CN108408772B - A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material - Google Patents

A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material Download PDF

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CN108408772B
CN108408772B CN201810390964.XA CN201810390964A CN108408772B CN 108408772 B CN108408772 B CN 108408772B CN 201810390964 A CN201810390964 A CN 201810390964A CN 108408772 B CN108408772 B CN 108408772B
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black phosphorus
transition metal
centrifugation
trisulfide
metal trisulfide
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萨百晟
周昊
杨洪雷
熊锐
朱龙鹏
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Fuzhou University
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Abstract

The invention discloses a kind of black phosphorus/transition metal trisulfide heterojunction material preparation methods, the technical solution adopted is that: the two-dimensional nano thin slice of transition metal trisulfide is prepared using presoma mixing method, and two-dimentional black phosphorus nano flake is obtained using the method for mechanical stripping, then transition metal trisulfide powder, black phosphorus powder and organic solvent are uniformly mixed, then black phosphorus/transition metal trisulfide hetero-junctions can be obtained after centrifugal treating.Heterojunction material produced by the present invention is combined with the natural Van der Waals for of storeroom, compared to traditional heterogenous junction epitaxy growth technique, is easier to prepare；And for the device made of such hetero-junctions compared to current block materials, volume is smaller, thinner, flexibility is more preferable, integrated level is higher, has more development potentiality.

