CN108315816B - Single crystal diamond film method and apparatus - Google Patents
Single crystal diamond film method and apparatus Download PDFInfo
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- CN108315816B CN108315816B CN201810353439.0A CN201810353439A CN108315816B CN 108315816 B CN108315816 B CN 108315816B CN 201810353439 A CN201810353439 A CN 201810353439A CN 108315816 B CN108315816 B CN 108315816B
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- resonant cavity
- ionization chamber
- single crystal
- ionization
- crystal diamond
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
Abstract
The present invention provides a kind of single crystal diamond film method and apparatus, can be realized the fast-growth of large size single crystal diamond.Single crystal diamond film method provided by the present invention, includes the following steps: for diamond substrate to be placed in resonant cavity；Reaction gas containing carbon source and hydrogen is passed through in ionization chamber and is adequately ionized, then the gas after ionization is passed through in resonant cavity and carries out microwave plasma CVD, on substrate fast-growth diamond.Device includes: vapor deposition portion, includes: for the resonant cavity of diamond epitaxial growth, being arranged in resonant cavity, the chip bench for placing diamond epitaxial substrate, and the microwave generator being connected with resonant cavity；And ionization part, include: the ionization chamber being connected with resonant cavity is separately positioned on the outlet end of ionization chamber and two pieces of electrodes of arrival end, and ionization chamber periphery is arranged in, carries out cooling cooling chamber to ionization chamber.
Description
Technical field
The invention belongs to diamond film preparation technical fields, and in particular to a kind of single crystal diamond film method and using should
Method grows the device of single-crystal diamond.
Background technique
Diamond has many distinguished performances as a kind of wide bandgap semiconductor materials, such as big forbidden bandwidth,
Low dielectric constant, high breakdown voltage, high electron hole mobility, high thermal conductivity and superior radiation resistance, and
Chemical stability is good.All these physics, chemically and electrically characteristic make diamond be likely to become the following high temperature, intense radiation etc.
The electronic device material to work under mal-condition.
From after the substance that discovery diamond in 1792 is made of carbon, people just persistently carry out artificial synthesized mechanism to it
Research, until 1954, GE company, the U.S. found that under 1700 DEG C of high temperature and the high pressure of 9.5GPa, graphite is through Fe base catalyst
Diamond can be transformed into, even grown up to large single crystal diamond scale from this high temperature and pressure (HPHT) diamond synthesis
?.1956 after 2 years, Russia had found another completely different method: low-temp low-pressure vapor phase synthetic diamond.1982
After year Matsumto et al. has invented chemical vapor deposition i.e. CVD method growing diamond membrane.It is many to having developed at present
The device and technique of kind CVD method growing diamond membrane, wherein mainly having: heat wire method, microwave method, oxygen-acetylene combustion flame
Method and direct-current plasma torch method.
Currently, domestic use MPCVD method, being all made of reduces microwave frequency and increase growth
The method of cavity size realizes the growth of large-area diamond film, using the method for improving microwave source power and methane concentration
To realize the fast-growth of diamond.For example, " a kind of increase gold disclosed in the Chinese patent of 106011781 A of Publication No. CN
The method of hard rock film deposition " increases the deposition of diamond film using making substrate do the method for quadrangle movement on sample stage
Area." large area high power microwave plasma ring shape microwave disclosed in the Chinese patent of 201947524 U of Publication No. CN
The device of chamber and its composition " expands reaction cavity, so that the depositional area of diamond reaches using the microwave source of 75kWBut its growth rate only has 4.1 μm/h.
Method disclosed above can effectively expand the depositional area of diamond film, rely primarily on and increase microwave power and shifting
Dynamic chip bench increases depositional area, but diamond film growth rate is low.
Summary of the invention
The present invention be to solve the above-mentioned problems and carry out, and it is an object of the present invention to provide a kind of single crystal diamond film method and
Device can be realized the fast-growth of large size single crystal diamond.
