CN111321462A - Substrate table for growing single crystal diamond by microwave plasma technology - Google Patents
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- CN111321462A CN111321462A CN201911273623.5A CN201911273623A CN111321462A CN 111321462 A CN111321462 A CN 111321462A CN 201911273623 A CN201911273623 A CN 201911273623A CN 111321462 A CN111321462 A CN 111321462A
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- 239000013078 crystal Substances 0.000 title claims abstract description 83
- 239000010432 diamond Substances 0.000 title claims abstract description 69
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 68
- 239000000758 substrate Substances 0.000 title claims abstract description 49
- 238000005516 engineering process Methods 0.000 title claims abstract description 10
- 230000012010 growth Effects 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 239000007789 gas Substances 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052799 carbon Inorganic materials 0.000 abstract description 18
- 238000000151 deposition Methods 0.000 description 9
- 230000008021 deposition Effects 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 238000005530 etching Methods 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 210000005239 tubule Anatomy 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000035040 seed growth Effects 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a substrate table for growing single crystal diamond by microwave plasma technology, which comprises a circular microwave plasma substrate table, wherein a spherical plasma excited by microwave is tightly attached to the surface of the substrate table above the substrate table, a pit is arranged at the axial symmetry center of the surface of the substrate table, and a crystal support for diamond growth can be placed in the pit. The bottom of the pit is supported by an annular metal thin tube around the crystal, the thin tube is provided with a small hole and is connected with a gas supply system, and the gas flow in the thin tube is controlled by a gas flowmeter. This scheme can avoid the accumulational non-diamond carbon in seed crystal side to influence the normal growth of seed crystal upper surface diamond.
Description
Technical Field
The invention belongs to the technical field of vacuum microelectronics, and particularly relates to a device for preparing single crystal diamond and a method for improving growth quality when the device is used for growing the single crystal diamond.
Background
Diamond, which is a high-quality single crystal diamond, has a wide application in many fields because of its excellent properties. The natural diamonds are rare in quantity and expensive in price; the artificial diamond prepared by the high temperature and high pressure method (HTHP method) also affects the properties of the diamond due to the metal catalyst; the Microwave Plasma Chemical Vapor Deposition (MPCVD) technology can grow high-quality single crystal diamond on the surface of a specific seed crystal, and is an ideal technology for artificial diamond growth.
The microwave plasma chemical vapor deposition device generally comprises a microwave system, a vacuum system, a gas supply system and a plasma reaction chamber, wherein a substrate table is arranged in the plasma reaction chamber, one or more pits are arranged on the upper surface of the substrate table, a crystal support is arranged in the center of each pit, and diamond seed crystals required by diamond growth are placed on the crystal support. The microwave generated by the microwave system enters the plasma reaction chamber, the gas provided by the gas supply system is excited above the substrate table to generate a plasma ball, the plasma ball is tightly attached to the surface of the seed crystal for diamond growth, and carbon deposition can be continuously formed on the surface of the diamond seed crystal by adjusting different reaction gases and adjusting the process parameters of the plasma, so that the diamond seed crystal grows from small to large.
The conventional way of introducing the reactive gas is to introduce the gas from the wall of the vacuum chamber so that the gas flows in the whole chamber and is in a relatively uniform flow state.
However, during the process of growing diamond on the surface of the diamond seed crystal, due to the difference of the atom arrangement structure of the upper surface and the side surface of the seed crystal, new diamond components are continuously deposited on the upper surface of the seed crystal, and meanwhile, a large amount of polycrystalline diamond and non-diamond carbon are generated on the side surface of the seed crystal, and the continuous accumulation of the polycrystalline diamond and the non-diamond carbon influences the growth of normal diamond components on the upper surface of the seed crystal. If the generation of polycrystalline diamond and non-diamond carbon on the side surface of the seed crystal can be inhibited or the generated polycrystalline diamond components and non-diamond carbon can be etched away in time in the growth process on the premise of not influencing the growth of the upper surface of the seed crystal, the method has great benefit for improving the normal deposition of the diamond components on the upper surface of the seed crystal. However, due to the uniqueness of the microwave, an air inlet pipe cannot be freely arranged inside the vacuum cavity. Since the pipe is generally made of metal, discharge is easily caused in the microwave electric field, and the metal affects the distribution of the microwave electric field. Therefore, in order not to affect the distribution of the electromagnetic field, the conventional vacuum chamber gas inlet is often disposed on the metal chamber wall.
