CN108145171A - 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 PDF

Info

Publication number
CN108145171A
CN108145171A CN201711429956.3A CN201711429956A CN108145171A CN 108145171 A CN108145171 A CN 108145171A CN 201711429956 A CN201711429956 A CN 201711429956A CN 108145171 A CN108145171 A CN 108145171A
Authority
CN
China
Prior art keywords
bismuth
nanometer sheet
alkene nanometer
water bath
bismuth alkene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711429956.3A
Other languages
Chinese (zh)
Other versions
CN108145171B (en
Inventor
张晗
黄浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen University
Original Assignee
Shenzhen University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen University filed Critical Shenzhen University
Priority to CN201711429956.3A priority Critical patent/CN108145171B/en
Publication of CN108145171A publication Critical patent/CN108145171A/en
Priority to PCT/CN2018/099563 priority patent/WO2019128245A1/en
Application granted granted Critical
Publication of CN108145171B publication Critical patent/CN108145171B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/056Submicron particles having a size above 100 nm up to 300 nm
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0551Flake form nanoparticles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/068Flake-like particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The present invention provides a kind of preparation method of bismuth alkene nanometer sheet, including:(1) by bismuth meal dispersion in organic solvent, dispersion liquid is obtained;(2) first time water bath sonicator first is carried out to the dispersion liquid, obtains the first ultrasonic liquid;Described first ultrasonic liquid is placed in closed container, heating reaction 12 24 hours at being 140 200 DEG C in temperature;After completion of the reaction, it is cooled to room temperature, second of water bath sonicator is carried out to gained reaction solution, obtain the second ultrasonic liquid;(3) to described second, ultrasonic liquid carries out Ultra-Low Speed centrifugation under 2000 4000rpm, collects supernatant, then carries out low-speed centrifugal under 5000 7000rpm to the supernatant, collects precipitation, and 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

