CN108284220A - A kind of bismuth alkene nanometer sheet and preparation method thereof - Google Patents
A kind of bismuth alkene nanometer sheet and preparation method thereof Download PDFInfo
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- CN108284220A CN108284220A CN201711431413.5A CN201711431413A CN108284220A CN 108284220 A CN108284220 A CN 108284220A CN 201711431413 A CN201711431413 A CN 201711431413A CN 108284220 A CN108284220 A CN 108284220A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B22F1/0551—Flake form nanoparticles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of preparation methods of bismuth alkene nanometer sheet, including:(1) in organic solvent by bismuth meal dispersion, dispersion liquid is obtained;(2) first time water bath sonicator first is carried out to the dispersion liquid, then carries out probe type ultrasonic, obtain the first ultrasonic liquid;Then second of water bath sonicator is carried out to the described first ultrasonic liquid, obtains the second ultrasonic liquid;(3) Ultra-Low Speed centrifugation at 2000 4000rpm is carried out to the described second ultrasonic liquid, collects supernatant, low-speed centrifugal is then carried out at 5000 7000rpm to the supernatant, collect precipitation, gained precipitation is bismuth alkene nanometer sheet.This method easy to operate, favorable reproducibility simple for process, the good bismuth alkene nanometer sheet of the controllable monodispersity of easily obtained size.The present invention also provides bismuth alkene nanometer sheets obtained.
Description
Technical field
The present invention relates to two-dimensional material fields, more particularly to a kind of bismuth alkene nanometer sheet and preparation method thereof.
Background technology
Two-dimensional material, refer to electronics only can on the non-nanosize (1-100nm) of two dimensions free movement (plane transport
It is dynamic) material, such as nano thin-film.Univ Manchester UK two scientists An Deliegaimu and Ke Siteyanuowo disappear
Graphene was made with tape method in 2004 in love for the first time.Hereafter black phosphorus (phosphorus alkene), silene, germanium alkene, antimony alkene, boron nitride, two
A series of quasi- two-dimensional material of only monoatomic layer thickness such as molybdenum sulfide is found in succession.
Bismuth alkene (Bismuthene) be it is a kind of by bulk metal bismuth remove from two-dimensional material, there is similar graphene
Structure.But bismuth alkene is the direct band-gap semicondictor (conduction band bottom and valence band at the top of in same position) for having 0.306eV energy gaps, can be with
Light direct-coupling, absorption spectrum ranges are wider.Further, since the biocompatibility of bismuth element is strong, bio-toxicity is small, therefore bismuth alkene exists
Optics, electricity, biologic pharmacological science etc. have wide application potential.And two-dimentional bismuth alkene lamellar structure carries medicine, light in biology
The fields such as heat, optical dynamic therapy are a kind of potential biomedical base materials.
Currently, being by mechanically pulling off method (such as adhesive tape tears point-score), chemical vapour deposition technique technology to prepare lamella
Bismuth alkene material.But the yield of the sheet bismuth alkene material of mechanical stripping method preparation is relatively low, is not suitable for commercially producing, and operate
It is cumbersome, time-consuming;And the amount of bismuth alkene prepared by chemical vapour deposition technique is less, and be not easy to repeat.
Invention content
In consideration of it, the present invention provides a kind of bismuth alkene nanometer sheet and preparation method thereof, the preparation method is by surpassing probe
Sound and water bath sonicator are combined, and by the stripping to act synergistically to realize to bismuth meal, obtain that monodispersity is good, bismuth of size uniformity
Alkene nanometer sheet.This method it is simple for process easy to operate, favorable reproducibility, the yield of bismuth alkene nanometer sheet or yield are higher, easily realize low
Cost industrial metaplasia is produced.
In a first aspect, the present invention provides a kind of preparation method of bismuth alkene nanometer sheet, include the following steps:
(1) in organic solvent by bismuth meal dispersion, dispersion liquid is obtained;Wherein, a concentration of 0.5- of the bismuth meal in dispersion liquid
10mg/mL;
(2) first time water bath sonicator first is carried out to the dispersion liquid, the power of the first time water bath sonicator is 400-
600W, time are 1-6 hours;Probe type ultrasonic is carried out in the case where power is 1080-1800W 10-24 hours, obtain the first ultrasound again
Liquid;
Then second of water bath sonicator is carried out to the described first ultrasonic liquid, obtains the second ultrasonic liquid;Wherein, described second
The power of water bath sonicator is 400-600W;
(3) Ultra-Low Speed centrifugation at 2000-4000rpm is carried out to the described second ultrasonic liquid, supernatant is collected, then to institute
It states supernatant and carries out low-speed centrifugal at 5000-7000rpm, collect precipitation, gained precipitation is bismuth alkene nanometer sheet.