The present invention to achieve the goals above, uses following scheme:
<method>
The present invention provides a kind of single crystal diamond film method, which comprises the steps of: by diamond substrate
It is placed in resonant cavity；Reaction gas containing carbon source and hydrogen is passed through in ionization chamber and is adequately ionized, it then will ionization
Gas afterwards, which is passed through in resonant cavity, carries out microwave plasma CVD, on substrate fast-growth diamond.
Preferably, single crystal diamond film method according to the present invention can also have the following features: in resonant cavity
The working frequency for carrying out microwave plasma CVD is 915MHz, and power is 70~75kW, the vacuum in resonant cavity
Degree is 0.1Pa or more, and underlayer temperature is 800~1200 DEG C.
Preferably, single crystal diamond film method according to the present invention can also have the following features: reaction gas
In carbon source be methane CH4, methane CH4Account for 0.5%~2% (V/V) of reaction gas total amount.
Preferably, single crystal diamond film method according to the present invention can also have the following features: reaction gas
For the H of purity 99.999%2With the CH of purity 99.999%4。
Preferably, single crystal diamond film method according to the present invention can also have the following features: methane CH4It accounts for
1~2% (V/V) of reaction gas total amount, underlayer temperature are controlled at 900~1000 DEG C.
Preferably, single crystal diamond film method according to the present invention can also have the following features: ionization chamber
High voltage power supply be 1~100,000 volts of direct current uninterruptable powers or direct current pulse power sources, more preferably 5~100,000 volts；Direct current pulse power source
Pulse width is 10~20ms.
<device>
The present invention also provides a kind of single crystal diamond film devices characterized by comprising vapor deposition portion includes: using
In the resonant cavity of diamond epitaxial growth, it is arranged in resonant cavity, the chip bench for placing diamond epitaxial substrate, Yi Jiyu
The connected microwave generator of resonant cavity；And ionization part, include: the ionization chamber being connected with resonant cavity is separately positioned on ionization chamber
Outlet end and arrival end two pieces of electrodes, and be arranged in ionization chamber periphery, cooling cooling chamber is carried out to ionization chamber.
Preferably, single crystal diamond film device according to the present invention can also have the following features: microwave
Device is mounted on the top of resonant cavity, and ionization chamber is mounted on the lower section of resonant cavity, and the junction of ionization chamber and resonant cavity is equipped with
Sealing ring, the outlet of ionization chamber and entrance are arranged at the center position of electrode, and electrode is metal plate-like electrode, and cooling chamber is
Waterway, and outer wall is equipped with inlet and outlet.
Preferably, it can also have the following features: resonant cavity in single crystal diamond film device according to the present invention
Internal diameter be 360mm, the microwave operational frequencies of microwave generator are 915MHz, and ionization chamber is quartz chamber body, and the wall thickness of cavity is
5mm, cavity internal diameter are 50~100mm, and cavity length is 150~300mm, the outlet of ionization chamber and the diameter of entrance be 20~
40mm。
Preferably, single crystal diamond film device according to the present invention can also have the following features: ionization chamber
Internal diameter is 80mm, and cavity length 240mm, draw ratio 3:1, the outlet of ionization chamber and the diameter of entrance are 30mm, in this way
Effect is best.
The action and effect of invention
Single crystal diamond film method and apparatus of the invention, are placed on single-crystal diamond substrate the chip bench of resonant cavity
On, it is adequately ionized the mixed reaction gas such as methane and hydrogen in ionization chamber by high voltage electric field before entering microwave cavity, so
Enter resonant cavity afterwards, under the action of microwave energy, unionized gas molecule is ionized again, so that hydrocarbon active group
Concentration increases, to realize the purpose for accelerating single-crystal diamond fast-growth, and can be used to growing large-size single crystal diamond
Stone, the single-crystal diamond size prepared can reach 300mm, and the speed of growth is about 25-40 μm/h.To sum up, present invention introduces
Ionization method accelerates the growth rate of large size single crystal diamond, for diamond answering in electronics and optical device
With being of great significance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of single crystal diamond film device in embodiment one；
Fig. 2 is the structural schematic diagram of ionization part in embodiment one.
Specific embodiment
Single crystal diamond film method and apparatus according to the present invention are elaborated referring to the drawings.
