CN110230037A - Microwave plasma reaction unit and microwave plasma reaction system - Google Patents
Microwave plasma reaction unit and microwave plasma reaction system Download PDFInfo
- Publication number
- CN110230037A CN110230037A CN201810181821.8A CN201810181821A CN110230037A CN 110230037 A CN110230037 A CN 110230037A CN 201810181821 A CN201810181821 A CN 201810181821A CN 110230037 A CN110230037 A CN 110230037A
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- Prior art keywords
- microwave
- plasma reaction
- antenna
- reaction unit
- microwave plasma
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/276—Diamond only using plasma jets
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Plasma & Fusion (AREA)
- Physics & Mathematics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
A kind of microwave plasma reaction unit and microwave plasma reaction system provided by the invention, are related to diamond fabrication technical field, including device cavity;Device cavity includes upper cavity and lower chamber, and the top of lower chamber is arranged in upper cavity;Air inlet and at least one gas outlet are provided on device cavity;The first microwave reflection body and the second microwave reflection body are provided in upper cavity;The top of upper cavity is arranged in first microwave reflection body, and the inside of the first microwave reflection body is arranged in the second microwave reflection body;The bottom of lower chamber is provided with antenna outer conductor and antenna inner conductor;The inside of antenna outer conductor is arranged in antenna inner conductor;It is formed with deposition table at the top of antenna inner conductor, substrate is provided in deposition table, is provided with plasma on substrate.In the above-mentioned technical solutions, which can be improved the service ability of device when being used to manufacture diamond, carry out the synthesis of high quality diamond material under high power conditions.
Description
Technical field
The present invention relates to diamond fabrication technical fields, more particularly, to a kind of microwave plasma reaction unit and microwave
Plasma reaction system.
Background technique
Diamond has numerous extremely excellent performances, for example, it is with high hardness and room temperature thermal conductivity, phase
To wider forbidden band and spectral transmission range and good chemical stability and high anti-radiation threshold value, also, work as vacuum
When energy level is lower than conduction band lower end, diamond also has rare negative electron compatibility.These excellent performances make Buddha's warrior attendant
Stone material is all with a wide range of applications in various fields.
When diamond is applied to certain specific areas, it is necessary to have high qualities and biggish when such as semiconductor
Area.And MPCVD method is because have many advantages, such as electrodeless pollution, and deposition process is steadily controllable, and one
It is directly the first choice for preparing diamond both at home and abroad.
And the preparation of high-quality and large-area diamond material needs higher plasma density simultaneously, i.e. device should
With can under high power and high pressure technique reliability service ability.
But the device in the prior art for being used to prepare diamond is also unable to satisfy demand, is unable to reach reliable
Service ability, it is therefore desirable to the device of a kind of structure and perfect performance is designed, to meet the preparation of high quality diamond material.
Summary of the invention
The purpose of the present invention is to provide a kind of microwave plasma reaction unit and microwave plasma reaction systems, with solution
The device service ability insecure technical problem certainly existing in the prior art for preparing diamond.
A kind of microwave plasma reaction unit provided by the invention, including device cavity;
Described device cavity includes upper cavity and lower chamber, and the top of the lower chamber is arranged in the upper cavity;
Air inlet and at least one gas outlet are provided on described device cavity;
The first microwave reflection body and the second microwave reflection body are provided in the upper cavity;The first microwave reflection body is set
It sets at the top of the upper cavity, the inside of the first microwave reflection body is arranged in the second microwave reflection body;
The bottom of the lower chamber is provided with antenna outer conductor and antenna inner conductor;The antenna inner conductor is arranged described
The inside of antenna outer conductor;
It is formed with deposition table at the top of the antenna inner conductor, substrate is provided in the deposition table, is set on the substrate
It is equipped with plasma.
In the above-mentioned technical solutions, which, can when being used to manufacture diamond
It solves quartz material and is easy etching, device is not easy to adjust, be not easy water cooling and vacuum is not easy the defects of keeping, and then dress can be improved
The service ability set carries out the synthesis of high quality diamond material under high power conditions.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes coaxial inner conductor
And coaxial outer conductor;
The bottom of the antenna outer conductor is arranged in the coaxial outer conductor;The coaxial inner conductor is arranged described
The inside of coaxial outer conductor, and the coaxial inner conductor is connect with the bottom of the antenna inner conductor.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes the first regulating mechanism;
First regulating mechanism is connect with the first microwave reflection body, for adjusting the first microwave reflection body
Position.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes the second regulating mechanism;
Second regulating mechanism is connect with the second microwave reflection body, for adjusting the second microwave reflection body
Position.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further include medium window and or
Support ring;
The medium window is arranged between the top of the antenna inner conductor and the antenna outer conductor;
The medium window is arranged between the bottom of the antenna inner conductor and the antenna outer conductor.