Optionally, the organic solvent includes N-Methyl pyrrolidone (NMP), dimethylformamide (DMF), dimethyl Asia
It is one or more in sulfone (DMSO), acetone, tetrahydrofuran, absolute ethyl alcohol, methanol, isopropanol, chloroform and dichloromethane,
But not limited to this.The surface energy of organic solvent used and the surface energy of two-dimensional layer bismuth alkene material match, and exist therebetween
Certain interaction balances the stripping required energy of bismuth meal.
Optionally, the grain size of the bismuth meal is no more than 75 μm.Such as 55-70 μm, 1-50 μm, 2-45 μm or 1-4 μm.Into one
Optionally, the grain size of the bismuth meal is no more than 50 μm to step.
In the embodiment of the present invention, the power of the first time water bath sonicator can be 400W, 450W, 500W, 550W, 580W
Or 600W.Optionally, the power of the first time water bath sonicator is 420-600W.
Optionally, the time of second of water bath sonicator is 1-6 hours.It is further chosen as 1-3 hours.
Wherein, the power of second of water bath sonicator can be 400W, 450W, 500W, 550W, 580W or 600W.It can
The power of selection of land, second of water bath sonicator is 420-600W.The power of second of water bath sonicator or time can be with
The power of the first time water bath sonicator or time are identical or different.
In the embodiment of the present invention, the power of the probe-type ultrasound can be 1100W, 1200W, 1300W, 1400W,
1500W, 1600W or 1700W.Optionally, the power of the probe type ultrasonic is 1200-1700W.
In the embodiment of the present invention, time of the probe-type ultrasound can be 10h, 12h, 15h, 20h or for 24 hours.Optionally,
The time of the probe type ultrasonic is 12-24 hours.
Optionally, the probe-type ultrasound is carried out in condition of ice bath of the temperature no more than 10 DEG C.Preferably, the spy
Temperature when pin type ultrasound is 0-10 DEG C, further preferably 4-10 DEG C.The condition of ice bath refers in probe-type ultrasound
It in the process, will be equipped with waiting for that the container of solution of ultrasound is placed in another container equipped with ice cube (such as beaker, test tube).
Optionally, the first time water bath sonicator be temperature be 5-10 DEG C at carry out.
Optionally, second of water bath sonicator be temperature be 5-10 DEG C at carry out.
Optionally, the centrifugation time of the Ultra-Low Speed centrifugation is 15-30min.For example, 12,15,20,25 or 30min.
Optionally, the rotating speed of the Ultra-Low Speed centrifugation is 2000-3000rpm.
Optionally, the centrifugation time of the Ultra-Low Speed centrifugation is 15-30min.For example, 12,15,20,25 or 30min.
Optionally, the rotating speed of the low-speed centrifugal is 6000-7000rpm.
The precipitation (i.e. bismuth alkene nanometer sheet) obtained after the low-speed centrifugal can be in redisperse to the second solvent, to obtain bismuth-containing
The solution of alkene nanometer sheet.Optionally, second solvent include N-Methyl pyrrolidone (NMP), dimethylformamide (DMF),
It is one or more in dimethyl sulfoxide (DMSO) (DMSO), acetone, tetrahydrofuran, absolute ethyl alcohol, methanol and isopropanol.
In the present invention, the first time water bath sonicator to bismuth meal dispersion liquid is tentatively to be beaten bismuth meal by ultrasonic Cavitation effect
It is broken, so that its part is dissolved in organic solvent, can avoid directly using loss of the probe type ultrasonic to probe type ultrasonic instrument, extends super
The sound time;Next probe-type ultrasound is that the bismuth meal that will tentatively smash is smashed, removes bismuth alkene at lamellar structure in large quantities, is made
It is largely dissolved in organic solvent;Bismuth alkene stratified material after stripping can be further broken by second last of water bath sonicator
Smaller particle obtains bismuth alkene nanometer sheet, and is further ensured that and will not reunite, subsequently to carry out centrifugal purification processing.
