CN115125614A - Technology for recycling carbon source gasified by hairs in process of growing diamond by MPCVD method - Google Patents
Technology for recycling carbon source gasified by hairs in process of growing diamond by MPCVD method Download PDFInfo
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- CN115125614A CN115125614A CN202210875318.9A CN202210875318A CN115125614A CN 115125614 A CN115125614 A CN 115125614A CN 202210875318 A CN202210875318 A CN 202210875318A CN 115125614 A CN115125614 A CN 115125614A
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- mpcvd
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- carbon source
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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
- 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
Abstract
The invention discloses a technology for recycling a hair gasified carbon source in a process of growing diamond by an MPCVD method, which comprises the following production steps: the method comprises the following steps: hair material treatment, step two: gasifying the hair to prepare a carbon source, and performing step three: and preparing the diamond. Compared with the traditional production method using high-purity methane gas as the carbon source, the technology for recycling the carbon source gasified by the hairs in the process of growing the diamonds by the MPCVD method not only greatly reduces the price, but also has no danger in use and does not need to comply with strict use specifications because the hair raw materials are convenient to collect and have huge quantity and do not need to be transported and stored by using professional equipment, thereby simplifying the production steps and reducing the production cost.
Description
Technical Field
The invention relates to the technical field of diamond growth by an MPCVD method, in particular to a technology for recycling a hair gasification carbon source in the process of growing diamond by the MPCVD method.
Background
MPCVD (Microwave Plasma Chemical Vapor Deposition), the word abbreviation of Microwave Plasma Chemical Vapor Deposition, is the Chinese meaning Microwave Plasma Chemical Vapor Deposition, is the most widely applied method for preparing single crystal diamond at home and abroad at present, can prepare diamond with large area and high quality, and the prepared diamond is used as missile hood, optical infrared window and the like and is widely applied in the fields of semiconductors, 5G communication, war industry and the like.
The carbon source used in the traditional MPCVD method for growing the diamond is generally high-purity methane gas, needs to be prepared and purchased, is expensive, has high transportation and storage cost, needs to comply with strict use specifications, and has certain potential safety hazard in use.
Therefore, there is a need to devise a technique for recycling carbon sources gasified by hair during the growth of diamond by the MPCVD method, which addresses the above problems.
Disclosure of Invention
The invention aims to provide a technology for recycling a carbon source gasified by hair in the process of growing diamond by an MPCVD (multi-phase chemical vapor deposition) method, and aims to solve the problems that the carbon source used in the traditional MPCVD method for growing diamond is generally high-purity methane gas, needs to be purchased and reported, is expensive, has high transportation and storage cost, needs to comply with strict use specifications, and has certain potential safety hazard in use.
In order to achieve the purpose, the invention provides the following technical scheme: the technology for recycling the carbon source gasified by the hairs in the process of growing the diamonds by the MPCVD method comprises the following production steps:
the method comprises the following steps: hair material treatment
Taking a proper amount of hair raw materials, cleaning and drying the hair raw materials by using deionized water, soaking the hair raw materials for a long time by using ethanol and acetone solutions in sequence, taking out the hair raw materials and airing the hair raw materials, bundling the hair raw materials into a plurality of small bundles, and placing the small bundles in a negative pressure storage device for later use.
Step two: carbon source preparation by gasifying hair
1) Placing a plurality of small hair bundles on a lower substrate table in an MPCVD furnace at intervals of 3-5 mm;
2) firstly, filling nitrogen into an MPCVD furnace, discharging air, filling the MPCVD furnace with the nitrogen, closing a discharge valve and an inflation valve, pumping out the nitrogen in the MPCVD furnace through a built-in vacuumizing mechanism of the MPCVD furnace, then controlling the vacuumizing mechanism to stop working, filling the hydrogen into the MPCVD furnace through the inflation valve, starting a microwave generating device after the air pressure in the MPCVD furnace is recovered to normal atmospheric pressure, generating hydrogen plasma in the MPCVD furnace through electron cyclotron resonance discharge, starting a chemical vapor deposition mechanism, and using a magnetic field to control high-energy hydrogen plasma to bombard hair bundles arranged on a lower substrate table so as to vaporize the hair, thereby obtaining a mixed gas carbon source;
3) and pumping out the mixed gas carbon source in the MPCVD furnace by using negative pressure storage equipment, and removing impurities and purifying for later use.
