CN104630879A - Method for preparing black phosphorus monocrystal from high-purity red phosphorus under atmospheric pressure - Google Patents
Method for preparing black phosphorus monocrystal from high-purity red phosphorus under atmospheric pressure Download PDFInfo
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- CN104630879A CN104630879A CN201510090509.4A CN201510090509A CN104630879A CN 104630879 A CN104630879 A CN 104630879A CN 201510090509 A CN201510090509 A CN 201510090509A CN 104630879 A CN104630879 A CN 104630879A
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Abstract
The invention provides a method for preparing black phosphorus monocrystal from high-purity red phosphorus under atmospheric pressure, which comprises the following steps: sufficiently mixing the raw material high-purity red phosphorus with AuSn and SnI4, sealing in a quartz tube, heating in a single-temperature-area furnace, keeping the temperature for some time, cooling to a certain temperature at a certain rate, and quickly cooling to obtain the black phosphorus monocrystal.
Description
Technical field
High-purity red phosphorus is utilized to prepare the method for black phosphorus monocrystalline under the present invention relates to a kind of normal pressure.
Background technology
Black phosphorus is the allotropic substance of the stable phosphorus of a kind of thermal property at normal temperatures and pressures, is normally under high pressure heated by white phosphorus and obtains.The laminate structure that the structure of black phosphorus and Graphene are very similar, and phonon, photon and electronics show the anisotropy of height in stratiform black phosphorus plane, make black phosphorus have important using value in fields such as Two-dimensional electron Infrared Opto-electronics.The preparation of monocrystal material, also referred to as the growth of crystal, is the reactant that the non-crystalline state of material, polycrystalline state maybe can be formed this material changes monocrystalline into process by the means of certain chemistry.The preparation method of monocrystalline usually can be divided into melt growth, solution growth and grow mutually.Melt growth method prepares the most frequently used and most important method of the monocrystalline of large single crystal and specified shape, has that fast growth, crystal grain are large, purity high.
Summary of the invention
In order to black phosphorus monocrystalline can be prepared safer, more easily, high-purity red phosphorus under the invention provides a kind of normal pressure, is utilized to prepare the method for black phosphorus monocrystalline.The technical solution adopted for the present invention to solve the technical problems is: with high-purity red phosphorus for starting material, with AuSn and SnI
4after abundant mixing, be together sealed in silica tube, be placed in the heating of single warm area stove and after constant temperature for some time, after being down to certain temperature with certain rate of temperature fall, more rapidly cooling obtains black phosphorus monocrystalline.
The invention has the beneficial effects as follows: compare traditional black phosphorus preparation method, former material is safer, operate easier, can carry out at ambient pressure.
Embodiment: the 1. SnI taking high-purity red phosphorus of 500mg, AuSn and 10mg of 364mg
4, fully to pour into after mixing in the one section of silica tube being about 12cm and to seal.
2. the silica tube of good seal is placed in single warm area stove, by the centre having one end of medicine to be placed on stove.
3. heat single warm area stove, within 10 hours, be warming up to 873K, and 873K constant temperature 24 hours.
4. with the rate of temperature fall of 40K/ hour, single warm area stove is cooled to 773K.
5. single warm area stove is down to normal temperature fast, takes out silica tube, black phosphorus monocrystalline can be obtained at the cold junction of silica tube.
Claims (3)
1. utilize high-purity red phosphorus to prepare a method for black phosphorus monocrystalline under normal pressure, it is characterized in that with high-purity red phosphorus, AuSn and SnI
4for starting material, in single warm area stove, obtain black phosphorus monocrystalline by series of steps such as heating, constant temperature, coolings.
2. utilize high-purity red phosphorus to prepare the method for black phosphorus monocrystalline under a kind of normal pressure according to claim 1, it is characterized in that the SnI of AuSn and 10mg of high-purity for 500mg red phosphorus, 364mg
4be sealed in the silica tube of 12 cm long.
3. utilize high-purity red phosphorus to prepare the method for black phosphorus monocrystalline under a kind of normal pressure according to claim 1, by series of steps such as heating, constant temperature, coolings in single warm area stove, single warm area stove is it is characterized in that to rise to 873K in 10 hours, constant temperature is down to normal temperature after cooling the temperature to 773K with 40K rate of temperature fall hourly after 24 hours fast, can obtain black phosphorus monocrystalline at the cold junction of silica tube.
