CN107032310A - A kind of preparation method of N doping phosphorus alkene - Google Patents
A kind of preparation method of N doping phosphorus alkene Download PDFInfo
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- CN107032310A CN107032310A CN201710495556.6A CN201710495556A CN107032310A CN 107032310 A CN107032310 A CN 107032310A CN 201710495556 A CN201710495556 A CN 201710495556A CN 107032310 A CN107032310 A CN 107032310A
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- phosphorus alkene
- alkene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses a kind of preparation method of N doping phosphorus alkene, including：Phosphorus alkene is placed in plasma gas phase deposition equipment, and pressure is evacuated to for below 5Pa, again nitrogenous gas is filled with into the gas ions vapor deposition apparatus, until the internal pressure of the gas ions vapor deposition apparatus is 100~1000Pa, then 200~1000 DEG C are warming up in 1~60min, and phosphorus 1~360min of alkene is bombarded under 5~500W of radio-frequency power, room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.The present invention can be by nitrogen-doping into phosphorus alkene, make phosphorus alkene that there is good antioxygenic property, not only the physical and chemical performance of phosphorus alkene will not be destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can use the fields such as electronic communication, communications and transportation extensively.
Description
Technical field
The present invention relates to phosphorus alkene field of compound material, more particularly to a kind of preparation method of N doping phosphorus alkene.
Background technology
Phosphorus alkene material is new two-dimentional phosphorus nano material, and its special stable micro-structure makes it have excellent electrification
Performance and heat-conductive characteristic are learned, therefore phosphorus alkene material has broad prospect of application in fields such as electronic communication, communications and transportation.
The environmental stability of phosphorus alkene is poor, and the stronger chemism of phosphorus atoms makes it easily be corroded by materials such as oxygen gas and waters
And original performance is lost, and strict protection must be carried out by equipment or other method when in use, otherwise can be rapid because of erosion
Decompose, this makes it significantly be limited in actual use.In addition, the mechanical performance of phosphorus alkene is weaker, in practical application mistake
It is vulnerable to external force in journey and is destroyed.
In the prior art, the environment unstability (shortcoming for being oxidized easily erosion) to phosphorus alkene is not located well
Reason method, and there is not N doping phosphorus alkene and its synthetic method.
The content of the invention
, can the invention provides a kind of preparation method of N doping phosphorus alkene for above-mentioned weak point of the prior art
Into phosphorus alkene, to make phosphorus alkene have good antioxygenic property nitrogen-doping, not only the physical and chemical performance of phosphorus alkene will not
It is destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can use electronic communication, friendship extensively
The fields such as logical transport.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of N doping phosphorus alkene, including：Phosphorus alkene is placed in plasma gas phase deposition equipment, and takes out true
Sky to pressure is below 5Pa, then is filled with nitrogenous gas into the gas ions vapor deposition apparatus, until the ion vapor-phase deposition
The internal pressure of equipment is 100~1000Pa, is then warming up to 200~1000 DEG C in 1~60min, and radio-frequency power 5~
Phosphorus 1~360min of alkene is bombarded under 500W, room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.
Preferably, described nitrogenous gas is at least one of ammonia, nitrogen, nitric oxide, nitrogen dioxide.
Preferably, into gas ions vapor deposition apparatus, the flow of insufflation gas is 5~100sccm.
As seen from the above technical solution provided by the invention, the preparation method of N doping phosphorus alkene provided by the present invention
Phosphorus alkene is placed in plasma gas phase deposition equipment, and using radio-frequency power supply to containing in the plasma gas phase deposition equipment
Nitrogen is ionized, and phosphorus alkene is bombarded, while being controlled to heating-up temperature, internal pressure, radio-frequency power, bombardment time
System, so as to by nitrogen-doping into phosphorus alkene, form N doping phosphorus alkene；It is different from simple phosphorus alkene, in the N doping phosphorus alkene
Nitrogen-atoms can make it have good antioxygenic property, and ensure that the excellent physical and chemical performance of phosphorus alkene is not destroyed, still
With performances such as good electric conductivity, thermal conductivity, stability, flexibilities, therefore the preparation of N doping phosphorus alkene provided by the present invention
Method can not only be such that the physical and chemical performance of phosphorus alkene is not destroyed, and simple to operate, low for equipment requirements, product quality
Good, yield is high, and product can use the fields such as electronic communication, communications and transportation extensively.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the electron scanning micrograph of the N doping phosphorus alkene prepared by the embodiment of the present invention 1.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The preparation method to N doping phosphorus alkene provided by the present invention is described in detail below.