Step three: preparation of diamond
1) Selecting natural single-crystal diamond with a proper size as a substrate, placing the substrate on a lower substrate table in another MPCVD furnace, closing the MPCVD furnace, vacuumizing the MPCVD furnace, then connecting a negative pressure storage device storing a gas carbon source with the MPCVD furnace, filling the gas carbon source into the MPCVD furnace, starting a chemical vapor deposition mechanism, and enabling carbon atoms in the gas carbon source to normally grow on the natural single-crystal diamond substrate under the constraint of a magnetic field;
2) and after observing that the artificial diamond on the diamond substrate grows to a sufficient volume through the observation window, controlling the MPCVD furnace to stop working, taking out the natural single crystal diamond substrate and the artificial diamond growing on the natural single crystal diamond substrate, and cutting and separating the natural single crystal diamond substrate and the artificial diamond to obtain an artificial diamond product.
Preferably, in the step one
Soaking the hair material in ethanol and acetone solution for more than 5 min;
the diameter of the small bundle bundled by the hair materials is 1.5-2.5 mm.
Preferably, in said step two
The pressure in the MPCVD furnace needs to be less than or equal to 0.1 x 10 after the nitrogen is pumped out -3 MPa；
The working temperature in the MPCVD furnace is more than or equal to 1200 ℃.
Preferably, said step three is
After the artificial diamond on the diamond substrate grows to be enough in volume, stopping magnetic field restriction, starting the vacuumizing device, pumping out residual gas carbon source in the MPCVD furnace, storing the carbon source in the negative pressure storage device, recycling the carbon source in the next artificial diamond production process, then opening the air valve, and enabling air to enter the MPCVD furnace until the other parts in the MPCVD furnace are recovered to be normal atmospheric pressure.
Compared with the prior art, the invention has the beneficial effects that: compared with the traditional production method using high-purity methane gas as the carbon source, the technology for recycling the carbon source gasified by the hairs in the process of growing the diamonds by the MPCVD method not only greatly reduces the price, but also has no danger in use and does not need to comply with strict use specifications because the hair raw materials are convenient to collect and have huge quantity and do not need to be transported and stored by using professional equipment, thereby simplifying the production steps and reducing the production cost.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a technical scheme that:
the technology for recycling the carbon source gasified by the hairs in the process of growing the diamonds by the MPCVD method comprises the following production steps:
the method comprises the following steps: hair material treatment
Taking a proper amount of hair raw materials, cleaning and drying the hair raw materials by using deionized water, sequentially soaking the hair raw materials by using ethanol and acetone solution for more than or equal to 5min, taking out and airing, bundling the hair raw materials into a plurality of small bundles, wherein the diameter of the small bundles bundled by the hair raw materials is 1.5-2.5mm, and placing the small bundles in a negative pressure storage device for later use.
Step two: carbon source preparation by gasifying hair
1) Placing a plurality of small hair bundles on a lower substrate table in an MPCVD furnace at intervals of 3-5 mm;
2) firstly, filling nitrogen into the MPCVD furnace, discharging air, filling nitrogen into the MPCVD furnace, closing a discharge valve and an inflation valve, pumping out the nitrogen from the MPCVD furnace through a built-in vacuum pumping mechanism of the MPCVD furnace, wherein the air pressure in the MPCVD furnace is less than or equal to 0.1 multiplied by 10 after the nitrogen is pumped out -3 Controlling the vacuumizing mechanism to stop working, filling hydrogen into the MPCVD furnace through the charging valve, starting the microwave generating device after the air pressure in the MPCVD furnace is recovered to normal atmospheric pressure, and discharging through electron cyclotron resonanceAt the moment, the working temperature in the MPCVD furnace is more than or equal to 1200 ℃, hydrogen plasma is generated in the MPCVD furnace, a chemical vapor deposition mechanism is started, the high-energy hydrogen plasma is controlled by a magnetic field to bombard hair bundles arranged on a lower substrate table, and the hair is vaporized to obtain a mixed gas carbon source;
3) and pumping out the mixed gas carbon source in the MPCVD furnace by using negative pressure storage equipment, and removing impurities and purifying for later use.