Disclosure of Invention
The technical problem to be solved by the invention is to input a second path of gas into the vacuum cavity through the substrate table, besides introducing reaction gas into the traditional cavity wall on the premise of not changing the integral fluidity of the gas in the vacuum cavity, aiming at the defects in the prior art. The gas type of the second path gas can be the same as the traditional gas type or different from the traditional gas type. Because the second gas input point is very close to the diamond growth, when selecting the gas with different types from the traditional growth gas, a plasma active body concentration distribution area different from the whole growth environment can be formed in the local area around the diamond seed crystal growth. The invention provides a substrate table for growing single crystal diamond by microwave plasma technology, which comprises a circular microwave plasma substrate table, wherein a spherical plasma excited by microwave is tightly attached to the surface of the substrate table above the substrate table, a pit is arranged in the center of the substrate table tightly attached to a plasma ball, and a crystal support for diamond growth can be placed in the pit.
Alternatively, a cylindrical shape with a diameter or a truncated cone shape with a thick upper part and a thin lower part; the depth of the pits is between 4.0 and 12.0 millimeters, and the diameter of the pits is between 10.0 and 30.0 millimeters.
Optionally, the pit is one in the entire substrate table, at the center of the upper surface of the substrate table; or a plurality of the substrates are symmetrically distributed on the upper surface of the substrate platform by the center of the substrate platform.
Optionally, an annular metal thin tube arranged around the crystal support is arranged at the bottom of the inner close contact, 2 or more small holes are symmetrically distributed on the metal thin tube by taking the crystal support as the center, and the outer diameter of the metal thin tube is 1.5-2.5 mm.
Optionally, the small holes on the metal thin tube are used for releasing a specified single gas or a mixture of a plurality of gases, and the diameter of each small hole is 0.2-0.5 mm.
The invention also provides a microwave plasma technology growth method, which comprises any one of the substrate tables, wherein a microwave excited plasma is arranged above the substrate table, the microwave plasma technology growth method further comprises a microwave system, a vacuum system, a gas supply system and a plasma reaction chamber, wherein diamond seed crystals for diamond growth are placed on the crystal support, the crystal support is placed in the concave pits, metal thin tubes for gas outlet are arranged in the concave pits, the surfaces of the thin tubes are provided with a plurality of gas outlet holes which are symmetrically distributed by taking the crystal support as the center, and one gas or a mixture of a plurality of gases can be selectively released during work.
The invention provides a method for growing single crystal diamond components on the surface of a seed crystal by utilizing a microwave plasma CVD method. Set up annular metal tubule through the pit bottom placing the seed crystal, have the gas outlet on the tubule, through flowmeter control gas flow, pour into the side region of diamond growth in-process seed crystal with specific gas, arouse into the plasma state under the effect of microwave energy, can be selective restrain or etch the non-diamond carbon that produces of seed crystal side to guarantee that the diamond composition of seed crystal upper surface growth can guarantee high quality. Furthermore, through the composition and the flow of the second path of reaction gas which is selectively input, the non-diamond carbon generated on the side surface of the seed crystal can be etched in time more effectively, and the growth of polycrystalline diamond carbon is inhibited at the same time. The type of the reaction gas can be flexibly adjusted, and O is usually selected2Or a gas capable of decomposing O atoms in a plasma environment, such as H2O, CO and other gases, wherein the O-containing gas can generate a large amount of O free radicals in a plasma environment and has a very strong etching effect on non-diamond carbon and polycrystalline carbon; the resistance of the single crystal diamond carbon deposited on the upper surface of the diamond seed crystal to O etching is far greater than that of polycrystalline diamond carbon and non-diamond carbon; and the introduced O-containing gas continuously reacts with the polycrystalline carbon and the non-diamond carbon on the side surface of the seed crystal to gradually reduce the etching capability of the gas to the carbon in the process of moving from the bottom of the seed crystal to the upper part of the seed crystal, so that the etching capability to the carbon is basically exhausted when the gas reaches the vicinity of the upper surface of the seed crystal. The type and the introduction amount of the introduced second path of reaction gas can be measured by a gas mass flow meterAnd (6) adjusting. The whole process is simple to operate and has obvious effect.
