CN103979505A - Preparation method of few-layer bismuth selenide nanosheets - Google Patents

Preparation method of few-layer bismuth selenide nanosheets Download PDF

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CN103979505A
CN103979505A CN201410208150.1A CN201410208150A CN103979505A CN 103979505 A CN103979505 A CN 103979505A CN 201410208150 A CN201410208150 A CN 201410208150A CN 103979505 A CN103979505 A CN 103979505A
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nanometer sheet
preparation
bismuth selenide
minority layer
powder
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CN103979505B (en
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翁建
孙莉萍
林智钦
彭健
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Xiamen University
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Xiamen University
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Abstract

The invention discloses a preparation method of few-layer bismuth selenide nanosheets, which relates to a bismuth selenide material. The preparation method comprises the following steps: putting selenium powder, bismuth oxide, polyvinylpyrrolidone, ethylene glycol and ethylenediamine tetraacetic acid into a reaction kettle to carry out a hydrothermal synthesis reaction, centrifugalizing obtained mixed liquid, removing liquid supernatant, and washing the obtained product respectively by using ultrapure water and anhydrous ethanol, and drying to obtain Bi2Se3 powder; and adding the Bi2Se3 powder into a N-methyl pyrrolidinone solvent or an acetic acid solution in which chitosan is dissolved, carrying out ultrasonic processing to obtain dispersion liquid of few-layer bismuth selenide nanosheets, standing the dispersion liquid, taking upper two thirds of the dispersion liquid and putting the taken dispersion liquid into a centrifuge to carry out low-speed centrifugalizing, collecting supernatant liquor obtained by centrifugalizing, and putting the supernatant liquor into a centrifuge to carry out high-speed centrifugalizing, removing a supernatant liquor part, and re-dispersing the obtained lower substance by using NMP (N-methyl pyrrolidinone) or an acetic acid solution, so that the few-layer bismuth selenide nanosheets dispersed in the solution are obtained finally. The preparation method is simple and quick.