Step three: preparation of diamond
1) Selecting natural single-crystal diamond with a proper size as a substrate, placing the substrate on a lower substrate table in another MPCVD furnace, closing the MPCVD furnace, vacuumizing the MPCVD furnace, then connecting a negative pressure storage device storing a gas carbon source with the MPCVD furnace, filling the gas carbon source into the MPCVD furnace, starting a chemical vapor deposition mechanism, and enabling carbon atoms in the gas carbon source to normally grow on the natural single-crystal diamond substrate under the constraint of a magnetic field;
2) and after observing that the artificial diamond on the diamond substrate grows to a sufficient volume through the observation window, controlling the MPCVD furnace to stop working, starting a vacuumizing device, pumping out residual gas carbon source in the MPCVD furnace, storing the carbon source in a negative pressure storage device, recycling the carbon source in the next artificial diamond production process, then opening an air valve, allowing air to enter the MPCVD furnace until other parts in the MPCVD furnace return to normal atmospheric pressure, taking out the natural single crystal diamond substrate and the artificial diamond growing on the natural single crystal diamond substrate, and cutting and separating the natural single crystal diamond substrate and the artificial diamond to obtain an artificial diamond product.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The technology for recycling the carbon source gasified by the hairs in the process of growing the diamond by the MPCVD method is characterized in that: the technology for recycling the gasified carbon source of the hair in the process of growing the diamond by the MPCVD method comprises the following production steps:
the method comprises the following steps: hair material treatment
Taking a proper amount of hair raw materials, cleaning and drying the hair raw materials by using deionized water, soaking the hair raw materials for a long time by using ethanol and acetone solutions in sequence, taking out the hair raw materials and airing the hair raw materials, bundling the hair raw materials into a plurality of small bundles, and placing the small bundles in a negative pressure storage device for later use.
Step two: carbon source preparation by gasifying hair
1) Placing a plurality of small hair bundles on a lower substrate table in an MPCVD furnace at intervals of 3-5 mm;
2) firstly, filling nitrogen into an MPCVD furnace, discharging air, filling the MPCVD furnace with the nitrogen, closing a discharge valve and an inflation valve, pumping out the nitrogen in the MPCVD furnace through a built-in vacuum pumping mechanism of the MPCVD furnace, then controlling the vacuum pumping mechanism to stop working, filling hydrogen into the MPCVD furnace through the inflation valve, starting a microwave generating device after the air pressure in the MPCVD furnace is recovered to normal atmospheric pressure, generating hydrogen plasma in the MPCVD furnace through electron cyclotron resonance discharge, starting a chemical vapor deposition mechanism, and utilizing a magnetic field to control high-energy hydrogen plasma to bombard hair bundles arranged on a lower substrate table so as to vaporize the hair, thereby obtaining a mixed gas carbon source;
3) and pumping out the mixed gas carbon source in the MPCVD furnace by using negative pressure storage equipment, and removing impurities and purifying for later use.
Step three: preparation of diamond
1) Selecting natural single-crystal diamond with proper size as a substrate, placing the natural single-crystal diamond on a lower substrate table in another MPCVD furnace, closing the MPCVD furnace, vacuumizing the MPCVD furnace, then connecting a negative pressure storage device in which a gas carbon source is stored with the MPCVD furnace, filling the gas carbon source into the MPCVD furnace, starting a chemical vapor deposition mechanism, and enabling carbon atoms in the gas carbon source to normally grow on the natural single-crystal diamond substrate under the constraint of a magnetic field;
2) and after observing that the artificial diamond on the diamond substrate grows to a sufficient volume through the observation window, controlling the MPCVD furnace to stop working, taking out the natural single crystal diamond substrate and the artificial diamond growing on the natural single crystal diamond substrate, and cutting and separating the natural single crystal diamond substrate and the artificial diamond to obtain an artificial diamond product.