Drawings
FIGS. 1A and 1B are schematic views showing arrangement of holes in pits of a substrate table, and arrangement of crystal supports and crystal seeds.
FIG. 2 shows that the inlet (a) of example 1 is not vented to O2A Raman spectrogram of the side surface of the seed crystal after growth; (b) general formula (I) O2Raman spectrum of the side surface of the seed crystal after growth.
Reference numerals: 1. plasma; 2. diamond seed crystals; 3. crystal support; 4. a metal thin tube; 5. a substrate stage; 6. a copper gas supply pipe; 7. a flow controller; 8. and an air outlet.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.
Referring to fig. 1A and 1B, an embodiment of the present invention includes a substrate stage (5) for microwave plasma deposition of diamond, the substrate stage (5) includes a circular microwave plasma (1), the substrate stage (5) has a pit in the center of its upper surface, a crystal holder (3) is placed in the pit, the height of the crystal holder ensures the upper surface of the diamond seed crystal to contact with the plasma, which is beneficial to diamond growth, a diamond seed crystal (2) is placed on the crystal holder, and the upper surface of the seed crystal is continuously deposited with diamond components, so as to realize diamond seed crystal growth, the pit is internally provided with a circular molybdenum metal thin tube, and the thin tube is provided with gas outlets which are distributed symmetrically with the crystal holder as the center; the air outlet (8) can selectively release O2The gas outlet direction faces the side wall of the pit, and the gas flowing out is more uniform through the rebound of the side wall, so that the influence on the uniform distribution of the plasma on the upper surface of the seed crystal is reduced; the flow rate of the gas flowing out of the gas hole is controlled by a flowmeter (7).
Example 1:
the diameter of the substrate table is 60 mm (5); a pit is arranged in the center of the substrate table, the diameter of the pit is 20 mm, and the depth of the pit is 4.0 mm; the outer diameter of the metal molybdenum thin tube (4) is 2.0 mm, the inner diameter of the metal molybdenum thin tube is 1.0 mm, 4 air outlet holes are symmetrically arranged by taking the crystal support as a center, the diameter of each air outlet hole is 0.5 mm, and the air outlet direction faces to the side wall of the pit. The crystal support (3) is high-purity metal tungsten with the diameter of 12 mm and the thickness of 3.5 mm. The diamond seed crystal (2) is a square diamond single crystal wafer with the geometric dimension of 5.0 x 0.2 mm.
The deposition process parameters of the diamond film are as follows: microwave power 4000W, deposition pressure 21.0kPa, H2And CH4The flow ratio of 200:3.0(sccm), the deposition temperature of 1060 ℃, and the gas released by the metal thin tube is O2The flow rate is as follows: 0(sccm), deposition time 8.0 h. (Note: sccm: standard cubic centimeters per minute).
The results were: the seed growth rate was 21.6 microns per hour; and detecting the components of the upper surface and the side surface of the grown seed crystal by using a Raman spectrum. The detection results are shown in FIG. 2 (a).
Example 2:
the diameter of the substrate table is 60 mm (5); a pit is arranged in the center of the substrate table, the diameter of the pit is 20 mm, and the depth of the pit is 4.0 mm; the outer diameter of the metal molybdenum thin tube (4) is 2.0 mm, the inner diameter of the metal molybdenum thin tube is 1.0 mm, 4 air outlet holes are symmetrically arranged by taking the crystal support as a center, the diameter of each air outlet hole is 0.5 mm, and the air outlet direction faces to the side wall of the pit. The crystal support (3) is high-purity metal tungsten with the diameter of 12 mm and the thickness of 3.5 mm. The diamond seed crystal (2) is a square diamond single crystal wafer with the geometric dimension of 5.0 x 0.2 mm.
The deposition process parameters of the diamond film are as follows: microwave power 4000W, deposition pressure 21.0kPa, H2And CH4The flow ratio of 200:3.0(sccm), the deposition temperature of 1060 ℃, and the gas released by the metal thin tube is O2The flow rate is as follows: 0.03(sccm), and a deposition time of 8.0 h.
