CN104310326A - Black phosphorus preparation method with high conversion rate - Google Patents
Black phosphorus preparation method with high conversion rate Download PDFInfo
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- CN104310326A CN104310326A CN201410589788.4A CN201410589788A CN104310326A CN 104310326 A CN104310326 A CN 104310326A CN 201410589788 A CN201410589788 A CN 201410589788A CN 104310326 A CN104310326 A CN 104310326A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a black phosphorus preparation method with a high conversion rate. The preparation method comprises the following steps: mixing red phosphorus, tin and tin tetraiodide in a mass ratio of (1-6):(40-50):(1-2), filling the mixture into a quartz tube, vacuumizing until the pressure in the quartz tube is smaller than 0.05 Pa, sealing the tube, heating to ensure that the raw material end temperature in the quartz tube is 100-400 DEG C, heating to 400-700 DEG C in 1-2 hours, keeping the temperature for 5-10 hours, then cooling to 200-500 DEG C in 6-8 hours, keeping the temperature for 1-3 days, and finally cooling to the room temperature in 10-15 hours to obtain black phosphorus. The preparation method disclosed by the invention is simple in step and strong in operability; on the one hand, a nontoxic raw material is adopted to achieve effects of cleanliness and environmental friendliness, and on the other hand, only a mild reaction condition is needed, so that the energy consumption and cost are reduced, and the prepared black phosphorus has good crystallinity and a high conversion rate. The preparation method disclosed by the invention has strong repeatability and is favorable for industrial popularization and application.
Description
Technical field
The present invention relates to a kind of preparation method of black phosphorus, be specifically related to a kind of preparation method with the black phosphorus of high conversion, belong to the synthesis field of chemical material.
Technical background
The Developing Application of novel material is one of Main way of scientific development in this century.2004, the success of Graphene was prepared in scientific circles and excites huge great waves, and it is owing to having high conductivity, high-tenacity and great specific surface area, was considered to be expected to alternative traditional semiconductor silicon, caused the research boom of a new round in electronics technology field.But, because Graphene does not have to be with, so the Push And Release of logical circuit can not be realized, this strongly limits its application at electron device and field of photoelectric devices, as field-effect transistor, photodetector, solar cell etc.In recent years, New Two Dimensional semiconductor material one of new direction becoming Materials science is found.
Black phosphorus is as the maximum (2.69g/cm of common four kinds of allotropic substances (that is: red phosphorus, white phosphorus, violet phosphorus, black phosphorus) Midst density of phosphorus
3), the most stable one, has metalluster, good conductivity.It has the laminate structure of similar graphite, combines between layers by Van der Waals force.But the maximum feature being different from graphite in its structure is, the phosphorus atom in its same layer, not in same plane, is the layered arrangement of fold along b axle, and interlamellar spacing larger than graphite (about 5 dust).In addition, it is direct band-gap semicondictor, has good electronic mobility and optical characteristics, and the theoretical cell capacity 2596mAh/g higher than graphite, and these advantages all make it have great application prospect at electronics and field of photoelectric devices.
Traditional black phosphorus method of preparing heats red phosphorus under high pressure (12000atm), high temperature (1000 DEG C), or make catalyzer with mercury at ambient pressure and be prepared.But because the method for above-mentioned synthesis black phosphorus often has high toxicity, productive rate is low, needs the deficiency such as ultra-high voltage, high temperature, therefore in the urgent need to improving the preparation technology of black phosphorus.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of preparation condition gentleness, energy consumption and cost low and the preparation method of the black phosphorus that transformation efficiency is high.