The preparation method for the bismuth alkene nanometer sheet that first aspect present invention provides, probe sonication and water bath sonicator are combined
Liquid phase stripping method, by the stripping to act synergistically to realize to bismuth meal, the method is simple for process easy to operate, and yield is higher, compares
Current mechanical stripping method and chemical vapour deposition technique etc. have apparent advantage, can get the good bismuth of the controllable monodispersity of size
Alkene nanometer sheet easily realizes inexpensive industrialization production.This lays the foundation for application of the bismuth alkene nanometer sheet in biomedical sector.
Second aspect, the present invention also provides the bismuth alkene nanometer sheets being prepared by above-mentioned preparation method.The bismuth alkene is received
The thickness of rice piece is in 20nm hereinafter, the lateral dimension of the bismuth alkene nanometer sheet is 100nm~10 μm.Wherein, lateral dimension refers to
The length or width of bismuth alkene nanometer sheet.
Optionally, the lateral dimension of the bismuth alkene nanometer sheet is 200nm~10 μm.For example, 300nm, 500nm, 800nm,
1 μm, 2 μm, 5 μm, 8 μm or 10 μm.
Optionally, the lateral dimension of the bismuth alkene nanometer sheet is 500nm~10 μm.
Optionally, the lateral dimension of the bismuth alkene nanometer sheet is 1 μm~10 μm.
Wherein, the bismuth alkene nanometer sheet includes that the single layer bismuth alkene of one layer of bismuth alkene or multilayer repeats on its vertical in-plane
It stacks.
Optionally, the thickness of the bismuth alkene nanometer sheet is 0.3-15nm.
Optionally, the bismuth alkene nanometer sheet is 1~64 atomic layer level thickness.That is, by 1-64 layers single layer bismuth alkene stack and
At.Still optionally further, the thickness of the bismuth alkene nanometer sheet is
Optionally, the bismuth alkene that the bismuth alkene nanometer sheet is 1~10 layer stacks.The thickness of the bismuth alkene nanometer sheet is
0.3-3nm。
Optionally, the shapes such as the shape of the bismuth alkene nanometer sheet is including but not limited to rectangular, round, triangle, polygon.
The shape of bismuth alkene nanometer sheet provided by the invention is more regular, size is more uniform, and preferably, toxicity is smaller for dispersibility,
Convenient for being used to prepare the fields such as optics, electricity, biological medicine (such as preparing photo-thermal therapy drug, optical markings drug).
The advantages of embodiment of the present invention, will partly illustrate in the following description, a part according to specification be it is aobvious and
Be clear to, or can be through the embodiment of the present invention implementation and know.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo of bismuth alkene nanometer sheet made from the embodiment of the present invention;
Fig. 2 is the analysis result of the atomic force microscope (AFM) of bismuth alkene nanometer sheet made from the embodiment of the present invention;
Fig. 3 is the raman spectrum of bismuth alkene nanometer sheet made from the embodiment of the present invention;
Fig. 4 is ultraviolet-visible-near infrared absorption light of the bismuth alkene nanometer sheet in nmp solvent made from the embodiment of the present invention
Spectrogram.
Specific implementation mode
As described below is the preferred embodiment of the embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, under the premise of not departing from principle of the embodiment of the present invention, several improvements and modifications can also be made, these improvement
The protection domain of the embodiment of the present invention is also considered as with retouching.
Divide multiple embodiments that the embodiment of the present invention is further detailed below.The embodiment of the present invention be not limited to
Under specific embodiment.In the range of constant principal right, implementation appropriate can be changed.
Embodiment 1
A kind of preparation method of bismuth alkene nanometer sheet, includes the following steps:
(1) the another name for Sichuan Province ox vial for taking a 250mL capacity, is packed into the nmp solvent of 120mL, adds 200 mesh of 120mg
(200/per square inch namely grain size is 0.074mm) bismuth meal, it is that 1mg/mL (or is to obtain bismuth meal initial concentration
Dispersion liquid 1000ppm);
(2) vial in (1) is placed in new sesame ultrasonic constant-temperature cleaning machine SBL-22DT, with maximum under 10 DEG C of constant temperature
70% (i.e. with the power of 420W) of power (600W) carries out water bath sonicator 3 hours;
Water bath sonicator and then acquired solution is placed in than (1800W maximum works in bright cell crushing instrument BILON-1800Y
Rate), at 4 DEG C, Probe Ultrasonic Searching is carried out 24 hours with 60% power (i.e. the power of 1080W), obtains the first ultrasonic liquid;
Then the described first ultrasonic liquid is placed in again in new sesame ultrasonic constant-temperature cleaning machine SBL-22DT, under 10 DEG C of constant temperature
With 70% power, second of progress water bath sonicator 3 hours, the second ultrasonic liquid is obtained;
(3) 4 parts are equally divided into the described second ultrasonic liquid, move into 50mL centrifuge tubes, is existed using He Xi HR20MW centrifuges
(5000g centrifugal force) carries out centrifugation 20 minutes under 3000rpm rotating speeds, and gained supernatant is moved into 4 new 50mL respectively to be centrifuged
Guan Zhong, (11667g centrifugal force) carries out centrifugation 20 minutes under 7000rpm rotating speeds, is precipitated in collecting pipe, as required bismuth
Alkene nanometer sheet (about 71.4mg).