Description

A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of black phosphorus/transition metal trisulfide hetero-junctions material The preparation method of material.
Background technique
Since graphene is found, two-dimensional semiconductor material, such as MoS2、WS2Deng because electronics, in terms of Increasingly attract the attention of numerous researchers with unique performance.Transition metal trisulfide MX3, it is typical model Moral China stacking material, wherein M represents Group IVB transition metals Ti, hafnium etc., and X represents chalcogen S, Se or Te.Also, scientist Two-dimentional black phosphorus is also found with thermal stability and excellent physics and chemical property.
Based on the permutation and combination of these two-dimension single layer materials, the two-dimentional Van der Waals hetero-junctions with different band structures It has been increasingly becoming current research hotspot.Novel heterojunction structure is constructed, surmounts independent two-dimensional material respectively Winnow-basket hedge, selects its technique It is excellent, learn from other's strong points to offset one's weaknesses, open up the wide world of heterojunction device.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, proposing a kind of two-dimentional black phosphorus/transition metal trisulfide The preparation method of heterojunction material is combined using two kinds of black phosphorus, transition metal trisulfide two-dimensional materials, is formd a kind of completely new Pn type hetero-junctions.This hetero-junctions is combined with the natural Van der Waals for of storeroom, raw compared to traditional heterogenous junction epitaxy Long technique is easier to prepare；And the device made of such hetero-junctions is compared to current block materials, volume is smaller, it is thinner, Flexibility is more preferable, integrated level is higher, has more development potentiality.
To achieve the above object, the present invention uses following technological means:
A kind of preparation step of black phosphorus/transition metal trisulfide heterojunction material is as follows:
(1) after grinding block black phosphorus, two-dimentional black phosphorus material is obtained through dissolution, ultrasound removing, centrifugation and cleaning；
(2) tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, stirring and dissolving is made into Then solution is ultrasonically treated again, be uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, make its icing, and by its into The processing of row vacuum freeze drying grinds after dry and obtains mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate region of aluminium oxide boat body, is forged Burning processing；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；Calcined product is finely ground, it is washed to Transition metal trisulfide powder is obtained until not having NaCl in product, after vacuum freeze drying；
(4) then by two dimension black phosphorus material made from transition metal trisulfide powder made from step (3), step (1) And it is in the agitator of 350r/min rotary cutter equipped with revolving speed that organic solvent, which is placed in, cutting stirring for 24 hours, is then allowed to stand at room temperature 8h, then by centrifugation, filtering and cleaning, obtain the black phosphorus/transition metal trisulfide heterojunction material.
In step (1), organic solvent needed for dissolving the black phosphorus after grinding is dimethyl sulfoxide, N, N- dimethyl formyl Amine, N-Methyl pyrrolidone are one such；In the ultrasonic strip step, supersonic frequency 30-50kHz, ultrasonic time For 20-40min；In the centrifugation step, centrifugal speed 10000-15000r/min, centrifugation time 10-50min；Institute The concrete operations for stating cleaning step are as follows: by the material dissolution after centrifugation in ethyl alcohol, supersound washing is simultaneously centrifuged, and then repeats to grasp Make 2 ~ 3 times；Wherein supersonic frequency is 30-50kHz, and ultrasonic time is 1 ~ 2min；Centrifugal rotational speed is 13000 ~ 14000r/min, Centrifugation time is 9 ~ 1lmin.
In step (2), the tetrachloride is titanium tetrachloride or hafnium tetrachloride.
According to the molar ratio, tetrachloride: thiocarbamide: sodium chloride: black phosphorus=1 ~ 1.2:3 ~ 4:150 ~ 250:1 ~ 1.2 or 1 ~ 1.2:3 ~ 4:150 ~ 250:2 ~ 2.4 or 2 ~ 2.4:6 ~ 8:150 ~ 250:1 ~ 1.2.
In step (2), mixing speed is 250r/min ~ 350r/min；The technological parameter of the ultrasonic treatment are as follows: supersonic frequency Rate is 30-50kHz, ultrasonic time 10-20min.
In step (2) and step (3), the temperature of the vacuum freeze drying is -40 DEG C ~ -60 DEG C.
The technological parameter of calcination processing described in step (3) are as follows: calcination temperature is 800 DEG C ~ 1000 DEG C, soaking time 4h ~ 8h。
Organic solvent described in step (4) is dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone It is one such or two kinds with isopropanol.
The beneficial effects of the present invention are: the invention proposes a kind of two-dimentional black phosphorus/transition metal trisulfide hetero-junctions The preparation method of material is combined using two kinds of black phosphorus, transition metal trisulfide two-dimensional materials, forms a kind of completely new pn type Hetero-junctions.This hetero-junctions is combined with the natural Van der Waals for of storeroom, compared to traditional heterogenous junction epitaxy growth technique, It is easier to prepare；And the device made of such hetero-junctions is compared to current block materials, and volume is smaller, thinner, flexibility More preferably, integrated level is higher, has more development potentiality.