Description

A kind of preparation method of minority layer bismuth selenide nanometer sheet
Technical field
The present invention relates to bismuth selenide body material, especially relate to a kind of preparation method of minority layer bismuth selenide nanometer sheet.
Background technology
Topology isolator is a class body phase insulation, but surface shows a kind of novel quantum material of Special Metal state, and it is starting one research boom at Condensed Matter Physics, chemical field and Material Field.Its this character is mainly (Nature, 2010, the 464:194-198 causing due to the coupling of its spin and time reversal symmetry; Nature Chemistry, 2011,3:845-849).Wherein, bismuth selenide (Bi 2se 3) the topological isolator character that represents allows it become a kind of material (Nature, 2009,460:1101-1105) with applications well prospect.At present, preparation minority layer or individual layer Bi 2se 3nanometer sheet mainly relies on mode from bottom to top, synthesizes (Journal of the American Chemical Society, 2012,134:6132-6135 by chemical reaction from atom or molecular scale; Journal of the American Chemical Society, 2012,134:2872-2875).In top-down building-up process, from monocrystalline block sample, obtain individual layer or minority layer Bi by the method for mechanically peel or chemical stripping 2se 3nanometer sheet (ACS Nano, 2011,5:2657-2663; Journal of the American Chemical Society, 2012,134:20294-20297).Wherein, in synthetic technology from bottom to top, synthesize as molecular beam epitaxy need to utilize accurate plant and instrument, apparatus expensive, consumes greatly, is not suitable for carrying out large batch of production; The individual layer obtaining from bottom to top or minority layer Bi 2se 3in the mode of nanometer sheet, as the mode of utilizing lithium ion intercalation to peel off, relatively loaded down with trivial details, need to carry out polystep reaction, washing, removal of impurities etc.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of minority layer bismuth selenide nanometer sheet.
The present invention includes following steps:
1) selenium powder, bismuth oxide, polyvinylpyrrolidone, ethylene glycol and ethylenediamine tetraacetic acid (EDTA) are packed in reactor and carry out hydrothermal synthesis reaction, the mixed solution obtaining is centrifugal, removes supernatant liquor, then uses respectively ultrapure water and absolute ethanol washing, after being dried, obtains Bi 2se 3powder;
2) by step 1) Bi that obtains 2se 3powder joins N-Methyl pyrrolidone solvent (NMP) or is dissolved with in the acetum (CS-HAc) of chitosan, ultrasonic after, obtain minority layer Bi 2se 3the dispersion liquid of nanometer sheet, leave standstill again, the part of getting its upper strata 2/3rds is put into low-speed centrifugal in whizzer, collect the upper strata liquid of centrifugal gained, again the upper strata liquid of gained is put into whizzer high speed centrifugal, remove supernatant part, lower floor's material of gained is heavily disperseed with NMP or acetum, finally obtain being dispersed in the minority layer bismuth selenide nanometer sheet in solution.
In step 1) in, the proportioning of described selenium powder, bismuth oxide, polyvinylpyrrolidone, ethylene glycol and ethylenediamine tetraacetic acid (EDTA) can be 3mmol: 1mmol: 0.9g: 36mL: 4mmol; The temperature of described hydrothermal synthesis reaction can be 180～200 DEG C, and the time of hydrothermal synthesis reaction can be 20h; The number of times of described washing can be 2 times; Described dry condition can be 60 DEG C of dry 96h in vacuum drying oven.
In step 2) in, described Bi 2se 3the proportioning of powder and N-Methyl pyrrolidone solvent (NMP) can be 50～100mg: 50mL; Described Bi 2se 3powder can be 50～100mg with the proportioning of the acetum (CS-HAc) that is dissolved with chitosan: 50mL; Described ultrasonic power can be 250W, and the ultrasonic time can be 0.5～50h; The described standing time can be 2～240h; The speed of described low-speed centrifugal can be 400～2000r/min, and the time of low-speed centrifugal can be 30min; Described ultracentrifugal speed can be 5000～20000r/min, and the ultracentrifugal time can be 20min.