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| CN201510090509.4A CN104630879A (en) | 2015-02-28 | 2015-02-28 | Method for preparing black phosphorus monocrystal from high-purity red phosphorus under atmospheric pressure |
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| CN201510090509.4A CN104630879A (en) | 2015-02-28 | 2015-02-28 | Method for preparing black phosphorus monocrystal from high-purity red phosphorus under atmospheric pressure |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116034A (en) * | 2015-09-08 | 2015-12-02 | 无锡百灵传感技术有限公司 | Sensor based on black phosphorus electrode and preparation method of sensor |
| CN105133009A (en) * | 2015-09-23 | 2015-12-09 | 清华大学 | Preparation method for orthorhombic crystal system black phosphorus monocrystalline |
| CN105460910A (en) * | 2015-11-19 | 2016-04-06 | 浙江大学 | A constant-temperature large-scale preparing method of belt-shaped black phosphorus |
| CN105565289A (en) * | 2016-01-29 | 2016-05-11 | 西北大学 | Black phosphorus and phosphinidene preparing methods |
| CN105603517A (en) * | 2016-01-11 | 2016-05-25 | 上海交通大学 | Method for growing monocrystal black phosphorus based on solid-source chemical vapor deposition method |
| WO2017020672A1 (en) * | 2015-08-06 | 2017-02-09 | 王贝贝 | Processing method of etching black phosphorus two-dimensional material using oxygen plasma |
| CN106498492A (en) * | 2016-11-01 | 2017-03-15 | 南京工业大学 | Method for preparing orthorhombic black phosphorus single crystal |
| CN106744754A (en) * | 2016-11-14 | 2017-05-31 | 深圳大学 | A kind of red phosphorus preprocess method prepared for black phosphorus |
| CN107188141A (en) * | 2017-07-10 | 2017-09-22 | 太原理工大学 | A kind of method that low temperature batch synthesizes black phosphorus nanometer sheet material |
| CN107285289A (en) * | 2016-04-01 | 2017-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus crystal, its preparation method and application with high photoelectric respone rate |
| CN108059138A (en) * | 2017-12-11 | 2018-05-22 | 昆明理工大学 | A kind of preparation method of high-purity black phosphorus |
| CN108538707A (en) * | 2018-03-05 | 2018-09-14 | 南京航空航天大学 | A kind of two dimension black phosphorus crystal preparation method |
| JP2019516650A (en) * | 2016-04-01 | 2019-06-20 | 中国科学院蘇州納米技術与納米▲ファン▼生研究所 | Black phosphorus crystal having high photoelectric response ratio, two-dimensional black phosphorus PN junction, method for producing the same and application thereof |
| WO2020262035A1 (en) * | 2019-06-27 | 2020-12-30 | 堺化学工業株式会社 | Production method for black phosphorus-containing composition and black phosphorus-containing composition |
| CN115522260A (en) * | 2022-10-31 | 2022-12-27 | 陕西科技大学 | Preparation method of high-stability black phosphorus single crystal |
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| CN102491294A (en) * | 2011-12-01 | 2012-06-13 | 东北师范大学 | Method for preparing black phosphorus of negative electrode materials of high-capacity lithium-ion battery |
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Patent Citations (1)
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| CN102491294A (en) * | 2011-12-01 | 2012-06-13 | 东北师范大学 | Method for preparing black phosphorus of negative electrode materials of high-capacity lithium-ion battery |
Non-Patent Citations (1)
| Title |
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| MARIAN CRISTIAN STAN, ET AL.: "Puzzling out the origin of the electrochemical activity of black P as a negative electrode material for lithium-ion batteries", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017020672A1 (en) * | 2015-08-06 | 2017-02-09 | 王贝贝 | Processing method of etching black phosphorus two-dimensional material using oxygen plasma |
| CN105116034A (en) * | 2015-09-08 | 2015-12-02 | 无锡百灵传感技术有限公司 | Sensor based on black phosphorus electrode and preparation method of sensor |
| CN105133009B (en) * | 2015-09-23 | 2017-09-26 | 清华大学 | A kind of preparation method of rhombic system black phosphorus monocrystalline |
| CN105133009A (en) * | 2015-09-23 | 2015-12-09 | 清华大学 | Preparation method for orthorhombic crystal system black phosphorus monocrystalline |
| CN105460910A (en) * | 2015-11-19 | 2016-04-06 | 浙江大学 | A constant-temperature large-scale preparing method of belt-shaped black phosphorus |
| CN105603517A (en) * | 2016-01-11 | 2016-05-25 | 上海交通大学 | Method for growing monocrystal black phosphorus based on solid-source chemical vapor deposition method |
| CN105565289A (en) * | 2016-01-29 | 2016-05-11 | 西北大学 | Black phosphorus and phosphinidene preparing methods |
| CN107285289A (en) * | 2016-04-01 | 2017-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus crystal, its preparation method and application with high photoelectric respone rate |
| JP2019516650A (en) * | 2016-04-01 | 2019-06-20 | 中国科学院蘇州納米技術与納米▲ファン▼生研究所 | Black phosphorus crystal having high photoelectric response ratio, two-dimensional black phosphorus PN junction, method for producing the same and application thereof |
| CN107285289B (en) * | 2016-04-01 | 2019-07-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus crystal, preparation method and application with high photoelectric respone rate |
| CN106498492A (en) * | 2016-11-01 | 2017-03-15 | 南京工业大学 | Method for preparing orthorhombic black phosphorus single crystal |
| CN106744754A (en) * | 2016-11-14 | 2017-05-31 | 深圳大学 | A kind of red phosphorus preprocess method prepared for black phosphorus |
| CN107188141A (en) * | 2017-07-10 | 2017-09-22 | 太原理工大学 | A kind of method that low temperature batch synthesizes black phosphorus nanometer sheet material |
| CN108059138A (en) * | 2017-12-11 | 2018-05-22 | 昆明理工大学 | A kind of preparation method of high-purity black phosphorus |
| CN108538707A (en) * | 2018-03-05 | 2018-09-14 | 南京航空航天大学 | A kind of two dimension black phosphorus crystal preparation method |
| CN108538707B (en) * | 2018-03-05 | 2020-04-24 | 南京航空航天大学 | Preparation method of two-dimensional black phosphorus crystal |
| WO2020262035A1 (en) * | 2019-06-27 | 2020-12-30 | 堺化学工業株式会社 | Production method for black phosphorus-containing composition and black phosphorus-containing composition |
| JP2021004161A (en) * | 2019-06-27 | 2021-01-14 | 堺化学工業株式会社 | Method for producing black phosphorus-containing composition and black phosphorus-containing composition |
| JP7248242B2 (en) | 2019-06-27 | 2023-03-29 | 堺化学工業株式会社 | Method for producing black phosphorus-containing composition and black phosphorus-containing composition |
| CN115522260A (en) * | 2022-10-31 | 2022-12-27 | 陕西科技大学 | Preparation method of high-stability black phosphorus single crystal |
| CN115522260B (en) * | 2022-10-31 | 2024-06-04 | 陕西科技大学 | Preparation method of high-stability black phosphorus single crystal |
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