The results were: the seed growth rate was 21.2 microns per hour; and detecting the components of the upper surface and the side surface of the grown seed crystal by using a Raman spectrum. The detection results are shown in FIG. 2 (b). As can be seen from a comparison of FIGS. 2(a) and 2(b), a small amount of O is introduced into the metal tubule in the pit2The growth of the upper surface of the seed crystal is basically not influenced, and the growth quality of the side surface of the seed crystal can be obviously improved.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A substrate table for growing single crystal diamond by microwave plasma technology is characterized in that: the diamond growth device comprises a circular microwave plasma substrate table, wherein a spherical plasma excited by microwaves is tightly attached to the surface of the substrate table above the substrate table, a pit is arranged in the center of the plasma table tightly attached to a plasma ball, and a crystal support for diamond growth can be placed in the pit.
2. The substrate table of claim 1, wherein: the concave pits are cylindrical or truncated cone-shaped with the same diameter from top to bottom or thick top and thin bottom; the depth of the pits is between 4.0 and 12.0 millimeters, and the diameter of the pits is between 10.0 and 30.0 millimeters.
3. The substrate table of claim 1, wherein: the concave pit is arranged on the whole substrate table and is positioned in the center of the upper surface of the substrate table; or a plurality of the substrates are symmetrically distributed on the upper surface of the substrate platform by the center of the substrate platform.
4. The substrate table of claim 1, wherein: an annular metal thin tube which is arranged around the crystal support is arranged in the pit and clings to the bottom, 2 or more small holes which are symmetrically distributed by taking the crystal support as the center are arranged on the metal thin tube, and the outer diameter of the metal thin tube is between 1.5 and 2.5 millimeters.
5. The substrate table of claim 4, wherein: the small holes on the metal thin tube are used for releasing specified single gas or mixture of a plurality of gases, and the diameter of the small holes is between 0.2 and 0.5 millimeter.
6. A method for growing by using microwave plasma technology is characterized in that: the substrate table comprises a substrate table according to any one of claims 1 to 5, wherein a microwave-excited plasma is arranged above the substrate table, and the substrate table further comprises a microwave system, a vacuum system, a gas supply system and a plasma reaction chamber, wherein diamond seed crystals for diamond growth are placed on a crystal support, the crystal support is placed in a pit, a metal thin tube for gas outlet is arranged in the pit, a plurality of gas outlet holes which are symmetrically distributed by taking the crystal support as a center are formed in the surface of the thin tube, and one gas or a mixture of a plurality of gases can be selectively released during operation.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111962048A (en) * | 2020-07-16 | 2020-11-20 | 上海征世科技有限公司 | Substrate table and equipment for microwave plasma equipment |
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JP2004060037A (en) * | 2002-07-31 | 2004-02-26 | Kobe Steel Ltd | Method for producing diamond and diamond product |
EP1555337A2 (en) * | 2004-01-16 | 2005-07-20 | Sumitomo Electric Industries, Ltd. | Diamond single crystal substrate manufacturing method and diamond single crystal substrate |
CN106048719A (en) * | 2016-07-08 | 2016-10-26 | 武汉大学 | Substrate holder and method for growing monocrystalline diamond |
CN108315816A (en) * | 2018-04-19 | 2018-07-24 | 武汉大学 | Single crystal diamond film method and apparatus |
CN108315817A (en) * | 2018-04-19 | 2018-07-24 | 武汉大学 | The growing method and device of efficient large size single crystal diamond |
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- 2019-12-12 CN CN201911273623.5A patent/CN111321462A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2004060037A (en) * | 2002-07-31 | 2004-02-26 | Kobe Steel Ltd | Method for producing diamond and diamond product |
EP1555337A2 (en) * | 2004-01-16 | 2005-07-20 | Sumitomo Electric Industries, Ltd. | Diamond single crystal substrate manufacturing method and diamond single crystal substrate |
CN106048719A (en) * | 2016-07-08 | 2016-10-26 | 武汉大学 | Substrate holder and method for growing monocrystalline diamond |
CN108315816A (en) * | 2018-04-19 | 2018-07-24 | 武汉大学 | Single crystal diamond film method and apparatus |
CN108315817A (en) * | 2018-04-19 | 2018-07-24 | 武汉大学 | The growing method and device of efficient large size single crystal diamond |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111962048A (en) * | 2020-07-16 | 2020-11-20 | 上海征世科技有限公司 | Substrate table and equipment for microwave plasma equipment |
CN111962048B (en) * | 2020-07-16 | 2021-08-20 | 上海征世科技股份有限公司 | Substrate table and equipment for microwave plasma equipment |
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