The present invention adopts simple, fast mode to prepare minority layer Bi 2se 3nanometer sheet, provides a kind of and has utilized the method that liquid phase is peeled off to prepare minority layer Bi 2se 3nanometer sheet.The method is utilized two kinds of different solution, under ultrasonic effect, by Bi 2se 3body material is peeled off, thereby obtains the minority layer Bi being dispersed in a large number in solution 2se 3nanometer sheet, can be by Bi 2se 3be used for this research field more widely.The prepared minority layer bismuth selenide nanometer sheet of the present invention all has good dispersiveness in N-Methyl pyrrolidone solvent and chitosan aqueous solution, and has specific absorbent properties in visible region.Material prepared by the method can carry out the application of wider scope, as biosensor, and laser apparatus manufacture etc.
Brief description of the drawings
Fig. 1 is the prepared Bi of the embodiment of the present invention 1 2se 3body material X-ray diffraction (XRD) spectrogram.
Fig. 2 is the embodiment of the present invention 1 prepared Bi in NMP 2se 3x-ray diffraction (XRD) spectrogram of nanometer sheet.
Fig. 3 is the embodiment of the present invention 1 prepared Bi in NMP 2se 3transmission electron microscope (TEM) figure of nanometer sheet.
Fig. 4 is the embodiment of the present invention 1 prepared Bi in NMP 2se 3atomic force microscope (AFM) figure of nanometer sheet.
Fig. 5 is the embodiment of the present invention 1 prepared Bi in NMP 2se 3the height map that nanometer sheet is corresponding with Fig. 4.
Fig. 6 is the embodiment of the present invention 1 prepared Bi in NMP 2se 3raman (Raman) figure of nanometer sheet.
Fig. 7 is that the embodiment of the present invention 1 is at the prepared Bi of NMP 2se 3nanometer sheet ultraviolet-visible light (UV-Vis) figure.
Fig. 8 is the embodiment of the present invention 2 prepared Bi in CS-HAc 2se 3x-ray diffraction (XRD) spectrogram of nanometer sheet.
Fig. 9 is the embodiment of the present invention 2 prepared Bi in CS-HAc 2se 3transmission electron microscope (TEM) figure of nanometer sheet.
Figure 10 is the embodiment of the present invention 2 prepared Bi in CS-HAc 2se 3atomic force microscope (AFM) figure of nanometer sheet.
Figure 11 is the embodiment of the present invention 2 prepared Bi in NMP 2se 3the height map that nanometer sheet is corresponding with Figure 10.
Figure 12 is the embodiment of the present invention 2 prepared Bi in CS-HAc 2se 3raman (Raman) figure of nanometer sheet.
Figure 13 is the embodiment of the present invention 2 prepared Bi in CS-HAc 2se 3nanometer sheet ultraviolet-visible light (UV-Vis) figure.
Embodiment
After now specific embodiments of the invention being discussed in.
Embodiment 1
Bi 2se 3the preparation of body material: take the dissolving of 0.9g polyvinylpyrrolidone with electronic balance and be to be equipped with in the beaker of 36mL ethylene glycol, get respectively in addition 1mmol bismuth oxide, 3mmol selenium powder and 4mmol ethylenediamine tetraacetic acid (EDTA) and join in above-mentioned solution, fully stirring and evenly mixing.Mixed solution is poured in autoclave and sealed, be then positioned over homogeneous reactor and be warmed up to 200 DEG C, and at 200 DEG C of reaction 20h, it is reacted completely.The mixed solution obtaining, by high speed centrifugation processing, is removed supernatant liquor, respectively washs 2 times respectively finally 60 DEG C of dry 96h in vacuum drying oven with ultrapure water and dehydrated alcohol.
Utilize NMP to prepare minority layer bismuth selenide nanometer sheet: to synthesize Bi 2se 3powder is raw material, by 50mg, grinds thin Bi 2se 3powder joins in 50mL NMP, ultrasonic 30h in the ultrasonic apparatus that is then 250W by this mixed system in electric power.Gained dispersion liquid is left standstill to 48h, obtain the part of upper strata dispersion liquid 2/3rds and by its low-speed centrifugal 30min in the whizzer of 1000 rpms, collect upper strata liquid after centrifugal and centrifugal 20min of whizzer high speed at 10000 rpms by it, remove supernatant liquor, obtain the centrifugal thing of lower floor, lower floor's material of gained is disperseed with NMP, finally obtain being dispersed in minority layer Bi in NMP 2se 3nanometer sheet.
Few layer Bi 2se 3the detection of nanometer sheet: to Bi 2se 3body material carries out XRD detection.To few layer of Bi 2se 3nanometer sheet is carried out XRD, TEM, AFM, Raman, the detections such as UV-Vis.
Fig. 1 is Bi synthetic in embodiment 1 2se 3body material carries out collection of illustrative plates that the detection of XRD obtains and the contrast of standard card, proves that synthetic powder is Bi 2se 3crystal.