<embodiment one>
As shown in Figure 1, single crystal diamond film device 10 includes vapor deposition portion 20, ionization part 30 and gas supply part 40.
Vapor deposition portion 20 is MPCVD equipment, it includes resonant cavity 21, chip bench 22 and microwave generator 23.
Resonant cavity 21 is used for diamond epitaxial growth, and 21 side lower of resonant cavity is equipped with exhaust outlet 21a, and exhaust outlet 21a is logical
Bellows 21b is crossed to connect with mechanical pump 21c；It, can will be intracavitary by mechanical pump 21c before being passed through gas into resonant cavity 21
Pressure is controlled in 0.1Pa or higher；Film silicon sensor 21d, electric current silicon sensor 21e and resistance are installed on bellows 21b
Silicon sensor 21f；Resonant cavity is also equipped with thermocouple sensor 21g on 21 side.
Chip bench 22 is erected in resonant cavity 21 by support frame 22a, and upper surface is for placing diamond epitaxial substrate
22b。
Microwave generator 23 includes waveguide mode converter 23a, waveguide 23b and microwave source 23c；Waveguide mode turns
Parallel operation 23a is arranged above resonant cavity 21, and waveguide mode converter 23a is connected by waveguide 23b with microwave source 23c.
In the present embodiment, the internal diameter of resonant cavity 21 is 360mm, and the microwave operational frequencies of microwave generator 23 are 915MHz.
Ionization part 30 includes 31, two pieces of metal plate-like electrodes 32 of ionization chamber and cooling chamber 33.
The lower entrances 31a of ionization chamber 31 is connected with gas supply part 40, upper outlet 31b by O-ring seal 31c with it is humorous
Vibration chamber 21 is connected, and in the present embodiment, ionization chamber 31 is quartz chamber body.Cavity internal diameter can be 50~100mm, and cavity length can
Think 150~300mm, the diameter of the entrance 31a and outlet 31b of ionization chamber 31 are 20~40mm.In the present embodiment, cavity
Wall thickness is 5mm, and the internal diameter of ionization chamber 31 is 80mm, cavity length 240mm, draw ratio 3:1, the entrance 31a of ionization chamber 31
Diameter with outlet 31b is 30mm, and setting effect in this way is best.In addition, the high voltage power supply that ionization chamber 31 uses can be straight
Uninterruptable power or direct current pulse power source are flowed, 31 high-voltage power voltage of ionization chamber is 1~100,000 volts, preferably 5~100,000 volts.
Two pieces of metal plate-like electrodes 32 are separately positioned on the outlet end and arrival end of ionization chamber 31, here metal plate-like electricity
Pole 32 can be the refractory metals electrodes such as tungsten, molybdenum, tantalum, rhenium and iridium.The center position of two pieces of metal plate-like electrodes 32 is all provided with
There is through hole, outlet 31b of the through hole for the metal plate-like electrode 32 being located above as ionization chamber 31；Underlying metal
Entrance 31a of the through hole of plate electrode 32 as ionization chamber 31.
The setting of cooling chamber 33 is in 31 periphery of ionization chamber, for being cooled down to ionization chamber 31, in the present embodiment, and cooling chamber 33
For waterway, and outer wall is equipped with inlet and outlet.
Gas supply part 40 includes air supply pipe 41, multiple gas source tanks 42 and multiple mass flowmenters 43.
The air supply opening of air supply pipe 41 is connected with the entrance 31a of ionization chamber 31.All gas source tanks 42 with air supply pipe 41
Collection port is connected.Mass flowmenter 43 is corresponded with 42 phase of gas source tank, and each mass flowmenter 43 is all disposed within a gas
On carrying shield 42, for monitoring throughput.In the present embodiment, the hydrogen H for being 99.999% equipped with purity in a gas source tank 422,
The methane CH for being 99.999% equipped with purity in another gas source tank 424。
<embodiment two>
Single-crystal diamond is grown using the method that ionization chamber 31 is combined with microwave plasma CVD, heavy
Before product, 10mm × 10mm × seeded growth face 0.5mm is polished first, then in strong acid mixed solution (concentrated hydrochloric acid: dense nitre
Acid=3:1) in plus hot acidizing 25min remove surface organic residue.Acid processing after respectively with acetone, dehydrated alcohol, go
Supersound washing 15min in ionized water, is finally used hot blast drying.Plasma etch conditions are as follows: microwave power 3000W, instead
Answer air pressure 20kPa, hydrogen flowing quantity: oxygen flow ratio is 300mL/min:9mL/min, 1000 DEG C of underlayer temperature or so, etches 2h.