A kind of preparation method of N doping phosphorus alkene, including：Phosphorus alkene is placed in plasma gas phase deposition equipment, and takes out true
Empty is below 5Pa to pressure, then is filled with into the gas ions vapor deposition apparatus nitrogenous gas, the flows of insufflation gas for 5~
100sccm, until the internal pressure of the gas ions vapor deposition apparatus is 100~1000Pa, then heats up in 1~60min
Phosphorus 1~360min of alkene is bombarded to 200~1000 DEG C, and under 5~500W of radio-frequency power, room temperature is cooled to afterwards, so as to be made
N doping phosphorus alkene.
Wherein, described nitrogenous gas is at least one of ammonia, nitrogen, nitric oxide, nitrogen dioxide.
Specifically, phosphorus alkene is placed in plasma gas phase deposition and set by the preparation method of N doping phosphorus alkene provided by the present invention
In standby, and the nitrogenous gas in the plasma gas phase deposition equipment is ionized using radio-frequency power supply, phosphorus alkene is banged
Hit, while be controlled to heating-up temperature, internal pressure, radio-frequency power, bombardment time, so that by nitrogen-doping to phosphorus alkene
In, form N doping phosphorus alkene；Different from simple phosphorus alkene, the nitrogen-atoms in the N doping phosphorus alkene can make it have anti-well
Oxidation susceptibility, and ensure that the excellent physical and chemical performance of phosphorus alkene is not destroyed, still with good electric conductivity, thermal conductivity, steady
The performance such as qualitative, flexible, therefore the preparation method of N doping phosphorus alkene provided by the present invention can not only make the physical chemistry of phosphorus alkene
Performance will not be destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can use electronics extensively
The fields such as communication, communications and transportation.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The preparation method for the N doping phosphorus alkene that body embodiment is provided the embodiment of the present invention is described in detail.
Embodiment 1
A kind of preparation method of N doping phosphorus alkene, its specific steps can include：Phosphorus alkene is placed in into plasma chemical vapor to sink
In product equipment, and pressure is evacuated to for below 5Pa, then be filled with ammonia, insufflation gas into the gas ions vapor deposition apparatus
Flow be 5sccm, until the gas ions vapor deposition apparatus internal pressure be 100Pa, be then warming up in 60min
200 DEG C, and phosphorus alkene 360min is bombarded under radio-frequency power 5W, room temperature is cooled to afterwards, so that N doping as shown in Figure 1 is made
Phosphorus alkene.
Embodiment 2
A kind of preparation method of N doping phosphorus alkene, its specific steps can include：Phosphorus alkene is placed in into plasma chemical vapor to sink
In product equipment, and pressure is evacuated to for below 5Pa, then be filled with nitrogen, insufflation gas into the gas ions vapor deposition apparatus
Flow be 20sccm, until the gas ions vapor deposition apparatus internal pressure be 250Pa, be then warming up in 45min
400 DEG C, and phosphorus alkene 250min is bombarded under radio-frequency power 700W, room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.
Embodiment 3
A kind of preparation method of N doping phosphorus alkene, its specific steps can include：Phosphorus alkene is placed in into plasma chemical vapor to sink
In product equipment, and pressure is evacuated to for below 5Pa, then is filled with nitric oxide into the gas ions vapor deposition apparatus, be filled with
The flow of gas is 50sccm, until the internal pressure of the gas ions vapor deposition apparatus is 500Pa, is then risen in 30min
Temperature bombards phosphorus alkene 150min to 600 DEG C, and under radio-frequency power 250W, and room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.
Embodiment 4
A kind of preparation method of N doping phosphorus alkene, its specific steps can include：Phosphorus alkene is placed in into plasma chemical vapor to sink
In product equipment, and pressure is evacuated to for below 5Pa, then be filled with ammonia and nitrogen dioxide into the gas ions vapor deposition apparatus
Mixed gas, the flow of insufflation gas is 75sccm, until the internal pressure of the gas ions vapor deposition apparatus is 800Pa, so
800 DEG C are warming up in 10min afterwards, and phosphorus alkene 60min is bombarded under radio-frequency power 400W, room temperature is cooled to afterwards, so as to make
Obtain N doping phosphorus alkene.