Fig. 2 is prepared Bi in embodiment 1 2se 3the XRD spectra of the dried sample of nanometer sheet dispersion liquid and the contrast of standard spectrogram, found the peak of [006] of enhancing, and the disappearance at some peaks, proves to obtain the Bi of few layer 2se 3nanometer sheet.
Fig. 3 is minority layer Bi in embodiment 1 2se 3the TEM figure of nanometer sheet, minority layer Bi as we know from the figure 2se 3for two-dimensional sheet structure.
Fig. 4 is gained minority layer Bi in embodiment 1 2se 3nanometer sheet AFM figure.
Fig. 5 is gained minority layer Bi in embodiment 1 2se 3nanometer sheet AFM schemes corresponding height map, can know the Bi of preparation 2se 3nanometer sheet is only layer 2-3.
Fig. 6 is embodiment 1 minority layer Bi 2se 3nanometer sheet and Bi 2se 3the Raman comparison diagram of body material, minority layer Bi in figure 2se 3nanometer sheet having there is red shift in vibration modes contrast Bi2Se3 body material Raman spectrogram, further confirms the Bi of preparation 2se 3nanometer sheet is minority layer.
Fig. 7 is minority layer Bi in embodiment 1 2se 3nanometer sheet and Bi 2se 3the UV-Vis comparison diagram of body material.Wherein the absorption peak of minority layer bismuth selenide nanometer sheet/NMP is 574nm.
Embodiment 2
Bi 2se 3the preparation of body material: take the dissolving of 0.9g polyvinylpyrrolidone with electronic balance and be to be equipped with in the beaker of 36ml ethylene glycol, get respectively in addition 1mmol bismuth oxide, 3mmol selenium powder and 4mmol ethylenediamine tetraacetic acid (EDTA) and join in above-mentioned solution, fully stirring and evenly mixing.Mixed solution is poured in autoclave and sealed, be then positioned over homogeneous reactor and be warmed up to 200 DEG C, and at 200 DEG C of reaction 20h, it is reacted completely.The mixed solution obtaining, by high speed centrifugation processing, is removed supernatant liquor, respectively washs 2 times respectively finally 60 DEG C of dry 96h in vacuum drying oven with ultrapure water and dehydrated alcohol.
Utilize CS-HAc minority layer bismuth selenide nanometer sheet: to synthesize Bi 2se 3powder is raw material, by 50mg, grinds thin Bi 2se 3powder joins in the aqueous acetic acid that 50mL chitosan concentration is every milliliter of 0.2mg, ultrasonic 30h in the ultrasonic apparatus that is then 250W by this mixed system in electric power.Gained dispersion liquid is left standstill to 48h, obtain the part of upper strata dispersion liquid 2/3rds and by its low-speed centrifugal 30min in the whizzer of 1000 rpms, collect upper strata liquid after centrifugal and centrifugal 20min of whizzer high speed at 10000 rpms by it, remove supernatant liquor, obtain the centrifugal thing of lower floor, lower floor's material of gained is disperseed with acetum, finally obtain disperseing the minority layer Bi of acetum 2se 3nanometer sheet.
Few layer Bi 2se 3the detection of nanometer sheet: to Bi 2se 3body material carries out XRD detection.To few layer of Bi 2se 3nanometer sheet is carried out XRD, TEM, AFM, Raman, the detections such as UV-Vis.
Fig. 8 is prepared Bi in embodiment 2 2se 3the XRD spectra of the dried sample of nanometer sheet dispersion liquid and the contrast of standard spectrogram, found the peak of [006] of enhancing, and the disappearance at some peaks, proves to obtain the Bi of few layer 2se 3nanometer sheet.
Fig. 9 is minority layer Bi in embodiment 2 2se 3the TEM figure of nanometer sheet, minority layer Bi as we know from the figure 2se 3for two-dimensional sheet structure.
Figure 10 is gained minority layer Bi in embodiment 2 2se 3nanometer sheet AFM figure.
Figure 11 is gained minority layer Bi in embodiment 2 2se 3nanometer sheet AFM schemes corresponding height map, can know the Bi of preparation 2se 3nanometer sheet is only layer 2-3.
Figure 12 is minority layer Bi in embodiment 2 2se 3nanometer sheet and Bi 2se 3the Raman comparison diagram of body material, minority layer Bi in figure 2se 3nanometer sheet vibration modes contrast Bi 2se 3having there is red shift in body material Raman spectrogram, further confirms the Bi of preparation 2se 3nanometer sheet is minority layer.
Figure 13 is minority layer Bi in embodiment 2 2se 3nanometer sheet and Bi 2se 3the UV-Vis comparison diagram of body material.Wherein, the absorption peak of minority layer bismuth selenide nanometer sheet/CS-HAc is 552nm.