A kind of bismuth alkene nanometer sheet and preparation method thereof
Technical field
The present invention relates to two-dimensional material field, 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 adhesive 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) is a kind of two-dimensional material removed by bulk metal bismuth, has 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.
At present, method (such as adhesive tape tears point-score), chemical vapour deposition technique technology are by mechanically pulling off to prepare lamella Bismuth alkene material.But the yield of sheet bismuth alkene material prepared by mechanical stripping method is relatively low, is not suitable for commercially producing, and operates It is cumbersome, time-consuming;And the amount of bismuth alkene prepared by chemical vapour deposition technique is less, and is 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 the way that probe is surpassed 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) by bismuth meal dispersion in organic solvent, dispersion liquid is obtained;Wherein, bismuth meal is in a concentration of 0.5- of dispersion liquid 10mg/mL;
(2) first time water bath sonicator first is carried out to the dispersion liquid, obtains the first ultrasonic liquid;The first time water bath sonicator Power for 400-600W, the time is 1-6 hours;
Described first ultrasonic liquid is placed in closed container, heating reaction 12-24 hours at being 140-200 DEG C in temperature;
After completion of the reaction, it is cooled to room temperature, second of water bath sonicator is carried out to gained reaction solution, obtain the second ultrasonic liquid; Wherein, the power of second of water bath sonicator is 400-600W;
(3) to described second, ultrasonic liquid carries out Ultra-Low Speed centrifugation under 2000-4000rpm, supernatant is collected, then to institute It states supernatant and low-speed centrifugal is carried out under 5000-7000rpm, collect precipitation, gained precipitation is bismuth alkene nanometer sheet.
Optionally, it is sub- to include N-Methyl pyrrolidone (NMP), dimethylformamide (DMF), dimethyl for the organic solvent 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 of organic solvent used can match with the surface of two-dimensional layer bismuth alkene material, 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 Selection of land, the power of 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.
Optionally, the first time water bath sonicator, second of water bath sonicator are in condition of ice bath of the temperature no more than 10 DEG C It carries out.Preferably 0-10 DEG C, further preferably 4-10 DEG C.The condition of ice bath, refers in ultrasonic procedure, will be equipped with and wait to surpass The container of the solution of sound is placed in another container equipped with ice cube (such as beaker, test tube).
Still optionally further, the first time water bath sonicator is to carry out at 5-10 DEG C in temperature.
Still optionally further, second of water bath sonicator is to carry out at 5-10 DEG C in temperature.
Optionally, in step (2), the temperature of the heating reaction is 165-200 DEG C.For example, 170,180,190 or 200 ℃。
Optionally, in step (2), the time of the heating reaction is 19-24 hours.For example, 20,22 or 24 hours.
Optionally, in step (2), the closed container is autoclave (such as ptfe autoclave) or three mouthfuls Bottle.
Further, it is preferable to ground, when the closed container is there-necked flask, also carries out during the heating reaction Stirring, wherein, the speed of the stirring is 1000-2500 revs/min.
Optionally, in step (3), 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, its part is made to dissolve in organic solvent;Next solvent thermal reaction, can by organic solvent under high temperature facing at high temperature Boundary's state activity further smashes the bismuth meal tentatively smashed in large quantities, removes bismuth alkene into lamellar structure, it is made, which largely to dissolve in, has In solvent;Bismuth alkene stratified material after stripping can be further broken into smaller particle by second last of water bath sonicator, Bismuth alkene nanometer sheet is obtained, 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, water bath sonicator and solvent-thermal method are combined Liquid phase stripping method by the stripping to act synergistically to realize to bismuth meal, obtains the bismuth alkene product of different scale, then by centrifuge come The bismuth alkene nanometer sheet of size needed for acquisition.The method is simple for process easy to operate, and yield is higher, compared to current mechanical stripping method and Chemical vapour deposition technique etc. has apparent advantage, can obtain the good bismuth alkene nanometer sheet of the controllable monodispersity of size, easily realize low Cost industrial metaplasia is produced.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 one layer of bismuth alkene or the individual layer bismuth alkene of 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 individual layer bismuth alkene stack and Into.Still optionally further, the thickness of the bismuth alkene nanometer sheet is-19.84nm。
Optionally, the bismuth alkene nanometer sheet is that 1~10 layer of bismuth alkene 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 Implementation being clear to or can be through the embodiment of the present invention 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 spectrogram 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 made from the embodiment of the present invention in nmp solvent Spectrogram.
Specific embodiment
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 principle of the embodiment of the present invention is not departed from, 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 can be suitably 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 of a 250mL capacity is taken, 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 first time water bath sonicator 3 hours, obtains the first ultrasonic liquid;
After first time water bath sonicator, the ultrasonic liquid of gained first is moved into the reaction kettle that capacity is 150mL and (gives Shen in Shanghai Instrument Ltd.), it is heated to 140 DEG C and is kept for 24 hours;
After completion of the reaction, it is cooled to room temperature, all substances in reaction kettle is all moved into 250mL another name for Sichuan Province ox vial, then It is small with 70% power, second of water bath sonicator 4 of progress under 10 DEG C of constant temperature using new sesame ultrasonic constant-temperature cleaning machine SBL-22DT When, obtain the second ultrasonic liquid;
(3) to described second, ultrasonic liquid is equally divided into 4 parts, moves 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 centrifuges 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).
It is computed to obtain, 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 of a 500mL capacity is taken, 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 first time water bath sonicator 2 hours, obtain the first ultrasonic liquid;
After first time water bath sonicator, the ultrasonic liquid of gained first is moved into the reaction kettle that capacity is 150mL and (gives Shen in Shanghai Instrument Ltd.), it is heated to 140 DEG C and is kept for 24 hours;
After completion of the reaction, it is cooled to room temperature, all substances in reaction kettle is all moved into 250mL another name for Sichuan Province ox vial, use New sesame ultrasonic constant-temperature cleaning machine SBL-22DT with power second of the progress water bath sonicator 3 hours of 450W, obtains the second ultrasound Liquid;
(3) to described second, ultrasonic liquid is equally divided into 4 parts, moves 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, collecting pipe is interior to be precipitated, 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.Visible apparent layer structure is seen in amplification, and explanation is 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 individual 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-19.84nm。
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 3-4nm (Δ Z), illustrate that preparation method provided by the invention can be removed successfully to form bismuth alkene and receive Rice piece, the bismuth alkene nanometer agreement that contracts a film or TV play to an actor or actress are stacked by 10-13 layers of individual layer bismuth alkene, that is, the bismuth alkene nanometer sheet is former for 10-13 bismuth Molecular layers thick.
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 the preparation method provided is provided.
Fig. 4 is ultraviolet-visible-near infrared absorption light of the bismuth alkene nanometer sheet made from the embodiment of the present invention in nmp solvent Spectrogram.From fig. 4, it can be seen that bismuth alkene nanometer sheet provided by the invention shows apparent absorption characteristic in 300-1100 nm regions.
For prominent beneficial effects of the present invention, present invention is alternatively directed to embodiments 1 to set following comparative example:
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, bismuth The yield of alkene nanometer sheet is 62.5mg/120mg=52.8%.
Compared with Example 1, the yield of the bismuth alkene nanometer sheet is 66.2mg/120mg=to product made from comparative example 2 55.1%.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 65.5mg/120mg=to product made from comparative example 3 54.8%.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 made within refreshing and principle etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of preparation method of bismuth alkene nanometer sheet, which is characterized in that include the following steps:
(1) by bismuth meal dispersion in organic solvent, dispersion liquid is obtained;Wherein, bismuth meal is in a concentration of 0.5-10mg/ of dispersion liquid mL;
(2) first time water bath sonicator first is carried out to the dispersion liquid, obtains the first ultrasonic liquid;The work(of the first time water bath sonicator Rate is 400-600W, and the time is 1-6 hours;
Described first ultrasonic liquid is placed in closed container, heating reaction 12-24 hours at being 140-200 DEG C in temperature;
After completion of the reaction, it is cooled to room temperature, second of water bath sonicator is carried out to gained reaction solution, obtain the second ultrasonic liquid;Wherein, The power of second of water bath sonicator is 400-600W;
(3) to described second, ultrasonic liquid carries out Ultra-Low Speed centrifugation under 2000-4000rpm, collection supernatant, then on described Clear liquid carries out low-speed centrifugal under 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 temperature of the heating reaction is 165-200 DEG C;It is described The time of heating reaction is 19-24 hours.
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 1-3 hours.
6. preparation method as described in claim 1, which is characterized in that the first time water bath sonicator be temperature be 5-10 DEG C Lower progress;Second of water bath sonicator is to carry out at 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.
It is 8. a kind of such as claim 1-7 any one of them bismuth alkene nanometer sheets, which is characterized in that the thickness of the bismuth alkene nanometer sheet In 20nm hereinafter, the lateral dimension of the bismuth alkene nanometer sheet is 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 individual layer Bismuth alkene stacks.
CN201711429956.3A 2017-12-26 2017-12-26 Bismuth-alkene nanosheet and preparation method thereof Active CN108145171B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201711429956.3A CN108145171B (en) 2017-12-26 2017-12-26 Bismuth-alkene nanosheet and preparation method thereof
PCT/CN2018/099563 WO2019128245A1 (en) 2017-12-26 2018-08-09 Bismuthene nanosheet and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711429956.3A CN108145171B (en) 2017-12-26 2017-12-26 Bismuth-alkene nanosheet and preparation method thereof