2. The technology for recycling carbon sources gasified by hair in the process of growing diamonds by the potential MPCVD method according to claim 1, wherein: in the step one
Soaking the hair material in ethanol and acetone solution for more than 5 min;
the diameter of the small bundle bundled by the hair materials is 1.5-2.5 mm.
3. The technology for recycling carbon sources gasified by hair in the process of growing diamonds by the potential MPCVD method according to claim 1, wherein: in the second step
The pressure in the MPCVD furnace needs to be less than or equal to 0.1 x 10 after the nitrogen is pumped out -3 MPa；
The working temperature in the MPCVD furnace is more than or equal to 1200 ℃.
4. The technology for recycling carbon sources gasified by hair in the process of growing diamonds by the potential MPCVD method according to claim 1, wherein: in the third step
After the artificial diamond on the diamond substrate grows to be enough in volume, stopping magnetic field restriction, starting the vacuumizing device, pumping out residual gas carbon source in the MPCVD furnace, storing the carbon source in the negative pressure storage device, recycling the carbon source in the next artificial diamond production process, then opening the air valve, and enabling air to enter the MPCVD furnace until the other parts in the MPCVD furnace are recovered to be normal atmospheric pressure.
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| CN202210875318.9A CN115125614A (en) | 2022-07-21 | 2022-07-21 | Technology for recycling carbon source gasified by hairs in process of growing diamond by MPCVD method |
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| CN202210875318.9A CN115125614A (en) | 2022-07-21 | 2022-07-21 | Technology for recycling carbon source gasified by hairs in process of growing diamond by MPCVD method |
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Citations (7)
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|---|---|---|---|---|
| US20100242834A1 (en) * | 2009-03-31 | 2010-09-30 | Rajneesh Bhandari | Method for producing single crystalline diamonds |
| JP2013001601A (en) * | 2011-06-16 | 2013-01-07 | National Institute For Materials Science | Method and apparatus for growing diamond crystal |
| CN105296959A (en) * | 2015-11-24 | 2016-02-03 | 武汉工程大学 | Method for synthesizing diamond by using human body hair as carbon source |
| CN107937980A (en) * | 2017-12-01 | 2018-04-20 | 武汉工程大学 | A kind of method for going out single-crystal diamond using human hair as carbon source for growth by the use of double chip bench MPCVD reaction units |
| CN108070842A (en) * | 2017-12-15 | 2018-05-25 | 武汉工程大学 | The method for using MPCVD methods growth single-crystal diamond as carbon source based on hairline |
| CN110565064A (en) * | 2018-06-05 | 2019-12-13 | 甘志银 | novel diamond material growth method |
| CN112877773A (en) * | 2021-01-13 | 2021-06-01 | 哈尔滨工业大学 | Non-air-flow MPCVD single crystal diamond growth method using solid carbon source |
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2022
- 2022-07-21 CN CN202210875318.9A patent/CN115125614A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100242834A1 (en) * | 2009-03-31 | 2010-09-30 | Rajneesh Bhandari | Method for producing single crystalline diamonds |
| JP2013001601A (en) * | 2011-06-16 | 2013-01-07 | National Institute For Materials Science | Method and apparatus for growing diamond crystal |
| CN105296959A (en) * | 2015-11-24 | 2016-02-03 | 武汉工程大学 | Method for synthesizing diamond by using human body hair as carbon source |
| CN107937980A (en) * | 2017-12-01 | 2018-04-20 | 武汉工程大学 | A kind of method for going out single-crystal diamond using human hair as carbon source for growth by the use of double chip bench MPCVD reaction units |
| CN108070842A (en) * | 2017-12-15 | 2018-05-25 | 武汉工程大学 | The method for using MPCVD methods growth single-crystal diamond as carbon source based on hairline |
| CN110565064A (en) * | 2018-06-05 | 2019-12-13 | 甘志银 | novel diamond material growth method |
| CN112877773A (en) * | 2021-01-13 | 2021-06-01 | 哈尔滨工业大学 | Non-air-flow MPCVD single crystal diamond growth method using solid carbon source |
Non-Patent Citations (2)
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| 张永宏主编: "《现代薄膜材料与技术》", 西北工业大学出版社, pages: 187 * |
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