CN107359341A - A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper - Google Patents
A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper Download PDFInfo
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- CN107359341A CN107359341A CN201710619873.4A CN201710619873A CN107359341A CN 107359341 A CN107359341 A CN 107359341A CN 201710619873 A CN201710619873 A CN 201710619873A CN 107359341 A CN107359341 A CN 107359341A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention devises the method and its application that a kind of one-step method synthesizes black phosphorus on carbon paper, mainly includes the following steps that：Phosphorus source is weighed, drying of annealing, a certain amount of phosphorus source presoma is then taken, is uniformly put into magnetic boat, then add empty carbon paper above, leads to protection gas, then at the uniform velocity heats up, heat, be then at the uniform velocity cooled to room temperature, that is, obtain black phosphorus on carbon paper；The present invention is using black phosphorus on vapour deposition process synthesis carbon paper, overcome in traditional industry high temperature process heat method, high energy consumption caused by high temperature, high request to equipment and need special catalyst, the shortcomings of generated time is longer, and the preparation method has manufacture method simple, it is easy to operate, cost is cheap, the features such as beneficial to industrialized production, test is separated out by chemical property and oxygen to find, black phosphorus has high specific capacity first on the carbon paper of the method synthesis, the advantages of good cycle performance and efficient oxygen separate out, therefore, its application environment is friendly, wide market.
Description
Technical field：
The preparing technical field of the electrocatalysis material separated out the present invention relates to lithium ion battery negative material and oxygen, is related to one
The synthetic method of kind black phosphorus, particularly a kind of one-step method synthesize the method and its application of black phosphorus on carbon paper.
Background technology：
P elements at least 10 kinds of allotropes in nature, but its simple substance be primarily present form for white phosphorus,
Three kinds of red phosphorus, black phosphorus, quite active different from white phosphorus and red phosphorus, black phosphorus is a kind of most stable of allotrope of phosphorus, density
Maximum (up to 2.69g/cm3), all it is difficult dissolving in general conventional organic solvent, is not susceptible to chemically react.Black phosphorus be by
The stratified material that single atomic layer is flocked together by Van der Waals interaction.Its composition and blocky graphite material
Like the inside of an individual layer.Each phosphorus atoms and three adjacent phosphorus atoms are combined to form a pleat by covalently bonded
The alveolate texture of wrinkle.As the new black phosphorus of two-dimensional semiconductor material one, cause extensive concern both at home and abroad.Individual layer is black at present
Phosphorus is dilute to be by mechanically pulling off method to obtain multilayer black phosphorus dilute, has then successfully been prepared by plasma stripping again.Black phosphorus
As a kind of new two-dimensional material, the concern of scientific research personnel is enjoyed.In early days, black phosphorus does not cause too much in semiconductor applications
Concern, it is likely to because at that time silicon dominated the field.But since 2014, to graphene, stratiform hexagonal boron nitride
And on the Research foundation such as transient metal sulfide, black phosphorus just is exploited out from the angle of two-dimensional material and thin-film material.
1914, American scientist Bridgman was prepared for black phosphorus by high pressure method, this be phosphorus allotrope in it is most stable of
It is a kind of.Bridgman also obtains Nobel Prize in physics for 1914, but prize-winning reason is to commend it in high-pressure physics field
Outstanding contribution, black phosphorus do not cause too many concern in itself.But in 2014, the research of black phosphorus obtains swift and violent development,
Its many special photoelectric property is exploited out, and wherein China scientist is also made that outstanding contributions, such as Fudan University
Remote ripple professor and the Chen Xianhui of Chinese University of Science and Technology teach seminar at the beginning of 2014《Natural nanometer technology》Magazine takes the lead in reporting
The road FET device of the high mobility based on two-dimentional black phosphorus.At present, the conventional preparation method of black phosphorus is still high
Prepared by warm high-pressure process, although black phosphorus can be successfully prepared out, Yield comparison is low, and the requirement to equipment and catalyst
Requirement it is higher, while the pollution to environment also results in large effect, therefore, it is this new to find easier method synthesis
Type two-dimensional material black phosphorus is imperative.Meanwhile lithium ion battery and oxygen precipitation (OER) field are applied it to, improve its specific volume
It is still a very challenging problem that amount, cycle performance and oxygen, which separate out performance, and therefore, design prepares a kind of one-step method in carbon paper
The method and its application of upper synthesis black phosphorus.