Publications (2)

Publication Number Publication Date
CN108145171A true CN108145171A (en) 2018-06-12
CN108145171B CN108145171B (en) 2020-11-27

Family

ID=62462951

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711429956.3A Active CN108145171B (en) 2017-12-26 2017-12-26 Bismuth-alkene nanosheet and preparation method thereof

Country Status (2)

Country Link
CN (1) CN108145171B (en)
WO (1) WO2019128245A1 (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019128245A1 (en) * 2017-12-26 2019-07-04 深圳大学 Bismuthene nanosheet and preparation method therefor
WO2019128244A1 (en) * 2017-12-26 2019-07-04 深圳大学 Method for preparing bismuth quantum dot and bismuth quantum dot
CN111653672A (en) * 2020-06-15 2020-09-11 安徽大学 Lattice-matched heterojunction composite film, preparation method and perovskite solar cell
CN111790904A (en) * 2020-05-25 2020-10-20 南京理工大学 Method for preparing bismuth-alkene nanosheets by liquid-phase laser irradiation method
CN112792350A (en) * 2019-10-25 2021-05-14 中国科学院福建物质结构研究所 Antimony and/or bismuth nanosheet, stibene and/or bislimonene and preparation method and application thereof
CN112846199A (en) * 2021-01-08 2021-05-28 新乡医学院 Method for preparing ultrathin bismuth-alkene nanosheets by heating, freezing, grinding and ultrasonic
CN113333736A (en) * 2021-05-10 2021-09-03 武汉理工大学 Microwave stripping-based stibene and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets
CN114990358A (en) * 2022-04-12 2022-09-02 中南大学 Arsenic-doped alkene nanosheet, and preparation method and application thereof
CN116984623A (en) * 2023-09-26 2023-11-03 之江实验室 Two-dimensional bismuth nanocrystal synthesis method based on sectional hydrothermal method