Embodiment 5
A kind of preparation method of N doping phosphorus alkene, its specific steps can include：Phosphorus alkene is placed in into plasma chemical vapor to sink
In product equipment, and pressure is evacuated to for below 5Pa, then is filled with nitrogen dioxide into the gas ions vapor deposition apparatus, be filled with
The flow of gas is 100sccm, until the internal pressure of the gas ions vapor deposition apparatus is 1000Pa, is then risen in 1min
Temperature bombards phosphorus alkene 1min to 1000 DEG C, and under radio-frequency power 500W, and room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.
As fully visible, the embodiment of the present invention can have phosphorus alkene anti-oxidant well by nitrogen-doping into phosphorus alkene
Performance, not only the physical and chemical performance of phosphorus alkene will not be destroyed, and simple to operate, low for equipment requirements, good product quality, production
Rate is high, and product can use the fields such as electronic communication, communications and transportation extensively.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (3)
1. a kind of preparation method of N doping phosphorus alkene, it is characterised in that including：Phosphorus alkene is placed in plasma gas phase deposition equipment
In, and pressure is evacuated to for below 5Pa, then nitrogenous gas is filled with into the gas ions vapor deposition apparatus, until the ion
The internal pressure of vapor-phase deposition equipment is 100~1000Pa, is then warming up to 200~1000 DEG C in 1~60min, and
Phosphorus 1~360min of alkene is bombarded under 5~500W of radio-frequency power, room temperature is cooled to afterwards, so that N doping phosphorus alkene is made.
2. the preparation method of N doping phosphorus alkene according to claim 1, it is characterised in that described nitrogenous gas is ammonia
At least one of gas, nitrogen, nitric oxide, nitrogen dioxide.
3. the preparation method of N doping phosphorus alkene according to claim 1 or 2, it is characterised in that to ion vapor-phase deposition
The flow of insufflation gas is 5~100sccm in equipment.
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| CN201710495556.6A CN107032310A (en) | 2017-06-26 | 2017-06-26 | A kind of preparation method of N doping phosphorus alkene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646439A (en) * | 2020-06-19 | 2020-09-11 | 昆明理工大学 | Method for doping nano black phosphorus or black phosphorus-based mixed material |
| CN111921552A (en) * | 2020-07-29 | 2020-11-13 | 浙江理工大学 | Transition metal nitrogen-doped phosphide catalyst and preparation method and application thereof |
| CN113122253A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
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| CN102745678A (en) * | 2012-07-12 | 2012-10-24 | 浙江大学 | Method for preparing nitrogen-doped graphene by utilizing plasma sputtering |
| CN104961113A (en) * | 2015-07-01 | 2015-10-07 | 北京石油化工学院 | Method for preparing phosphaalkene |
| CN106744898A (en) * | 2016-12-06 | 2017-05-31 | 中国石油大学(北京) | A kind of modifies three-dimensional grapheme powder of nitrogen plasma and its preparation and application |
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- 2017-06-26 CN CN201710495556.6A patent/CN107032310A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102745678A (en) * | 2012-07-12 | 2012-10-24 | 浙江大学 | Method for preparing nitrogen-doped graphene by utilizing plasma sputtering |
| CN104961113A (en) * | 2015-07-01 | 2015-10-07 | 北京石油化工学院 | Method for preparing phosphaalkene |
| CN106744898A (en) * | 2016-12-06 | 2017-05-31 | 中国石油大学(北京) | A kind of modifies three-dimensional grapheme powder of nitrogen plasma and its preparation and application |
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| DANIL W. BOUKHVALOV: "The atomic and electronic structure of nitrogen- and boron-doped phosphorene", 《PHYS. CHEM. CHEM. PHYS.》 * |
| LIFANG YANG ET AL.: "Tailoring magnetism of black phosphorene doped with B, C, N, O, F, S and Se atom: A DFT calculation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| WEIYANG YU ET AL.: "Anomalous doping effect in black phosphorene using first-principles calculations", 《PHYS. CHEM. CHEM. PHYS.》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122253A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
| CN113122253B (en) * | 2019-12-30 | 2022-03-01 | Tcl科技集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
| CN111646439A (en) * | 2020-06-19 | 2020-09-11 | 昆明理工大学 | Method for doping nano black phosphorus or black phosphorus-based mixed material |
| CN111921552A (en) * | 2020-07-29 | 2020-11-13 | 浙江理工大学 | Transition metal nitrogen-doped phosphide catalyst and preparation method and application thereof |
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Application publication date: 20170811 |