The preparation method with the black phosphorus of high conversion of the present invention, comprises the steps:
Be the ratio mixing of 1 ~ 6:40 ~ 50:1 ~ 2 in mass ratio by red phosphorus, tin and tin tetraiodide, load in silica tube, be evacuated to quartzy intraductal pressure and be less than 0.05pa, tube sealing, heating makes silica tube Raw end temperature be 100 DEG C ~ 400 DEG C, 400 DEG C ~ 700 DEG C are warming up to again in 1 ~ 2 hour, be incubated 5 ~ 10 hours, then in 6 ~ 8 hours, be cooled to 200 DEG C ~ 500 DEG C, be incubated after 1 to 3 day, in 10 ~ 15 hours, be cooled to room temperature, obtain black phosphorus.
The red phosphorus adopted in technique scheme can be powder or particle, and the tin adopted can be sheet or particle, and the tin tetraiodide adopted can be particle or powder.
Beneficial effect of the present invention is: preparation method of the present invention can obtain black phosphorus without the need to using the harsh preparation conditions such as High Temperature High Pressure, can reduce energy consumption and cost greatly; Black phosphorus crystallinity prepared by the present invention is good, and namely gained black phosphorus quality up to 97%, can have high transformation efficiency with the mass ratio of red phosphorus in initial feed, and the inventive method step is simple, by force repeatable in addition, and the industry of being beneficial to is applied.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the black phosphorus that embodiment 1 obtains.
Fig. 2 is the SEM figure of the black phosphorus that embodiment 1 obtains.
Embodiment
Below in conjunction with drawings and the specific embodiments, the invention will be further described.
Embodiment 1
Be the ratio mixing of 3:40:1 in mass ratio by red phosphorus, tin and tin tetraiodide, load in silica tube, be evacuated to quartzy intraductal pressure and be less than 0.05pa, tube sealing, heating makes silica tube Raw end temperature be 200 DEG C, 600 DEG C are warming up to again with 1 hour, be incubated 6 hours, be then cooled to 300 DEG C with 6 hours, be incubated after 2 days, be down to room temperature with 10 hours, take out product.
Products therefrom is black block, and Fig. 1 is its XRD figure, and its SEM as shown in Figure 2, can find out that products therefrom is black phosphorus.And through measuring, gained black phosphorus quality is about 97% of red phosphorus quality in raw material.
Embodiment 2
Be the ratio mixing of 3:25:1 in mass ratio by red phosphorus, tin and tin tetraiodide, load in silica tube, be evacuated to quartzy intraductal pressure and be less than 0.05pa, tube sealing, heating makes silica tube Raw end temperature be 400 DEG C, 700 DEG C are warming up to again with 2 hours, be incubated 10 hours, be then cooled to 500 DEG C with 8 hours, be incubated after 3 days, be down to room temperature with 15 hours, in silica tube, obtain black phosphorus.
Embodiment 3
Be the ratio mixing of 1:40:1 in mass ratio by red phosphorus, tin and tin tetraiodide, load in silica tube, be evacuated to quartzy intraductal pressure and be less than 0.05pa, tube sealing, heating makes silica tube Raw end temperature be 100 DEG C, 400 DEG C are warming up to again with 1 hour, be incubated 5 hours, be then cooled to 200 DEG C with 6 hours, be incubated after 1 day, be down to room temperature with 10 hours, in silica tube, obtain black phosphorus.
Claims (1)
1. one kind has the black phosphorus preparation method of high conversion, it is characterized in that comprising the steps: by red phosphorus, tin and tin tetraiodide be in mass ratio 1 ~ 6:40 ~ 50:1 ~ 2 ratio mixing, load in silica tube, be evacuated to quartzy intraductal pressure and be less than 0.05pa, tube sealing, heating makes silica tube Raw end temperature be 100 DEG C ~ 400 DEG C, 400 DEG C ~ 700 DEG C are warming up to again in 1 ~ 2 hour, be incubated 5 ~ 10 hours, then in 6 ~ 8 hours, 200 DEG C ~ 500 DEG C are cooled to, be incubated 1 to 3 day, finally in 10 ~ 15 hours, be cooled to room temperature, obtain black phosphorus.