The mixed gas of methane and hydrogen is passed through ionization chamber 31, reaction gas used in diamond film deposition is that purity is 99.999%
Hydrogen H2The methane CH for being 99.999% with purity4。H2Flow velocity is 500mL/min, CH4Flow velocity is 5mL/min, ionization chamber 31
Interior pressure is 20kPa, applies 50,000 volts of direct current continuous voltages at two pieces of 32 both ends of metal plate-like electrode, opens microwave source 23c and start
Deposition, microwave power supply 5kW, the speed of growth of single-crystal diamond are 30 μm/h.
<embodiment three>
Single-crystal diamond is grown using the method that ionization chamber 31 is combined with microwave plasma CVD, heavy
Before product, 10mm × 10mm × seeded growth face 0.5mm is polished first, then in strong acid mixed solution (concentrated hydrochloric acid: dense nitre
Acid=3:1) in plus hot acidizing 25min remove surface organic residue.Acid processing after respectively with acetone, dehydrated alcohol, go
Supersound washing 15min in ionized water, is finally used hot blast drying.Plasma etch conditions are as follows: microwave power 3000W, instead
Answer air pressure 20kPa, hydrogen flowing quantity: oxygen flow ratio is 300mL/min:9mL/min, 1000 DEG C of underlayer temperature or so, etches 2h.
By methane CH4With hydrogen H2Mixed gas be passed through ionization chamber 31, reaction gas used in diamond film deposition is that purity is
99.999% H2The CH for being 99.999% with purity4。H2Flow velocity is 500mL/min, CH4Flow velocity is 10mL/min, ionization chamber 31
Interior pressure is 30kPa, applies 100,000 volts of direct current continuous voltages at two pieces of 32 both ends of metal plate-like electrode, opens microwave source 23c and open
Begin deposition, microwave power supply 5kW, and the speed of growth of single-crystal diamond is 38 μm/h.
Above embodiments are only the illustration done to technical solution of the present invention.Single crystal diamond according to the present invention
Stone growing method and device are not merely defined in described structure in the embodiment above, but are limited with claim
Range subject to.Any modify or supplement or equivalent that those skilled in the art of the invention are done on the basis of the embodiment
Replacement, all in claim range claimed of the invention.
Claims (6)
1. a kind of single crystal diamond film method, which comprises the steps of:
Diamond substrate is placed in resonant cavity；Reaction gas containing carbon source and hydrogen is passed through in ionization chamber and is carried out sufficiently
Ionization；Then the gas after ionization is passed through in the resonant cavity and carries out microwave plasma CVD, on substrate
Fast-growth diamond,
Wherein, in the reaction gas, the carbon source is the methane CH of purity 99.999%4, methane CH4Account for the reaction gas
0.5%~2% (V/V) of body total amount, the purity of hydrogen are 99.999%,
The high voltage power supply of the ionization chamber is 1~100,000 volts of direct current uninterruptable powers or direct current pulse power sources, direct current pulse power source arteries and veins
Rushing width is 10~20ms,
The working frequency that microwave plasma CVD is carried out in the resonant cavity is 915MHz, power is 70~
75kW, for the vacuum degree in the resonant cavity in 0.1Pa or more, underlayer temperature is 800~1200 DEG C.