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110982900B (en) * 2019-12-13 2023-10-03 深圳瀚光科技有限公司 Biosensor based on bismuth alkene nanosheet fluorescence quenching, miRNA detection kit and application
CN114939406B (en) * 2022-03-24 2024-01-30 淮北师范大学 Bi2MoO6 photocatalyst and preparation method and application thereof
CN114672831B (en) * 2022-04-29 2023-05-09 华中科技大学 Atomic-level-thickness two-dimensional bismuth nanosheet material and preparation method and application thereof
CN116694089B (en) * 2022-09-19 2024-03-26 广州贝奥吉因生物科技股份有限公司 Hydrogel for inhibiting scar as well as preparation method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090129965A1 (en) * 2005-12-07 2009-05-21 Stegelmann Norman R Bi-material ultrasonic horn with integral isolation member
CN103692763A (en) * 2013-12-06 2014-04-02 深圳先进技术研究院 Peeling method of two-dimensional layered nano material
CN103771406A (en) * 2014-01-22 2014-05-07 中国工程物理研究院化工材料研究所 Graphene/manganese tetraoxide nanocomposite and preparation method thereof
CN104070178A (en) * 2014-07-01 2014-10-01 扬州大学 Preparation method for monodisperse bismuth nano-particles with controllable particle sizes
CN105600760A (en) * 2015-12-25 2016-05-25 中国科学院深圳先进技术研究院 Small-sized black phosphorus flakes and preparation method thereof
CN107234244A (en) * 2017-06-23 2017-10-10 南京理工大学 A kind of ultrasonic liquid-phase strip preparation method of big yield antimony alkene quantum dot
CN107275628A (en) * 2017-07-19 2017-10-20 华中科技大学 The preparation method and lithium ion battery of a kind of two-dimentional bismuth alkene

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108145171B (en) * 2017-12-26 2020-11-27 深圳大学 Bismuth-alkene nanosheet and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090129965A1 (en) * 2005-12-07 2009-05-21 Stegelmann Norman R Bi-material ultrasonic horn with integral isolation member
CN103692763A (en) * 2013-12-06 2014-04-02 深圳先进技术研究院 Peeling method of two-dimensional layered nano material
CN103771406A (en) * 2014-01-22 2014-05-07 中国工程物理研究院化工材料研究所 Graphene/manganese tetraoxide nanocomposite and preparation method thereof
CN104070178A (en) * 2014-07-01 2014-10-01 扬州大学 Preparation method for monodisperse bismuth nano-particles with controllable particle sizes
CN105600760A (en) * 2015-12-25 2016-05-25 中国科学院深圳先进技术研究院 Small-sized black phosphorus flakes and preparation method thereof
CN107234244A (en) * 2017-06-23 2017-10-10 南京理工大学 A kind of ultrasonic liquid-phase strip preparation method of big yield antimony alkene quantum dot
CN107275628A (en) * 2017-07-19 2017-10-20 华中科技大学 The preparation method and lithium ion battery of a kind of two-dimentional bismuth alkene

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
唐春娟等: "铋纳米线和纳米片的制备", 《材料研究学报》 *