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Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787736A (en) * | 2015-04-04 | 2015-07-22 | 成都育芽科技有限公司 | Method for large-scale preparation of black phosphorus with bilayer structure |
| 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 |
| CN105668531A (en) * | 2016-01-11 | 2016-06-15 | 上海交通大学 | Liquid phase stripping preparation method for phosphaalkene nanoribbon or phosphorus nanoribbon |
| 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 | A kind of method for preparing rhombic system black phosphorus monocrystalline |
| CN106711408A (en) * | 2015-11-13 | 2017-05-24 | 中国科学院金属研究所 | Flexible lithium ion battery black phosphorus nanosheet-graphene composite film anode, and preparation thereof |
| CN106744754A (en) * | 2016-11-14 | 2017-05-31 | 深圳大学 | A kind of red phosphorus preprocess method prepared for black phosphorus |
| CN106800282A (en) * | 2017-03-23 | 2017-06-06 | 深圳市来源新材料科技有限公司 | A kind of nanometer of preparation method of black phosphorus |
| CN106941205A (en) * | 2016-01-05 | 2017-07-11 | 中芯国际集成电路制造(上海)有限公司 | Waveguide and forming method thereof |
| 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 |
| CN107359341A (en) * | 2017-07-26 | 2017-11-17 | 青岛大学 | A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper |
| CN107447193A (en) * | 2016-11-14 | 2017-12-08 | 深圳大学 | A kind of black phosphorus film and preparation method thereof |
| CN108059137A (en) * | 2017-12-04 | 2018-05-22 | 中国科学院电工研究所 | A kind of preparation method of black phosphorus nano 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 |
| CN108128761A (en) * | 2018-01-30 | 2018-06-08 | 昆明理工大学 | A kind of continuous preparation method of black phosphorus |
| TWI658515B (en) * | 2016-12-05 | 2019-05-01 | 上海新昇半導體科技有限公司 | Low contact resistivity finfet with black phosphorus channel and the method for making the same |
| CN109970036A (en) * | 2019-05-14 | 2019-07-05 | 闽江学院 | A kind of method that nucleus assisted with high-temperature difference method quickly prepares black phosphorus |
| CN110498404A (en) * | 2019-07-22 | 2019-11-26 | 山东玥能新材料科技有限公司 | A method of black phosphorus-carbon nano tube compound material is prepared in situ |
| CN111170291A (en) * | 2020-01-21 | 2020-05-19 | 上海交通大学 | Method for quickly preparing black phosphorus at low cost |
| CN111422840A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof |
| CN111420639A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene composite two-dimensional material and preparation method and application thereof |
| CN112110429A (en) * | 2019-06-21 | 2020-12-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method and application of black phosphorus nanosheet |
| 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 |
| CN112830462A (en) * | 2021-02-03 | 2021-05-25 | 陕西科技大学 | Method for safely and efficiently synthesizing high-purity black phosphorus |
| CN115010104A (en) * | 2022-06-29 | 2022-09-06 | 西安交通大学 | Method for preparing needle-shaped purple phosphorus crystal by using tin as catalyst |
| CN115010103A (en) * | 2022-04-20 | 2022-09-06 | 贵州民族大学 | Preparation method of purple phosphorus nanobelt material |
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| CN104787736A (en) * | 2015-04-04 | 2015-07-22 | 成都育芽科技有限公司 | Method for large-scale preparation of black phosphorus with bilayer structure |
| CN104787736B (en) * | 2015-04-04 | 2016-12-28 | 重庆市金升机械配件制造有限公司 | A kind of method preparing double-decker black phosphorus on a large scale |
| WO2017020672A1 (en) * | 2015-08-06 | 2017-02-09 | 王贝贝 | Processing method of etching black phosphorus two-dimensional material using oxygen plasma |
| CN105133009A (en) * | 2015-09-23 | 2015-12-09 | 清华大学 | Preparation method for orthorhombic crystal system black phosphorus monocrystalline |
| CN105133009B (en) * | 2015-09-23 | 2017-09-26 | 清华大学 | A kind of preparation method of rhombic system black phosphorus monocrystalline |
| CN106711408B (en) * | 2015-11-13 | 2019-05-10 | 中国科学院金属研究所 | Flexible lithium ion battery black phosphorus nanometer sheet-graphene composite film cathode and preparation |
| CN106711408A (en) * | 2015-11-13 | 2017-05-24 | 中国科学院金属研究所 | Flexible lithium ion battery black phosphorus nanosheet-graphene composite film anode, and preparation thereof |
| CN105460910A (en) * | 2015-11-19 | 2016-04-06 | 浙江大学 | A constant-temperature large-scale preparing method of belt-shaped black phosphorus |
| CN106941205B (en) * | 2016-01-05 | 2019-12-31 | 中芯国际集成电路制造(上海)有限公司 | Waveguide and method of forming the same |
| CN106941205A (en) * | 2016-01-05 | 2017-07-11 | 中芯国际集成电路制造(上海)有限公司 | Waveguide and forming method thereof |
| 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 |
| CN105668531A (en) * | 2016-01-11 | 2016-06-15 | 上海交通大学 | Liquid phase stripping preparation method for phosphaalkene nanoribbon or phosphorus nanoribbon |
| 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 |
| 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 |
| CN106498492A (en) * | 2016-11-01 | 2017-03-15 | 南京工业大学 | A kind of method for preparing rhombic system black phosphorus monocrystalline |
| CN107447193A (en) * | 2016-11-14 | 2017-12-08 | 深圳大学 | A kind of black phosphorus film and preparation method thereof |
| CN106744754A (en) * | 2016-11-14 | 2017-05-31 | 深圳大学 | A kind of red phosphorus preprocess method prepared for black phosphorus |
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| CN106800282B (en) * | 2017-03-23 | 2019-11-08 | 深圳市来源新材料科技有限公司 | A kind of preparation method of nanometer of black phosphorus |
| CN106800282A (en) * | 2017-03-23 | 2017-06-06 | 深圳市来源新材料科技有限公司 | A kind of nanometer of preparation method of black phosphorus |
| CN107359341A (en) * | 2017-07-26 | 2017-11-17 | 青岛大学 | A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper |
| CN108059137A (en) * | 2017-12-04 | 2018-05-22 | 中国科学院电工研究所 | A kind of preparation method of black phosphorus nano 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 |
| CN108128761A (en) * | 2018-01-30 | 2018-06-08 | 昆明理工大学 | A kind of continuous preparation method of black phosphorus |
| CN109970036A (en) * | 2019-05-14 | 2019-07-05 | 闽江学院 | A kind of method that nucleus assisted with high-temperature difference method quickly prepares black phosphorus |
| CN112110429A (en) * | 2019-06-21 | 2020-12-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method and application of black phosphorus nanosheet |
| CN112110429B (en) * | 2019-06-21 | 2021-11-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method and application of black phosphorus nanosheet |
| 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 |
| CN110498404A (en) * | 2019-07-22 | 2019-11-26 | 山东玥能新材料科技有限公司 | A method of black phosphorus-carbon nano tube compound material is prepared in situ |
| CN111170291A (en) * | 2020-01-21 | 2020-05-19 | 上海交通大学 | Method for quickly preparing black phosphorus at low cost |
| CN111420639A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene composite two-dimensional material and preparation method and application thereof |
| CN111422840A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof |
| CN112830462A (en) * | 2021-02-03 | 2021-05-25 | 陕西科技大学 | Method for safely and efficiently synthesizing high-purity black phosphorus |
| CN115010103A (en) * | 2022-04-20 | 2022-09-06 | 贵州民族大学 | Preparation method of purple phosphorus nanobelt material |
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Application publication date: 20150128 |