The content of the invention：
It is an object of the invention to overcome the shortcomings of the prior art and defect, design and provide a kind of one-step method in carbon
The method and its application of black phosphorus are synthesized on paper, this method is simple to operate, cost is cheap, the black phosphorus beneficial to industrialized production
Preparation method, and also directly synthesize black phosphorus on conductive material carbon paper, the black phosphorus that can make to prepare is in lithium ion battery
And there is more preferable application prospect in oxygen precipitation (OER).
To achieve these goals, the method and its application of black phosphorus are synthesized on carbon paper the present invention relates to a kind of one-step method,
This method synthesizes black phosphorus using vapour deposition process on carbon paper, and is applied in lithium ion battery and oxygen separate out (OER), tool
Body comprises the following steps：
S1, first red phosphorus is uniformly put into quartz boat, then quartz boat is put into tube furnace, guarantor will be passed through in tube furnace
Shield gas simultaneously makes annealing treatment to red phosphorus in tube furnace, and annealing temperature is 180~250 DEG C, and the time is 1.5~4.5h；In annealing process
Strict control is at the uniform velocity passed through protection gas, to ensure that obtained material is evenly distributed, is further ensured that the electrification of prepared material
Learn performance and oxygen separates out performance；
The red phosphorus after annealing is made after S2, annealing, is placed in room air that to be cooled to room temperature standby；
S3, the red phosphorus obtained in S2 is transferred in mortar be ground with grinding fore-telling, the presoma red phosphorus for being made required is standby
With；
S4, obtained a certain amount of red phosphorus is uniformly put into quartz boat, while the carbon paper of blank is placed on quartz boat
Above, transfer it among tube furnace；
S5, tube furnace is passed through to protection gas, and strictly controls the flow velocity of gas, to ensure the black phosphorus material on carbon paper
The quality and performance of material, then tube furnace is at the uniform velocity warming up to 500~750 DEG C to be heated, after 1~5h is incubated, by temperature
Degree is reduced to 350 DEG C, continues 1~3h of insulation, the black phosphorus material on carbon paper is finally made.
Preferably, phosphorus source of the present invention is common commercialization red phosphorus, and the carbon paper is the common carbon paper of purchase, institute
That states abradant grind fore-telling and grinds fore-telling for common agate.
Preferably, the process conditions ground in mortar of the present invention are 20~60min of grinding at room temperature.
Preferably, carbon paper of the present invention is that other are miscellaneous for the nothing that is obtained after the hollow burning 24h of Muffle furnace of common model
The bare carbon paper of matter.
Preferably, the empty temperature of burning required for bare carbon paper of the present invention is 300~400 DEG C, and the time that sky burns is
12~20h.
Preferably, the speed that tube furnace of the present invention at the uniform velocity heats up and at the uniform velocity cooled is 6~10 DEG C/min.
Preferably, for the present invention in the step of preparing presoma red phosphorus, logical protection gas is inert gas or nitrogen, is led to
Gas velocity rate is 5~10sccm, and in the step of black phosphorus material on synthesizing carbon paper, the gas that is passed through is high-purity argon gas, Ventilation Rate
For 3-9sccm.