2. single crystal diamond film method according to claim 1, it is characterised in that:
Wherein, the methane CH4Account for 1~2% (V/V) of the reaction gas total amount, the underlayer temperature control 900~
1000℃。
3. a kind of single crystal diamond film device characterized by comprising
Vapor deposition portion includes: for the resonant cavity of diamond epitaxial growth, being arranged in the resonant cavity, for placing gold
The chip bench of hard rock epitaxial substrate, and the microwave generator being connected with the resonant cavity；With
Ionization part includes: the ionization chamber being connected with the resonant cavity, is separately positioned on outlet end and the entrance of the ionization chamber
Two pieces of electrodes at end, and the ionization chamber periphery is set, carries out cooling cooling chamber to the ionization chamber.
4. single crystal diamond film device according to claim 3, it is characterised in that:
Wherein, the microwave generator is mounted on the top of the resonant cavity,
The ionization chamber is mounted on the lower section of the resonant cavity, and the junction of the ionization chamber and the resonant cavity is equipped with close
Seal,
The outlet of the ionization chamber and entrance are arranged at the center position of the electrode,
The electrode is metal plate-like electrode,
The cooling chamber is waterway, and outer wall is equipped with inlet and outlet.
5. single crystal diamond film device according to claim 3, it is characterised in that:
Wherein, the internal diameter of the resonant cavity is 360mm, and the microwave operational frequencies of the microwave generator are 915MHz,
The ionization chamber is quartz chamber body, and the wall thickness of cavity is 5mm, and cavity internal diameter is 50~100mm, cavity length is 150~
300mm, the outlet of the ionization chamber and the diameter of entrance are 20~40mm.
6. single crystal diamond film device according to claim 3, it is characterised in that:
Wherein, the internal diameter of the ionization chamber be 80mm, cavity length 240mm, draw ratio 3:1,
The outlet of the ionization chamber and the diameter of entrance are 30mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810353439.0A CN108315816B (en) | 2018-04-19 | 2018-04-19 | Single crystal diamond film method and apparatus |
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| CN201810353439.0A CN108315816B (en) | 2018-04-19 | 2018-04-19 | Single crystal diamond film method and apparatus |
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| CN108315816B true CN108315816B (en) | 2019-06-25 |
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| CN110373651B (en) * | 2019-09-04 | 2023-07-04 | 成都道启弘环境科技有限公司 | Equipment for microwave plating of nano diamond film |
| CN110468449B (en) * | 2019-09-12 | 2021-09-07 | 宁波晨鑫维克工业科技有限公司 | Microwave plasma reactor for manufacturing single crystal diamond and diffusion device thereof |
| CN111321462A (en) * | 2019-12-12 | 2020-06-23 | 上海征世科技有限公司 | Substrate table for growing single crystal diamond by microwave plasma technology |
| CN111235634A (en) * | 2020-03-09 | 2020-06-05 | 上海三朗纳米技术有限公司 | Microwave plasma diamond growth equipment and application method thereof |
| CN111519248A (en) * | 2020-03-31 | 2020-08-11 | 上海征世科技有限公司 | Substrate table for growing single crystal diamond by microwave plasma technology and growing method |
| CN111437773A (en) * | 2020-04-21 | 2020-07-24 | 江苏卓远半导体有限公司 | Process for crystallizing diamond single crystal at high temperature by microwave gas |
| CN113088937B (en) * | 2021-03-01 | 2023-04-28 | 杭州超然金刚石有限公司 | Device for preparing monocrystalline diamond by microwave plasma CVD (chemical vapor deposition) with improved stability and monocrystalline diamond preparation method |
| CN113265649B (en) * | 2021-06-18 | 2024-02-06 | 航天科工(长沙)新材料研究院有限公司 | Flange for connecting MPCVD cavity and MPCVD device |
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| CN106400110A (en) * | 2016-08-31 | 2017-02-15 | 兰州空间技术物理研究所 | Polycrystalline diamond composite pressure sensing diaphragm, preparing method thereof and capacitance diaphragm vacuum gauge |
| CN106835069A (en) * | 2016-12-21 | 2017-06-13 | 武汉大学 | Semiconductor diamond film doping post-processing approach and device based on femtosecond laser |
| CN107675249B (en) * | 2017-09-08 | 2020-07-07 | 西安电子科技大学 | Diameter expanding growth method of single crystal diamond |
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