency or radio frequency heating coil.
4. equipment according to claim 1 or 2, which is characterized in that the graphite block is column graphite block, the deflector hole Along the axial direction setting of column graphite block.
5. equipment according to claim 1 or 2, which is characterized in that the graphite block is pyrolytic graphite block.
6. equipment according to claim 1 or 2, which is characterized in that the other end of the graphite block and fire end shape phase Together, it is used for compensation temperature;Alternatively, the fire end of the graphite block is equipped with the cooling fin for compensation temperature.
7. equipment according to claim 1, which is characterized in that the supporting surface of the sample stage of the sample stage component with to heavy The shape of product substrate bottom surface is identical.
8. equipment according to claim 1, which is characterized in that the reaction gas of the gas handling system is the reaction of no hydrogen Gas.
9. equipment according to claim 1, which is characterized in that the equipment further includes vacuum system,
The spray equipment of the graphite heating device assembly, the sample stage of the sample stage component and the gas handling system is respectively positioned on institute It states in the vacuum chamber of vacuum system.
10. according to claim 1 or equipment described in 9, which is characterized in that the equipment further includes electrical power control cabinet,
The electrical power control cabinet for controlling graphite heating device assembly, sample stage component, gas handling system and vacuum system respectively The operation of power supply and technical process.
CN201810299894.7A 2018-04-04 2018-04-04 The equipment of the super Nano diamond of graphite heating chemical vapor deposition Pending CN110344021A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115466940B (en) * 2022-08-15 2023-10-20 中国电子科技集团公司第十二研究所 Diamond-based microwave body attenuation material, preparation and application

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