Detailed description of the invention
Fig. 1 is black phosphorus/TiS made from embodiment 13The structure of hetero-junctions；
Fig. 2 is black phosphorus/TiS made from embodiment 13The XRD spectrum that 8 ° -70 ° of hetero-junctions；
Fig. 3 is black phosphorus/HfS made from embodiment 33The stereoscan photograph of hetero-junctions；
Fig. 4 is black phosphorus/HfS made from embodiment 33The optical absorption spectra of hetero-junctions；
Fig. 5 is black phosphorus/TiS made from embodiment 53The structure of/black phosphorus hetero-junctions；
Fig. 6 is black phosphorus/TiS made from embodiment 53The XRD spectrum that 8 ° -70 ° of hetero-junctions；
Fig. 7 is TiS made from embodiment 63/ black phosphorus/TiS3The structure of hetero-junctions.
Specific embodiment
Combined with specific embodiments below, the present invention is described in further detail, and of the invention protects content not limit to In following embodiment.It is all according to equivalent changes and modifications within the scope of the patent application of the present invention, should all belong to of the invention and cover model It encloses.
Embodiment 1
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Titanium: thiocarbamide: sodium chloride: black phosphorus=1:3:200:1.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in dimethyl sulfoxide, ultrasound removing, frequency 40kHz, the time is 30min, high speed centrifugation, centrifugal speed be 12500 r/min, time 30min, it is then that the mixed material containing two-dimentional black phosphorus is molten Solution is in ethyl alcohol, supersound washing, centrifugation, then repeatedly polar solvent supersound washing, centrifugation step 2 times；Wherein ultrasonic frequency For 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus material Material；
(2) titanium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 40kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 900 DEG C are heated to, 5h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；By calcined product It is finely ground, it is washed to until there is no NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtain two dimension TiS3Nano flake；
(4) then by two-dimentional TiS3Two dimension black phosphorus material made from nano flake, step (1) and dimethyl sulfoxide are placed in dress Have in the agitator that revolving speed is 350r/min rotary cutter, cutting stirring for 24 hours, is then allowed to stand 8h, then pass through centrifugation, mistake at room temperature Filter and cleaning, obtain two-dimentional black phosphorus/TiS3Hetero-junctions.
Embodiment 2
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Titanium: thiocarbamide: sodium chloride: black phosphorus=1:3:200:1.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in n,N-Dimethylformamide, ultrasound removing, frequency 40kHz, the time For 30min, high speed centrifugation, centrifugal speed is 12500 r/min, time 30min, then by the mixed material containing two-dimentional black phosphorus It is dissolved in ethyl alcohol, supersound washing, is centrifuged, then repeatedly polar solvent supersound washing, centrifugation step 2 times；Wherein ultrasonic frequency Rate is 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus material Material；
(2) titanium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 40kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa.The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 800 DEG C are heated to, 7h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；By calcined product It is finely ground, it is washed to until there is no NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtain two dimension TiS3Nano flake；
(4) then by two-dimentional TiS3Two dimension black phosphorus material made from nano flake, step (1) and dimethyl sulfoxide are placed in dress Have in the agitator that revolving speed is 350r/min rotary cutter, cutting stirring for 24 hours, is then allowed to stand 8h, then pass through centrifugation, mistake at room temperature Filter and cleaning, obtain two-dimentional black phosphorus/TiS3Hetero-junctions.
Embodiment 3
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Hafnium: thiocarbamide: sodium chloride: black phosphorus=1:3:200:1.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in N-Methyl pyrrolidone, ultrasound removing, frequency 40kHz, the time is 30min, high speed centrifugation, centrifugal speed be 12500 r/min, time 30min, it is then that the mixed material containing two-dimentional black phosphorus is molten Solution is in ethyl alcohol, supersound washing, centrifugation, then repeatedly polar solvent supersound washing, centrifugation step 3 times；Wherein ultrasonic frequency For 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus material Material；
(2) hafnium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 30kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 1000 DEG C are heated to, 4h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；Calcining is produced Object is finely ground, is washed to until not having NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtains two Tie up TiS3Nano flake；
(4) then by two-dimentional HfS3Two dimension black phosphorus material and N made from nano flake, step (1), N- dimethyl formyl It is in the agitator of 350r/min rotary cutter equipped with revolving speed that amine, which is placed in, and cutting stirring for 24 hours, is then allowed to stand 8h, then lead at room temperature Centrifugation, filtering and cleaning are crossed, two-dimentional black phosphorus/HfS is obtained3Hetero-junctions.