Black phosphorus on carbon paper prepared by the present invention has good in anode material for lithium-ion batteries and oxygen precipitation (OER) is prepared
Good application, on the carbon paper of preparation black phosphorus assembled battery have obvious discharge platform in 0.78V, it was demonstrated that it can in 0.78V platforms
Inverse property is good；The chemical property of black phosphorus is good on the carbon paper of preparation, and first discharge specific capacity can reach 2234.5mAhg-1；
2234.1mAh·g-1；The stable cycle performance of black phosphorus positive electrode on the carbon paper of preparation, after 200 circle charge and discharge cycles, than
Capacity still can reach 1677.3mAhg-1, 200 circle after capability retention be 75.14%；Black phosphorus material on the carbon paper of preparation
Overpotential be 1.47V, and in 1.6V, current density can reach 100mAcm-2(RHE)。
The present invention compared with prior art, the advantage of the invention is that：Black phosphorus is synthesized on carbon paper using vapour deposition process,
Overcome in traditional industry high temperature process heat method, high energy consumption, high request and generated time to equipment caused by high temperature
It is longer, the shortcomings of expensive catalyst is needed in course of reaction.The electrification of black phosphorus product made from conventional high-temperature solid phase method
It is insufficient contact to learn performance bad mainly raw material and catalyst, or vacuum degree control is not in place during high―temperature nuclei,
The heterogencity of product partial structurtes will be result in, therefore the impurity of other phases can be produced.But this vapour deposition process synthesizes
Carbon paper on black phosphorus avoid these shortcomings, and impurity is less, and than more uniform, particle also compares obtained product cut size
It is small, beneficial to the production of the industrial high efficiency rate of black phosphorus on positive electrode carbon paper, while the preparation method have manufacture method it is simple,
Easy to operate, cost is cheap and black phosphorus material that directly obtained on conductive carbon paper, so beneficial to industrialized production, passes through
Chemical property and electro-catalysis test discovery, the black phosphorus on carbon paper that the method synthesizes, not only with high specific capacity first
And the advantages of good cycle, but also (OER) performance is separated out with good oxygen, there are fabulous market prospects
Brief description of the drawings：
Fig. 1 is that obtained discharge curve first is tested in black phosphorus assembled battery on the carbon paper of preparation of the present invention.
Fig. 2 is the cycle performance curve map that black phosphorus assembled battery obtains on the carbon paper of preparation of the present invention.
Fig. 3 is the linearity curve that black phosphorus oxygen separates out on the carbon paper of preparation of the present invention.
Embodiment：
For the ease of understanding the present invention, the invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1：
A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper, specifically includes following steps：
S1, weigh 5.0g red phosphorus and be uniformly put into quartz boat, then quartz boat is put into tube furnace, then will lead in tube furnace
Enter argon gas protection gas；Tube furnace is at the uniform velocity warming up to 180 DEG C, 4h is heated, is made annealing treatment；
The sample after annealing is made after S2, annealing, and it is standby to be cooled to room temperature；
S3, S2 sample is transferred in mortar and foretells grinding 40min with grinding, it is standby that required presoma red phosphorus is made；
S4, the presoma red phosphorus prepared in 0.5g S3 is weighed, be uniformly put into quartz boat, then the carbon paper of blank is put
On quartz boat, transfer it among tube furnace；
S5, protection gas argon gas will be passed through in tube furnace, the flow velocity for strictly controlling argon gas is 4sccm, and tube furnace is at the uniform velocity risen
Temperature is incubated 3h, temperature then is reduced into 350 DEG C to 500 DEG C, continues that the black phosphorus material on carbon paper is made after being incubated 3h.