Further, in an embodiment of the present invention, excessive inclined-plane, the mistake are formed at the top of the antenna inner conductor
Degree inclined-plane is located at around the deposition table.
Further, in an embodiment of the present invention, the inside of the second microwave reflection body is arranged in the air inlet,
And it is stretched out from the top of the upper cavity.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes inlet tube;
The inlet tube is connected on the air inlet.
Further, in an embodiment of the present invention, the outer wall of the lower chamber is arranged in the gas outlet.
The present invention also provides a kind of microwave plasma reaction systems, including the microwave plasma reaction unit.
In the above-mentioned technical solutions, the microwave plasma reaction system uses the microwave plasma reaction unit,
The microwave plasma reaction unit is able to solve quartz material and is easy etching, device when being used to manufacture diamond
It is not easy to adjust, is not easy water cooling and vacuum is not easy the defects of keeping, and then the service ability of device can be improved, in high power conditions
The lower synthesis for carrying out high quality diamond material.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the first structure diagram of microwave plasma reaction unit provided by one embodiment of the present invention;
Fig. 2 is the second structural schematic diagram of microwave plasma reaction unit provided by one embodiment of the present invention;
Fig. 3 is the third structural schematic diagram of microwave plasma reaction unit provided by one embodiment of the present invention;
Fig. 4 is the 4th structural schematic diagram of microwave plasma reaction unit provided by one embodiment of the present invention.
Appended drawing reference:
1- upper cavity;2- lower chamber;3- antenna outer conductor;
The gas outlet 4-;5- medium window;6- coaxial inner conductor;
7- coaxial outer conductor;8- the second microwave reflection body;9- the first microwave reflection body;
The first regulating mechanism of 10-;The second regulating mechanism of 11-;12- air inlet;
13- plasma;14- substrate;The excessive inclined-plane 15-;
16- antenna inner conductor;17- deposition table;18- support ring.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected;It can
To be mechanical connection, it is also possible to be electrically connected;It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
Fig. 1 is the first structure diagram of microwave plasma reaction unit provided by one embodiment of the present invention;Such as Fig. 1 institute
Show, a kind of microwave plasma reaction unit provided in this embodiment, including device cavity;
Described device cavity includes upper cavity 1 and lower chamber 2, and the top of the lower chamber 2 is arranged in the upper cavity 1;
Air inlet 12 and at least one gas outlet 4 are provided on described device cavity;
The first microwave reflection body 9 and the second microwave reflection body 8 are provided in the upper cavity 1;First microwave reflection
The top of the upper cavity 1 is arranged in body 9, and the second microwave reflection body 8 is arranged in the first microwave reflection body 9
Portion;
The bottom of the lower chamber 2 is provided with antenna outer conductor 3 and antenna inner conductor 16;The antenna inner conductor 16 is arranged
In the inside of the antenna outer conductor 3;
The top of the antenna inner conductor 16 is formed with deposition table 17, and substrate 14 is provided in the deposition table 17, described
Plasma 13 is provided on substrate 14.
In the above-mentioned technical solutions, which, can when being used to manufacture diamond
It solves quartz material and is easy etching, device is not easy to adjust, be not easy water cooling and vacuum is not easy the defects of keeping, and then dress can be improved
The service ability set carries out the synthesis of high quality diamond material under high power conditions.
When specifically used, illustrated with specific embodiment, can choose using diameter is 50mm, with a thickness of 5mm,
The monocrystalline silicon substrate 14 for being oriented to (100) is used as 14 material of substrate.
Before manufacture, the diadust that partial size is 20 μm is first used to grind 14 material of substrate, then respectively using going
Ionized water and dehydrated alcohol are cleaned by ultrasonic 20 minutes, are then placed on 17 face of the deposition table of device cavity.
Then cooling circulating water is opened, water cooling is carried out to device using cooling water, and use vacuum pump by plasma 13
The air pressure of chamber be extracted into 1Pa or less.
It is passed through two kinds of unstrpped gases of hydrogen and methane again, wherein selectable hydrogen flowing quantity is 300sccm, methane flow
For 9sccm.The intracorporal gas pressure of regulating device chamber, which reaches 500Pa, to be advisable.
The microwave that frequency is 2.45GHz, power 800W is inputted, again for exciting the plasma above the substrate 14
Body 13.
Finally, the first microwave reflection body 9 and the second microwave reflection body 8 are adjusted, so that the plasma 13
The uniform distribution above the substrate 14.
Adjustable gas pressure and microwave power respectively reach 14kPa and 6kW at this time, selectable, deposit 100 hours
Afterwards, orderly close-down unstrpped gas, microwave power supply and vacuum pump terminate deposition.