Embodiment 4
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Hafnium: thiocarbamide: sodium chloride: black phosphorus=1:3:200:1.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in n,N-Dimethylformamide, ultrasound removing, frequency 40kHz, when Between be 30min, high speed centrifugation, centrifugal speed be 12500 r/min, time 30min, then by the mixture containing two-dimentional black phosphorus Material is dissolved in ethyl alcohol, supersound washing, centrifugation, then repeatedly polar solvent supersound washing, centrifugation step 3 times；It is wherein ultrasonic Frequency is 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus Material；
(2) hafnium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 30kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa.The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 900 DEG C are heated to, 6h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；By calcined product It is finely ground, it is washed to until there is no NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtain two dimension HfS3Nano flake；
(4) then by two-dimentional HfS3Two dimension black phosphorus material made from nano flake, step (1) and isopropanol, which are placed in be equipped with, to be turned Speed is in the agitator of 350r/min rotary cutter, and cutting stirring for 24 hours, is then allowed to stand 8h at room temperature, then by centrifugation, filtering and Cleaning, obtains two-dimentional black phosphorus/HfS3Hetero-junctions.
Embodiment 5
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Titanium: thiocarbamide: sodium chloride: black phosphorus=1:3:200:2.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in dimethyl sulfoxide, ultrasound removing, frequency 40kHz, the time is 30min, high speed centrifugation, centrifugal speed be 12500 r/min, time 30min, it is then that the mixed material containing two-dimentional black phosphorus is molten Solution is in ethyl alcohol, supersound washing, centrifugation, then repeatedly polar solvent supersound washing, centrifugation step 2 times；Wherein ultrasonic frequency For 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus material Material；
(2) titanium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 50kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 900 DEG C are heated to, 5h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；By calcined product It is finely ground, it is washed to until there is no NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtain two dimension TiS3Nano flake；
(4) then by two-dimentional TiS3Two dimension black phosphorus material made from nano flake, step (1) and dimethyl sulfoxide are placed in dress Have in the agitator that revolving speed is 350r/min rotary cutter, cutting stirring for 24 hours, is then allowed to stand 8h, then pass through centrifugation, mistake at room temperature Filter and cleaning, obtain two-dimentional black phosphorus/TiS3Hetero-junctions.
Embodiment 6
A kind of black phosphorus/transition metal trisulfide heterojunction material, raw material composition are as follows: according to the molar ratio, four chlorinations Titanium: thiocarbamide: sodium chloride: black phosphorus=2:6:200:1.
Specific preparation process is as follows:
(1) block black phosphorus is ground, is dissolved in N-Methyl pyrrolidone, ultrasound removing, frequency 40kHz, the time is 30min, high speed centrifugation, centrifugal speed be 12500 r/min, time 30min, it is then that the mixed material containing two-dimentional black phosphorus is molten Solution is in ethyl alcohol, supersound washing, centrifugation, then repeatedly polar solvent supersound washing, centrifugation step 2 times；Wherein ultrasonic frequency For 40kHz, time 2min；Centrifugal rotational speed is 13500 r/min, and centrifugation time is 10min, obtains two-dimentional black phosphorus material Material；
(2) titanium tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, with mixing speed The magnetic stirring apparatus of 300r/min, stirring and dissolving wiring solution-forming are then super for the ultrasonic device ultrasound 15min(of 400W with power again Acoustic frequency is 50kHz), it is uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making solution freeze, and it is dry to place it in freezing - 50 DEG C of vacuum drying in dry machine, until drying obtains mixture, milled mixtures obtain mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and makes aluminium oxide boat body In vacuum degree be 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate high-temperature area of aluminium oxide boat body, and 1000 DEG C are heated to, 4h is kept the temperature；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；Calcining is produced Object is finely ground, is washed to until not having NaCl in product, carries out vacuum drying 8h at -50 DEG C in freeze drier, obtains two Tie up TiS3Nano flake；
(4) then by two-dimentional TiS3Two dimension black phosphorus material and N made from nano flake, step (1), N- dimethyl formyl It is in the agitator of 350r/min rotary cutter equipped with revolving speed that amine, which is placed in, and cutting stirring for 24 hours, is then allowed to stand 8h, then lead at room temperature Centrifugation, filtering and cleaning are crossed, two-dimentional black phosphorus/TiS is obtained3Hetero-junctions.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (6)

1. a kind of black phosphorus/transition metal trisulfide heterojunction material preparation method, it is characterised in that: include the following steps
(1) after grinding block black phosphorus, two-dimentional black phosphorus material is obtained through dissolution, ultrasound removing, centrifugation and cleaning；
(2) tetrachloride, thiocarbamide and sodium chloride of specified molar ratio are mixed and is dissolved in deionized water, stirring and dissolving is made into molten Then liquid is ultrasonically treated again, be uniformly mixed；Then acquired solution is placed in 0 DEG C hereinafter, making its icing, and carried out Vacuum freeze drying processing grinds after dry and obtains mix powder；
(3) it is passed through nitrogen detergent line, flow 400sccm, time 15min is then vacuumized, and is made in aluminium oxide boat body Vacuum degree is 4 × 10-3Pa；The mix powder that step (2) obtains is placed in the intermediate region of aluminium oxide boat body, is carried out at calcining Reason；It is cooled to room temperature under the protection of nitrogen after reaction, obtains calcined product；Calcined product is finely ground, it is washed to product In there is no NaCl until, transition metal trisulfide powder is obtained after vacuum freeze drying；
(4) and then by two dimension black phosphorus material made from transition metal trisulfide powder made from step (3), step (1) and have It is in the agitator of 350r/min rotary cutter equipped with revolving speed that solvent, which is placed in, and cutting stirring for 24 hours, is then allowed to stand 8h at room temperature, Again by centrifugation, filtering and cleaning, the black phosphorus/transition metal trisulfide heterojunction material is obtained；
In step (2), the tetrachloride is titanium tetrachloride or hafnium tetrachloride；
According to the molar ratio, tetrachloride: thiocarbamide: sodium chloride: black phosphorus=1 ~ 1.2:3 ~ 4:150 ~ 250:1 ~ 1.2 or 1 ~ 1.2:3 ~ 4: 150 ~ 250:2 ~ 2.4 or 2 ~ 2.4:6 ~ 8:150 ~ 250:1 ~ 1.2；
The technological parameter of calcination processing described in step (3) are as follows: calcination temperature is 800 DEG C ~ 1000 DEG C, soaking time 4h ~ 8h.
2. black phosphorus according to claim 1/transition metal trisulfide heterojunction material preparation method, feature exist In: in step (1), organic solvent needed for dissolving the black phosphorus after grinding is dimethyl sulfoxide, n,N-Dimethylformamide, N- Methyl pyrrolidone is one such；In the ultrasonic strip step, supersonic frequency 30-50kHz, ultrasonic time 20- 40min；In the centrifugation step, centrifugal speed 10000-15000r/min, centrifugation time 10-50min.
3. black phosphorus according to claim 1/transition metal trisulfide heterojunction material preparation method, feature exist In: in step (1), the concrete operations of the cleaning step are as follows: by the material dissolution after centrifugation in ethyl alcohol, supersound washing is simultaneously Centrifugation, then repetitive operation 2 ~ 3 times；Wherein supersonic frequency is 30-50kHz, and ultrasonic time is 1 ~ 2min；Centrifugal rotational speed is 13000 ~ 14000r/min, centrifugation time are 9 ~ 1lmin.
4. black phosphorus according to claim 1/transition metal trisulfide heterojunction material preparation method, feature exist In: in step (2), mixing speed is 250r/min ~ 350r/min；The technological parameter of the ultrasonic treatment are as follows: supersonic frequency is 30-50kHz, ultrasonic time 10-20min.
5. black phosphorus according to claim 1/transition metal trisulfide heterojunction material preparation method, feature exist In: in step (2) and step (3), the temperature of the vacuum freeze drying is -40 DEG C ~ -60 DEG C.
6. black phosphorus according to claim 1/transition metal trisulfide heterojunction material preparation method, feature exist In: organic solvent described in step (4) is dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone and isopropyl Alcohol is one such or two kinds.
CN201810390964.XA 2018-04-27 2018-04-27 A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material Expired - Fee Related CN108408772B (en)

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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
CN106384811A (en) * 2016-10-14 2017-02-08 福州大学 Blue phosphorus/transition metal disulfide heterojunction anode material and preparation method thereof
CN107117590A (en) * 2017-06-14 2017-09-01 合肥工业大学 A kind of method that gradient sphere grinding prepares two-dimentional black phosphorus

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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
CN106384811A (en) * 2016-10-14 2017-02-08 福州大学 Blue phosphorus/transition metal disulfide heterojunction anode material and preparation method thereof
CN107117590A (en) * 2017-06-14 2017-09-01 合肥工业大学 A kind of method that gradient sphere grinding prepares two-dimentional black phosphorus

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