Being computed can obtain, and in the embodiment of the present invention 1, the yield of the bismuth alkene nanometer sheet is 71.4mg/120mg=
59.5%.
Embodiment 2
A kind of preparation method of bismuth alkene nanometer sheet, includes the following steps:
(1) the another name for Sichuan Province ox vial for taking a 500mL capacity, is packed into the nmp solvent of 400mL, adds 300 mesh of 200mg
Bismuth meal obtains the dispersion liquid that bismuth meal initial concentration is 0.5mg/mL;
(2) vial in (1) is placed in new sesame ultrasonic constant-temperature cleaning machine SBL-22DT, with 480W under 4 DEG C of constant temperature
Power carry out water bath sonicator 2 hours;
Water bath sonicator and then acquired solution is placed in than (1800W maximum works in bright cell crushing instrument BILON-1800Y
Rate), Probe Ultrasonic Searching is carried out 15 hours with 75% power (i.e. the power of 1350W), obtains the first ultrasonic liquid;
Then the described first ultrasonic liquid is placed in again in new sesame ultrasonic constant-temperature cleaning machine SBL-22DT, with the power of 450W
It carries out second water bath sonicator 3 hours, obtains the second ultrasonic liquid;
(3) 4 parts are equally divided into the described second ultrasonic liquid, move into 50mL centrifuge tubes, is existed using He Xi HR20MW centrifuges
It is centrifuged 30 minutes under 2000rpm rotating speeds, gained supernatant is moved into respectively in 4 new 50mL centrifuge tubes, turned then at 6500rpm
The lower centrifugation of speed 25 minutes, the interior precipitation of collecting pipe, as required bismuth alkene nanometer sheet (yield 65%).
Fig. 1 is scanning electron microscope (SEM) photo of bismuth alkene nanometer sheet made from the embodiment of the present invention.It can from Fig. 1
Find out there are a large amount of apparent flaky substances, i.e. bismuth alkene nanometer sheet in figure.Amplification sees that visible apparent layer structure, explanation are adopted
Required bismuth alkene nanometer sheet can be stripped out with the preparation method of the present invention.The lateral dimension of the bismuth alkene nanometer sheet 100nm~
10 μm, by one or more layers single layer bismuth alkene, repeatedly stacking forms stratiform feather spline structure on its vertical in-plane.It is formed
The thickness of the bismuth alkene nanometer sheet be
Fig. 2 is the analysis result of the atomic force microscope (AFM) of bismuth alkene nanometer sheet made from the embodiment of the present invention.Figure memory
In the laminated structure that a large amount of thickness are 3nm (Δ Z), illustrate that preparation method provided by the invention can successfully be removed to form bismuth alkene nanometer
Piece, the bismuth alkene nanometer agreement that contracts a film or TV play to an actor or actress are stacked by 10 layers of single layer bismuth alkene, that is, the bismuth alkene nanometer sheet is 10 bismuth atom thickness
Degree.
Fig. 3 is the Raman curve graph of bismuth alkene nanometer sheet made from the embodiment of the present invention.Under the excitation wavelength of 1064nm,
70cm-1And 97cm-1(correspond respectively to the E of Bi elementsgAnd A1gVibrating mould) the two characteristic peaks are all more apparent, and this illustrates this
The peelable formation bismuth alkene nanometer sheet of preparation method provided is provided.
Fig. 4 is ultraviolet-visible-near infrared absorption light of the bismuth alkene nanometer sheet in nmp solvent made from the embodiment of the present invention
Spectrogram.From fig. 4, it can be seen that bismuth alkene nanometer sheet provided by the invention shows apparent absorption characteristic in the regions 300-1100nm.