Black phosphorus can be applied to anode material for lithium-ion batteries on carbon paper made from the present embodiment and oxygen separates out (OER) neck
Domain, Fig. 1 are that obtained discharge curve first is tested in black phosphorus assembled battery on the carbon paper of embodiment preparation, can from Fig. 1
Go out, have obvious discharge platform in 0.78V, black phosphorus material is in 0.78V platform good reversibilities on this explanation carbon paper；From Fig. 1 also
, it can be seen that the first discharge specific capacity of black phosphorus positive electrode is 2234.5mAhg on the carbon paper of the present embodiment synthesis-1, it was demonstrated that
Material electrochemical performance manufactured in the present embodiment is good；Fig. 2 follows for what black phosphorus assembled battery on carbon paper manufactured in the present embodiment obtained
Ring performance chart, it can be seen that the specific capacity first of black phosphorus positive electrode is on carbon paper manufactured in the present embodiment from Fig. 2
2234.1mAh·g-1, after 200 circle charge and discharge cycles, specific capacity still can reach 1677.3mAhg-1, after 200 enclose
Capability retention is 75.14%, illustrates that the cycle performance of black phosphorus positive electrode on the carbon paper of preparation is more stable；Fig. 3 is this reality
The linearity curve that black phosphorus oxygen separates out on the carbon paper of example preparation is applied, it can be seen that the overpotential of black phosphorus material is on carbon paper from figure
1.47V, and in 1.6V, current density can reach 100mAcm-2(RHE)。
Embodiment 2：
A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper, specifically includes following steps：
S1, weigh 4.0g red phosphorus and be uniformly put into quartz boat, then quartz boat is put into tube furnace, then will lead in tube furnace
Enter argon gas protection gas；Tube furnace is at the uniform velocity warming up to 180 DEG C, 2h is heated, is made annealing treatment；
The sample after annealing is made after S2, annealing, and it is standby to be cooled to room temperature；
S3, S2 sample is transferred in mortar and foretells grinding 20min with grinding, it is standby that required presoma red phosphorus is made；
S4, the presoma red phosphorus prepared in 0.4g S3 is weighed, be uniformly put into quartz boat, then the carbon paper of blank is put
On quartz boat, transfer it among tube furnace；
S5, protection gas argon gas will be passed through in tube furnace, the flow velocity for strictly controlling argon gas is 5sccm, and tube furnace is at the uniform velocity risen
Temperature is incubated 2h, temperature then is reduced into 350 DEG C to 550 DEG C, continues that the black phosphorus material on carbon paper is made after being incubated 2h.
Embodiment 3：
A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper, specifically includes following steps：
S1, weigh 6.0g red phosphorus and be uniformly put into quartz boat, then quartz boat is put into tube furnace, then will lead in tube furnace
Enter argon gas protection gas；Tube furnace is at the uniform velocity warming up to 250 DEG C, 4h is heated, is made annealing treatment；
The sample after annealing is made after S2, annealing, and it is standby to be cooled to room temperature；
S3, S2 sample is transferred in mortar and foretells grinding 60min with grinding, it is standby that required presoma red phosphorus is made；
S4, the presoma red phosphorus prepared in 0.4g S3 is weighed, be uniformly put into quartz boat, then the carbon paper of blank is put
On quartz boat, transfer it among tube furnace；
S5, protection gas argon gas will be passed through in tube furnace, the flow velocity for strictly controlling argon gas is 6sccm, and tube furnace is at the uniform velocity risen
Temperature is incubated 2h, temperature then is reduced into 350 DEG C to 600 DEG C, continues that the black phosphorus material on carbon paper is made after being incubated 1h.
Claims (9)
1. a kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that preparation method specifically includes following
Step：
S1, first red phosphorus is uniformly put into quartz boat, then quartz boat is put into tube furnace, protection gas will be passed through in tube furnace
And red phosphorus in tube furnace is made annealing treatment, annealing temperature is 180~250 DEG C, and the time is 1.5~4.5h；It is strict in annealing process
Control is at the uniform velocity passed through protection gas, to ensure that obtained material is evenly distributed, is further ensured that the electrochemistry of prepared material
Energy and oxygen separate out performance；
The red phosphorus after annealing is made after S2, annealing, is placed in room air that to be cooled to room temperature standby；
S3, the red phosphorus obtained in S2 is transferred in mortar be ground with grinding fore-telling, the presoma red phosphorus for being made required is standby；
S4, obtained a certain amount of red phosphorus is uniformly put into quartz boat, while the carbon paper of blank is placed on above quartz boat,
Transfer it among tube furnace；
S5, tube furnace is passed through to protection gas, and strictly controls the flow velocity of gas, to ensure the black phosphorus material on carbon paper
Quality and performance, then tube furnace is at the uniform velocity warming up to 500~750 DEG C to be heated, after 1~5h is incubated, temperature is dropped
Low to 350 DEG C, continue 1~3h of insulation, the black phosphorus material on carbon paper is finally made.
2. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
Described phosphorus source is common commercialization red phosphorus, and the carbon paper is the common carbon paper of purchase, and described abradant to grind fore-telling be common
Agate grind fore-telling.
3. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
Described carbon paper be common model Muffle furnace it is hollow burn one day after the obtained bare carbon paper without other impurities.
4. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
Empty temperature of burning required for described bare carbon paper is 300~400 DEG C, and the time that sky burns is 12~20h.
5. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
The process conditions ground in described mortar are 20~60min of grinding at room temperature.
6. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
The speed that described tube furnace at the uniform velocity heats up and at the uniform velocity cooled is 6~10 DEG C/min.
7. a kind of one-step method according to claim 1 synthesizes the method and its application of black phosphorus on carbon paper, it is characterised in that
The protection gas led in the step S1 is inert gas or nitrogen, and Ventilation Rate is 5~10sccm, the black phosphorus on synthesis carbon paper
In the step of material, the gas being passed through is high-purity argon gas, and Ventilation Rate is 3~9sccm.
8. a kind of one-step method according to claim 1-7 any claims synthesizes the method for black phosphorus and its answered on carbon paper
With, it is characterised in that the black phosphorus material on obtained carbon paper is in anode material for lithium-ion batteries and oxygen precipitation (OER) is prepared
Using.
9. a kind of one-step method according to any claim in claim 1-7 synthesized on carbon paper black phosphorus method and its
Using, it is characterised in that black phosphorus assembled battery has obvious discharge platform in 0.78V on the carbon paper of preparation, it was demonstrated that it is in 0.78V
Platform good reversibility；The chemical property of black phosphorus is good on the carbon paper of preparation, and first discharge specific capacity can reach 2234.5mAh
g-1；2234.1mAh·g-1；The stable cycle performance of black phosphorus positive electrode on the carbon paper of preparation, by 200 circle charge and discharge cycles
Afterwards, specific capacity still can reach 1677.3mAhg-1, 200 circle after capability retention be 75.14%；It is black on the carbon paper of preparation
The overpotential of phosphate material is 1.47V, and in 1.6V, current density can reach 100mAcm-2。
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| CN108059138A (en) * | 2017-12-11 | 2018-05-22 | 昆明理工大学 | A kind of preparation method of high-purity black phosphorus |
| CN109786628A (en) * | 2019-03-20 | 2019-05-21 | 广西师范大学 | A kind of preparation method and applications of cobalt nickel bimetal sulfide/carbon paper composite |
| CN111029594A (en) * | 2019-12-31 | 2020-04-17 | 南通大学 | Black phosphorus-TiO2nanotube/Ti anode direct methanol fuel cell |
| CN111129509A (en) * | 2019-12-31 | 2020-05-08 | 南通大学 | Direct methanol fuel cell anode catalyst and preparation method thereof |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109786628A (en) * | 2019-03-20 | 2019-05-21 | 广西师范大学 | A kind of preparation method and applications of cobalt nickel bimetal sulfide/carbon paper composite |
| CN111029594A (en) * | 2019-12-31 | 2020-04-17 | 南通大学 | Black phosphorus-TiO2nanotube/Ti anode direct methanol fuel cell |
| CN111129509A (en) * | 2019-12-31 | 2020-05-08 | 南通大学 | Direct methanol fuel cell anode catalyst and preparation method thereof |
| CN111029594B (en) * | 2019-12-31 | 2022-05-17 | 南通大学 | Black phosphorus-TiO2nanotube/Ti anode direct methanol fuel cell |
| CN111129509B (en) * | 2019-12-31 | 2022-05-17 | 南通大学 | Direct methanol fuel cell anode catalyst and preparation method thereof |
| 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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Application publication date: 20171117 |