And the step of being manufactured using above-described embodiment, having obtained diamond, that hydrofluoric acid and nitric acid can be used is mixed
It closes liquid and washes off silicon materials, and then obtain self-supporting diamond thin film.
The diamond thin that the embodiment obtains found after measuring diamond film deposition rate can achieve 3.6 μm/it is small
When, scanning electron microscope shows diamond film surface topography even compact.It is only deposited at 1332cm-1 during Raman test display Raman is general
In diamond characteristic peak, occur without apparent impurity peaks, the halfwidth of diamond characteristic peak is only 2.2cm-1, this shows institute
The diamond film of preparation has excellent quality.
It can be preparation so carrying out the manufacture of diamond using microwave plasma reaction unit described above
Process provides stable service ability, and then carries out the synthesis of high quality diamond material under high power conditions.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes coaxial inner conductor 6
With coaxial outer conductor 7;
The bottom of the antenna outer conductor 3 is arranged in the coaxial outer conductor 7;The setting of coaxial inner conductor 6 exists
The inside of the coaxial outer conductor 7, and the coaxial inner conductor 6 is connect with the bottom of the antenna inner conductor 16.
Fig. 4 is the 4th structural schematic diagram of microwave plasma reaction unit provided by one embodiment of the present invention;Such as Fig. 4 institute
Show, in an embodiment of the present invention, the microwave plasma reaction unit further includes the first regulating mechanism 10;
First regulating mechanism 10 is connect with the first microwave reflection body 9, for adjusting first microwave reflection
The position of body 9.
Utilize the position of the adjustable first microwave reflection body 9 of first regulating mechanism 10, wherein also include institute
The upper and lower position (as shown in the direction of Fig. 1) for stating the first microwave reflection body 9, this makes it possible to according to preparation process needs, so that
The plasma 13 uniform distribution above the substrate 14.
Further, in an embodiment of the present invention, the microwave plasma reaction unit further includes the second regulating mechanism
11;
Second regulating mechanism 11 is connect with the second microwave reflection body 8, for adjusting second microwave reflection
The position of body 8.
Utilize the position of the adjustable second microwave reflection body 8 of second regulating mechanism 11, wherein also include institute
The upper and lower position (as shown in the direction of Fig. 1) for stating the second microwave reflection body 8, this makes it possible to according to preparation process needs, so that
The plasma 13 uniform distribution above the substrate 14.
Fig. 2 is the second structural schematic diagram of microwave plasma reaction unit provided by one embodiment of the present invention;Fig. 3 is this
The third structural schematic diagram for the microwave plasma reaction unit that invention one embodiment provides;As shown in Figure 3 and Figure 4, in this hair
In bright embodiment, the microwave plasma reaction unit further includes 5 He of medium window or support ring 18;
The medium window 5 is arranged between the top of the antenna inner conductor 16 and the antenna outer conductor 3;
The medium window 5 is arranged between the bottom of the antenna inner conductor 16 and the antenna outer conductor 3.
The antenna inner conductor 16 can be fixed using the medium window 5 and the support ring 18, then
Guarantee that the antenna inner conductor 16 is more stable relative to the position of the antenna outer conductor 3.
Further, in an embodiment of the present invention, the top of the antenna inner conductor 16 is formed with excessive inclined-plane 15, institute
Excessive inclined-plane 15 is stated to be located at around the deposition table 17.
Selectable, in an embodiment of the present invention, the air inlet 12 is arranged in the second microwave reflection body 8
Portion, and stretched out from the top of the upper cavity 1.
Selectable, in an embodiment of the present invention, the microwave plasma reaction unit further includes that air inlet 12 is managed;
12 pipe of air inlet is connected on the air inlet 12.
Selectable, in an embodiment of the present invention, the outer wall of the lower chamber 2 is arranged in the gas outlet 4.
The present invention also provides a kind of microwave plasma reaction systems, including the microwave plasma reaction unit.
Since specific structure, the principle of work and power and the technical effect of the microwave plasma reaction unit are detailed above
It states, just repeats no more herein.
So any technology contents about the microwave plasma reaction unit, can refer to above for described
The record of microwave plasma reaction unit.
From the foregoing, it will be observed that the microwave plasma reaction system uses the microwave plasma reaction unit, the microwave etc.