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019128244A1 (en) * 2017-12-26 2019-07-04 深圳大学 Method for preparing bismuth quantum dot and bismuth quantum dot
WO2019128245A1 (en) * 2017-12-26 2019-07-04 深圳大学 Bismuthene nanosheet and preparation method therefor
CN112792350B (en) * 2019-10-25 2022-04-19 中国科学院福建物质结构研究所 Antimony and/or bismuth nanosheet, stibene and/or bislimonene and preparation method and application thereof
CN112792350A (en) * 2019-10-25 2021-05-14 中国科学院福建物质结构研究所 Antimony and/or bismuth nanosheet, stibene and/or bislimonene and preparation method and application thereof
CN111790904A (en) * 2020-05-25 2020-10-20 南京理工大学 Method for preparing bismuth-alkene nanosheets by liquid-phase laser irradiation method
CN111653672B (en) * 2020-06-15 2022-07-01 安徽大学 Lattice-matched heterojunction composite film, preparation method and perovskite solar cell
CN111653672A (en) * 2020-06-15 2020-09-11 安徽大学 Lattice-matched heterojunction composite film, preparation method and perovskite solar cell
CN112846199A (en) * 2021-01-08 2021-05-28 新乡医学院 Method for preparing ultrathin bismuth-alkene nanosheets by heating, freezing, grinding and ultrasonic
CN113333736A (en) * 2021-05-10 2021-09-03 武汉理工大学 Microwave stripping-based stibene and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets
CN113817927B (en) * 2021-10-09 2022-09-02 中南大学 Method for efficiently preparing arsenic-alkene nanosheets
CN114990358A (en) * 2022-04-12 2022-09-02 中南大学 Arsenic-doped alkene nanosheet, and preparation method and application thereof
CN114990358B (en) * 2022-04-12 2023-02-03 中南大学 Arsenic-doped alkene nanosheet, and preparation method and application thereof
CN116984623A (en) * 2023-09-26 2023-11-03 之江实验室 Two-dimensional bismuth nanocrystal synthesis method based on sectional hydrothermal method
CN116984623B (en) * 2023-09-26 2024-02-09 之江实验室 Two-dimensional bismuth nanocrystal synthesis method based on sectional hydrothermal method

Also Published As

Publication number Publication date
WO2019128245A1 (en) 2019-07-04
CN108145171B (en) 2020-11-27

Similar Documents

Publication Publication Date Title
CN108145171A (en) A kind of bismuth alkene nanometer sheet and preparation method thereof
CN108284220A (en) A kind of bismuth alkene nanometer sheet and preparation method thereof
CN108247069A (en) A kind of bismuth quantum dot and preparation method thereof
US10304937B2 (en) Scalable process for producing exfoliated defect-free, non-oxidised 2-dimensional materials in large quantities
CN102086025A (en) Preparation method of one-dimensional (1D) flexible nano-material assembly body
TW200906718A (en) Method for dispersion, alignment and deposition of nanotubes
Perumal et al. Recent studies on dispersion of graphene–polymer composites
CN108473802A (en) Stratified material and its processing method
CN108580908A (en) A kind of bismuth quantum dot and preparation method thereof
Shen et al. Self-assembled three-dimensional structures of single-crystalline ZnS submicrotubes formed by coalescence of ZnS nanowires
CN105439133B (en) A kind of preparation method of elecrtonegativity single-layer graphene
Bilisik et al. Graphene nanocomposites: A review on processes, properties, and applications
CN103732538B (en) The thermodynamic solution of metal-oxide and metal chalcogenide and mixed-metal oxides and chalcogenide
CN103922323A (en) Method for preparing small-diameter graphene
WO2015176045A1 (en) Methods and systems for the synthesis of nanoparticles including strained nanoparticles
Chuah et al. Synthesis and characterization of reduced graphene oxide using the aqueous extract of Eclipta prostrata
JP2015003833A (en) Formation method of graphene layer
CN107083530B (en) A kind of method of graphene quantum dot chemical activity induced growth rubrene film
Nenashev et al. Composite films based on carbon quantum dots in a matrix of PEDOT: PSS conductive polymer
Saxena et al. Synthesis of Ge-based nanosheet bundles using calcium germanides as templates in IP6 aqueous solution
CN106145095A (en) A kind of method obtaining Graphene based on shearing force machine stripping graphite
Zhong et al. Research progress and applications of 2D antimonene
Phule et al. Negative optical absorption and up-energy conversion in dendrites of nanostructured silver grafted with α/β-poly (vinylidene fluoride) in small hierarchical structures
RU2478563C2 (en) Method of manufacturing polymer composite with aligned array of carbon nanotubes of controlled density
CN106006575B (en) A kind of one-dimensional inorganic macromolecule and its general preparative methods

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant