CN108622867A - A kind of method that black phosphorus is thinned in short annealing - Google Patents
A kind of method that black phosphorus is thinned in short annealing Download PDFInfo
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- CN108622867A CN108622867A CN201710163992.3A CN201710163992A CN108622867A CN 108622867 A CN108622867 A CN 108622867A CN 201710163992 A CN201710163992 A CN 201710163992A CN 108622867 A CN108622867 A CN 108622867A
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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
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of method that black phosphorus is thinned in short annealing, includes the following steps：(1) blocky black phosphorus is decomposed into slabbing black phosphorus；(2) sheet black phosphorus obtained by step (1) is put into quick anneal oven, anneal 30s 10min under 290 350 DEG C of Oxygen Conditions, then the 1min that anneals under a nitrogen atmosphere.It is simple that the beneficial effects of the invention are as follows operating processes, and process costs are cheap, and obtained two-dimensional material black phosphorus has complete lattice structure and smooth, clean surface.
Description
Technical field
The invention belongs to functional material preparing technical field, more particularly, to a kind of method that black phosphorus is thinned in short annealing,
The thin layer black phosphorus of preparation can be applied to the fields such as photoelectric material, sensor.
Background technology
Two-dimensional material, such as graphene, black phosphorus, transient metal sulfide, due to its special nature and in nanoelectronic
Potential application greatly paid close attention to.Wherein, graphene, molybdenum disulfide, black phosphorus have existed as representative two-dimensional material
Flexible electronic, photodetector, electro-catalysis, the application fields such as gas sensing are widely studied.The property of black phosphorus is played with application
It is heavily dependent on the thickness of two-dimensional material.Such as being thinned with black phosphorus, band gap increases to 2.0eV from 0.3eV.
Its carrier mobility is also related with thickness.
The method being mainly by mechanically pulling off at present obtains thin layer black phosphorus material.But this method randomness is very big, and
The thin layer black phosphorus of stripping, surface defect is more, influences its electrical properties.Based on this researcher, several, such as oxygen has been probed into
Plasma is thinned, but surface can remain the oxide of phosphorus.AFM equally can be used for that black phosphorus is thinned, but by instrument
Limitation, rate and thinned scale, which is thinned, significant limitations.Therefore, under the basis that known black phosphorus has broad prospect of application,
A kind of clean surface is urgently developed, and not will produce the method that black phosphorus is thinned in surface defect fast and easy.
Invention content
The drawbacks of in order to overcome thin layer black phosphorus method made above, the object of the present invention is to provide a kind of easy to operate, nothings
It need to can be completed under the conditions of anhydrous and oxygen-free, the method that black phosphorus is thinned in the short annealing of flow can be completed without professional.
The technical scheme is that：
The method that black phosphorus is thinned in a kind of short annealing of the present invention, includes the following steps：
Sheet black phosphorus is put into quick anneal oven, anneal 30s-10min under 290-350 DEG C of Oxygen Condition, then in nitrogen
Under the conditions of anneal 30s-10min.
Preferably, annealing time is 3-4min under the Oxygen Condition.
Preferably, annealing time is 1min under the condition of nitrogen gas.
Preferably, the sheet black phosphorus is decomposed by blocky black phosphorus；
Preferably, the apportioned effort can be by mechanically pulling off or ultrasound, mechanical agitation are completed.
Another aspect of the present invention further includes the black phosphorus prepared by above-mentioned short annealing thining method.
The invention has the advantages and positive effects that：
1, operating process of the invention is simple, and process costs are cheap, be not required to expensive large-scale instrument can be achieved with it is black
Phosphorus is thinned.
2, the two-dimensional material black phosphorus that the present invention obtains has complete lattice structure and smooth, clean surface, so as to
It can realize industrialization.
3, the present invention obtains clean, complete plane of crystal, has desorption to make the air of absorption in addition to making material be thinned
With reduction FET transports hesitation.
Description of the drawings
Fig. 1 is the optical microscope of sheet black phosphorus, is that sheet black phosphorus has been transferred to Si/ by the method that is by mechanically pulling off
SiO2In substrate, through different temperatures annealing 3min, wherein：
Fig. 1 a, 1c, 1e are that blocky black phosphorus is transferred to Si/SiO through mechanical stripping2Optical microscope in substrate.
Fig. 1 b, 1d, 1f are 360 DEG C, 330 DEG C, 300 DEG C of annealing under oxygen respectively by the sample in Fig. 1 a, 1c, 1e
3min, then the optical microscope of annealing 1min under a nitrogen atmosphere.
Atomic force microscopy diagram when Fig. 2 is 330 DEG C before and after oxygen annealing 3min.Wherein：
Fig. 2 a are that blocky black phosphorus is transferred to Si/SiO through mechanical stripping2Atomic force microscopy diagram in substrate.
Fig. 2 b are the atomic force microscopy diagram after 330 degree of oxygen annealing 3min by the sample in Fig. 1.
Fig. 3 is through thickness thinning under different temperatures with annealing time change curve.
Legend is as follows：
a:It is 360 DEG C and spends lower thickness thinning with annealing time change curve.It is 5.6nm/min. that rate, which is thinned,
b:It is 330 DEG C and spends lower thickness thinning with annealing time change curve.It is 3.8nm/min. that rate, which is thinned,
c:It is 300 DEG C and spends lower thickness thinning with annealing time change curve.It is 2.6nm/min. that rate, which is thinned,
Specific implementation mode
It elaborates below in conjunction with the accompanying drawings to the present invention.
As one embodiment, it is illustrated so that black phosphorus is thinned in oxygen annealing as an example：
Embodiment 1
(1) a small amount of blocky black phosphorus is placed on blue light adhesive tape, folded adhesive tape is several times, thin by dimethyl silicone polymer
Sheet black phosphorus is transferred to Si/SiO by film2In substrate, the optical microscope of gained sample as illustrated in figure 1 c, gained sample
Atomic force microscopy diagram is as shown in Figure 2 a, thickness of sample 10.6nm.
(2) by step (1) gained sample under Oxygen Condition, 330 DEG C of short annealing 3min.
(3) oxygen is changed into nitrogen, in 340 DEG C of short annealing 1min.The optical microscope of gained sample such as figure is as schemed
Shown in 1d, the atomic force microscopy diagram of gained sample is as shown in Figure 2 b, thickness of sample 2.7nm.
In thinning process, the thickness thinning of different time points sample is measured, thickness thinning is obtained and changes with annealing time
Curve is shown in Fig. 3 b.
Embodiment 2
(1) a small amount of blocky black phosphorus is placed on blue light adhesive tape, folded adhesive tape is several times, thin by dimethyl silicone polymer
Sheet black phosphorus is transferred to Si/SiO by film2In substrate, the optical microscope of gained sample is as shown in fig. le.
(2) by step (1) gained sample under Oxygen Condition, 300 DEG C of short annealing 3min.
(3) oxygen is changed into nitrogen, in 340 DEG C of short annealing 1min, optical microscope such as Fig. 1 f institutes of gained sample
Show.
In thinning process, the thickness thinning of different time points sample is measured, thickness thinning is obtained and changes with annealing time
Curve is shown in Fig. 3 c.
Embodiment 3
1) a small amount of blocky black phosphorus is placed on blue light adhesive tape, folded adhesive tape several times, by polydimethylsiloxanefilm film,
Sheet black phosphorus is transferred to Si/SiO2In substrate, the optical microscope of gained sample is as shown in Figure 1a.
(2) by step (1) gained sample under Oxygen Condition, 360 DEG C of short annealing 3min.
(3) oxygen is changed into nitrogen, in 340 DEG C of short annealing 1min, optical microscope such as Fig. 1 b institutes of gained sample
Show.
In thinning process, the thickness thinning of different time points sample is measured, thickness thinning is obtained and changes song with annealing time
Line is shown in Fig. 3 a.
One embodiment of the present invention has been described in detail above, but the content be only the present invention preferable implementation
Example should not be construed as limiting the practical range of the present invention.It is all according to all the changes and improvements made by the present patent application range
Deng should all still fall within the scope of the patent of the present invention.
Claims (6)
1. a kind of method that black phosphorus is thinned in short annealing, it is characterised in that：Include the following steps：
Gained sheet black phosphorus is put into quick anneal oven, and anneal 30s-10min under 290-350 DEG C of Oxygen Condition, then in nitrogen item
Anneal 30s-10min under part.
2. the method that black phosphorus is thinned in a kind of short annealing according to claim 1, it is characterised in that：The step (1)
Sheet black phosphorus is resolved by blocky black phosphorus.
3. the method that black phosphorus is thinned in a kind of short annealing according to claim 2, it is characterised in that：It states in step (2)
Apportioned effort can be by mechanically pulling off or ultrasound, mechanical agitation are completed.
4. the method that black phosphorus is thinned in a kind of short annealing according to claim 1, it is characterised in that：Under the Oxygen Condition
Annealing time is 3-4min.
5. the method that black phosphorus is thinned in a kind of short annealing according to claim 1, it is characterised in that：It moves back under a nitrogen atmosphere
The fiery time is 1-2min.
6. a kind of black phosphorus prepared by any one of claim 1-4 short annealing thining methods.
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| CN201710163992.3A CN108622867A (en) | 2017-03-17 | 2017-03-17 | A kind of method that black phosphorus is thinned in short annealing |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101522350B1 (en) * | 2014-10-10 | 2015-05-26 | 한국기초과학지원연구원 | Preparation method of monolayer black phosphorous using ultrasound irradiation |
| CN105565289A (en) * | 2016-01-29 | 2016-05-11 | 西北大学 | Black phosphorus and phosphinidene preparing methods |
| CN106024861A (en) * | 2016-05-31 | 2016-10-12 | 天津理工大学 | Two-dimensional black phosphorus/transitional metal chalcogenide heterojunction device and preparation method therefor |
| CN106315531A (en) * | 2016-08-23 | 2017-01-11 | 深圳先进技术研究院 | Black phosphorus modified by aromatic compound and preparation method and application thereof |
| CN106424197A (en) * | 2016-10-31 | 2017-02-22 | 江西凯安智能股份有限公司 | Processing technology for high-purity and high-electric conductivity oxygen-free copper wire |
-
2017
- 2017-03-17 CN CN201710163992.3A patent/CN108622867A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101522350B1 (en) * | 2014-10-10 | 2015-05-26 | 한국기초과학지원연구원 | Preparation method of monolayer black phosphorous using ultrasound irradiation |
| CN105565289A (en) * | 2016-01-29 | 2016-05-11 | 西北大学 | Black phosphorus and phosphinidene preparing methods |
| CN106024861A (en) * | 2016-05-31 | 2016-10-12 | 天津理工大学 | Two-dimensional black phosphorus/transitional metal chalcogenide heterojunction device and preparation method therefor |
| CN106315531A (en) * | 2016-08-23 | 2017-01-11 | 深圳先进技术研究院 | Black phosphorus modified by aromatic compound and preparation method and application thereof |
| CN106424197A (en) * | 2016-10-31 | 2017-02-22 | 江西凯安智能股份有限公司 | Processing technology for high-purity and high-electric conductivity oxygen-free copper wire |
Non-Patent Citations (1)
| Title |
|---|
| SHENGHUANG LIN ET AL.: "In situ observation of the thermal stability of black phosphorus", 《2D MATERIALS》 * |
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Application publication date: 20181009 |