Ionic reaction device is able to solve quartz material and is easy etching when being used to manufacture diamond, device is not easy to adjust,
It is not easy water cooling and vacuum is not easy the defects of keeping, and then the service ability of device can be improved, carry out under high power conditions high
The synthesis of quality diamond material.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of microwave plasma reaction unit, which is characterized in that including device cavity;
Described device cavity includes upper cavity and lower chamber, and the top of the lower chamber is arranged in the upper cavity;
Air inlet and at least one gas outlet are provided on described device cavity;
The first microwave reflection body and the second microwave reflection body are provided in the upper cavity;The first microwave reflection body setting exists
The inside of the first microwave reflection body is arranged in the top of the upper cavity, the second microwave reflection body;
The bottom of the lower chamber is provided with antenna outer conductor and antenna inner conductor;The antenna inner conductor is arranged in the antenna
The inside of outer conductor;
It is formed with deposition table at the top of the antenna inner conductor, substrate is provided in the deposition table, is provided on the substrate
Plasma.
2. microwave plasma reaction unit according to claim 1, which is characterized in that further include coaxial inner conductor and same
Axis outer conductor;
The bottom of the antenna outer conductor is arranged in the coaxial outer conductor;The coaxial inner conductor setting is described coaxial
The inside of line outer conductor, and the coaxial inner conductor is connect with the bottom of the antenna inner conductor.
3. microwave plasma reaction unit according to claim 1, which is characterized in that further include the first regulating mechanism;
First regulating mechanism is connect with the first microwave reflection body, for adjusting the position of the first microwave reflection body
It sets.
4. microwave plasma reaction unit according to claim 1, which is characterized in that further include the second regulating mechanism;
Second regulating mechanism is connect with the second microwave reflection body, for adjusting the position of the second microwave reflection body
It sets.
5. microwave plasma reaction unit according to claim 1, which is characterized in that further include medium window and or branch
Pushing out ring;
The medium window is arranged between the top of the antenna inner conductor and the antenna outer conductor;
The medium window is arranged between the bottom of the antenna inner conductor and the antenna outer conductor.
6. microwave plasma reaction unit according to claim 1, which is characterized in that the top shape of the antenna inner conductor
At there is excessive inclined-plane, the excessive inclined-plane is located at around the deposition table.
7. microwave plasma reaction unit according to claim 1, which is characterized in that air inlet setting is described the
The inside of two microwave reflection bodies, and stretched out from the top of the upper cavity.
8. microwave plasma reaction unit according to claim 7, which is characterized in that further include inlet tube;
The inlet tube is connected on the air inlet.
9. microwave plasma reaction unit according to claim 1, which is characterized in that the gas outlet is arranged under described
The outer wall of cavity.
10. a kind of microwave plasma reaction system, which is characterized in that including microwave as claimed in any one of claims 1-9 wherein
Plasma reaction device.
Priority Applications (1)
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CN201810181821.8A CN110230037A (en) | 2018-03-06 | 2018-03-06 | Microwave plasma reaction unit and microwave plasma reaction system |
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CN201810181821.8A CN110230037A (en) | 2018-03-06 | 2018-03-06 | Microwave plasma reaction unit and microwave plasma reaction system |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111286713A (en) * | 2020-02-17 | 2020-06-16 | 北京科技大学 | High-efficiency treatment method and device for diamond micro powder |
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JPH09148097A (en) * | 1995-11-22 | 1997-06-06 | Hitachi Ltd | Plasma producing device, manufacture of semiconductor element using it, and semiconductor element |
CN101864560A (en) * | 2010-05-24 | 2010-10-20 | 北京科技大学 | High power microwave plasma diamond film deposition device |
CN103668127A (en) * | 2013-12-10 | 2014-03-26 | 北京科技大学 | Domical microwave plasma chemical vapor deposition diamond film device |
CN103695865A (en) * | 2013-12-13 | 2014-04-02 | 北京科技大学 | TM021 modal high-power microwave plasma diamond film deposition device |
CN104388910A (en) * | 2014-12-13 | 2015-03-04 | 太原理工大学 | High-power microwave plasma reaction unit for chemical vapor deposition of diamond films |
-
2018
- 2018-03-06 CN CN201810181821.8A patent/CN110230037A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09148097A (en) * | 1995-11-22 | 1997-06-06 | Hitachi Ltd | Plasma producing device, manufacture of semiconductor element using it, and semiconductor element |
CN101864560A (en) * | 2010-05-24 | 2010-10-20 | 北京科技大学 | High power microwave plasma diamond film deposition device |
CN103668127A (en) * | 2013-12-10 | 2014-03-26 | 北京科技大学 | Domical microwave plasma chemical vapor deposition diamond film device |
CN103695865A (en) * | 2013-12-13 | 2014-04-02 | 北京科技大学 | TM021 modal high-power microwave plasma diamond film deposition device |
CN104388910A (en) * | 2014-12-13 | 2015-03-04 | 太原理工大学 | High-power microwave plasma reaction unit for chemical vapor deposition of diamond films |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111286713A (en) * | 2020-02-17 | 2020-06-16 | 北京科技大学 | High-efficiency treatment method and device for diamond micro powder |
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Application publication date: 20190913 |