For prominent beneficial effects of the present invention, present invention is alternatively directed to embodiments 1, and following comparative example is arranged:
Comparative example 1 and embodiment 1 difference lies in:In step (2), Probe Ultrasonic Searching is carried out only with than bright cell crushing instrument
24 hours;
Comparative example 2 and embodiment 1 difference lies in:It is first super using probe is carried out than bright cell crushing instrument in step (2)
Sound, then carry out water bath sonicator;
Comparative example 3 and embodiment 1 difference lies in:In step (2), water bath sonicator is first carried out, then carry out probe type ultrasonic,
Without Secondary water-bath ultrasound is carried out after probe type ultrasonic again again.
Product made from comparative example 1 is compared with the bismuth alkene nanometer sheet of embodiment 1, and lateral dimension is mainly at 1 μm or more, institute
The yield for stating bismuth alkene nanometer sheet is 63.9mg/120mg=53.25%.
Compared with Example 1, the yield of bismuth alkene nanometer sheet is 67.8mg/120mg=to product made from comparative example 2
56.5%.Wherein, also contain nanometer sheet of many lateral dimensions at 1 μm or more.
Compared with Example 1, the yield of the bismuth alkene nanometer sheet is 68.2mg/120mg=to product made from comparative example 3
56.83%.And the product of comparative example 3 is disperseing in organic solvent, micro agglomeration to be had after standing 6 hours.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of preparation method of bismuth alkene nanometer sheet, which is characterized in that include the following steps:
(1) in organic solvent by bismuth meal dispersion, dispersion liquid is obtained;Wherein, a concentration of 0.5-10mg/ of the bismuth meal in dispersion liquid
mL;
(2) first time water bath sonicator first being carried out to the dispersion liquid, the power of the first time water bath sonicator is 400-600W, when
Between be 1-6 hours;Probe type ultrasonic is carried out in the case where power is 1080-1800W 10-24 hours, obtain the first ultrasonic liquid again;
Then second of water bath sonicator is carried out to the described first ultrasonic liquid, obtains the second ultrasonic liquid;Wherein, second of water-bath
The power of ultrasound is 400-600W;
(3) Ultra-Low Speed centrifugation carried out at 2000-4000rpm to the described second ultrasonic liquid, collection supernatant, then on described
Clear liquid carries out low-speed centrifugal at 5000-7000rpm, collects precipitation, and gained precipitation is bismuth alkene nanometer sheet.
2. preparation method as described in claim 1, which is characterized in that the grain size of the bismuth meal is no more than 75 μm.
3. preparation method as described in claim 1, which is characterized in that the organic solvent includes N-Methyl pyrrolidone, two
In methylformamide, dimethyl sulfoxide (DMSO), acetone, tetrahydrofuran, absolute ethyl alcohol, methanol, isopropanol, chloroform and dichloromethane
It is one or more.
4. preparation method as described in claim 1, which is characterized in that the power of the first time water bath sonicator is 400-
600W。
5. preparation method as described in claim 1, which is characterized in that the power of second of water bath sonicator is 400-
600W;The time of second of water bath sonicator is 1-6 hours.
6. preparation method as described in claim 1, which is characterized in that it is 5-10 DEG C that the first time water bath sonicator, which is in temperature,
Lower progress;The probe-type ultrasound is carried out in condition of ice bath of the temperature no more than 10 DEG C;Second of water bath sonicator be
It is carried out at being 5-10 DEG C in temperature.
7. preparation method as described in claim 1, which is characterized in that the rotating speed of the Ultra-Low Speed centrifugation is 2000-
3000rpm;The rotating speed of the low-speed centrifugal is 6000-7000rpm.
8. a kind of bismuth alkene nanometer sheet, which is characterized in that the thickness of the bismuth alkene nanometer sheet is in 20nm hereinafter, the bismuth alkene nanometer sheet
Lateral dimension be 100nm~10 μm.
9. bismuth alkene nanometer sheet as claimed in claim 8, which is characterized in that the lateral dimension of the bismuth alkene nanometer sheet is 200nm
~10 μm;The thickness of the bismuth alkene nanometer sheet is 0.3-15nm.
10. bismuth alkene nanometer sheet as claimed in claim 8, which is characterized in that the bismuth alkene nanometer sheet includes 1-64 layers of single layer
Bismuth alkene stacks.
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WO2019128247A1 (en) * | 2017-12-26 | 2019-07-04 | 深圳大学 | Bismuthene nanosheets and preparation method therefor |
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