Claims (10)

1. a preparation method for minority layer bismuth selenide nanometer sheet, is characterized in that comprising the following steps:
1) selenium powder, bismuth oxide, polyvinylpyrrolidone, ethylene glycol and ethylenediamine tetraacetic acid (EDTA) are packed in reactor and carry out hydrothermal synthesis reaction, the mixed solution obtaining is centrifugal, removes supernatant liquor, then uses respectively ultrapure water and absolute ethanol washing, after being dried, obtains Bi 2se 3powder;
2) by step 1) Bi that obtains 2se 3powder joins N-Methyl pyrrolidone solvent or is dissolved with in the acetum of chitosan, ultrasonic after, obtain minority layer Bi 2se 3the dispersion liquid of nanometer sheet, leave standstill again, the part of getting its upper strata 2/3rds is put into low-speed centrifugal in whizzer, collect the upper strata liquid of centrifugal gained, again the upper strata liquid of gained is put into whizzer high speed centrifugal, remove supernatant part, lower floor's material of gained is heavily disperseed with NMP or acetum, finally obtain being dispersed in the minority layer bismuth selenide nanometer sheet in solution.
2. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, it is characterized in that in step 1) in, the proportioning of described selenium powder, bismuth oxide, polyvinylpyrrolidone, ethylene glycol and ethylenediamine tetraacetic acid (EDTA) is 3mmol: 1mmol: 0.9g: 36mL: 4mmol.
3. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 1) in, the temperature of described hydrothermal synthesis reaction is 180～200 DEG C, the time of hydrothermal synthesis reaction is 20h.
4. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 1) in, the number of times of described washing is 2 times.
5. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 1) in, described dry condition is 60 DEG C of dry 96h in vacuum drying oven.
6. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 2) in, described Bi 2se 3the proportioning of powder and N-Methyl pyrrolidone solvent is 50～100mg: 50mL; Described Bi 2se 3powder is 50～100mg: 50mL with the proportioning of the acetum that is dissolved with chitosan.
7. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 2) in, described ultrasonic power is 250W, the ultrasonic time is 0.5～50h.
8. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 2) in, the described standing time is 2～240h.
9. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 2) in, the speed of described low-speed centrifugal is 400～2000r/min, the time of low-speed centrifugal is 30min.
10. a kind of preparation method of minority layer bismuth selenide nanometer sheet as claimed in claim 1, is characterized in that in step 2) in, described ultracentrifugal speed is 5000～20000r/min, the ultracentrifugal time is 20min.
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Cited By (9)

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CN104528663A (en) * 2014-12-18 2015-04-22 长春理工大学 Method for preparing bismuth selenide micron-tablet
CN109081315A (en) * 2017-06-13 2018-12-25 天津大学 A kind of preparation method of two-dimensional material telluride germanium
CN109943338A (en) * 2019-03-18 2019-06-28 中国计量大学 A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method
CN110586930A (en) * 2019-10-22 2019-12-20 广东银纳科技有限公司 Preparation method of nano titanium material for corrosion prevention
CN110745790A (en) * 2019-11-25 2020-02-04 东北大学 Hydrothermal preparation method of bismuth selenide nano powder
CN111229199A (en) * 2019-10-09 2020-06-05 武汉纺织大学 Method for preparing two-dimensional bismuth-based oxygen group compound nanosheet by liquid phase stripping method and application
CN111261737A (en) * 2020-01-21 2020-06-09 广东工业大学 SnSe/Bi2Se3Nanosheet heterojunction and preparation method thereof
CN113257933A (en) * 2021-05-26 2021-08-13 哈尔滨工业大学 Bismuth selenide/gallium nitride ultraviolet-infrared broadband detector and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets

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CN103046110A (en) * 2011-10-13 2013-04-17 国家纳米科学中心 Method for preparing monocrystal Bi2Se3 nano structure
CN103288061A (en) * 2013-06-24 2013-09-11 福州大学 Bismuth selenide nanometer material, preparation method and applications thereof
CN103641079A (en) * 2013-10-21 2014-03-19 东南大学 Preparation method for large-size ultrathin bismuth selenide nanosheet

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CN101746738A (en) * 2009-09-29 2010-06-23 武汉理工大学 Preparing method of nano laminar thermoelectric Bi2Se3 compound
CN103046110A (en) * 2011-10-13 2013-04-17 国家纳米科学中心 Method for preparing monocrystal Bi2Se3 nano structure
CN103288061A (en) * 2013-06-24 2013-09-11 福州大学 Bismuth selenide nanometer material, preparation method and applications thereof
CN103641079A (en) * 2013-10-21 2014-03-19 东南大学 Preparation method for large-size ultrathin bismuth selenide nanosheet

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104528663A (en) * 2014-12-18 2015-04-22 长春理工大学 Method for preparing bismuth selenide micron-tablet
CN109081315A (en) * 2017-06-13 2018-12-25 天津大学 A kind of preparation method of two-dimensional material telluride germanium
CN109943338A (en) * 2019-03-18 2019-06-28 中国计量大学 A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method
CN109943338B (en) * 2019-03-18 2021-12-28 中国计量大学 Preparation method of near-infrared luminescent rare earth doped indium selenide nanosheet
CN111229199A (en) * 2019-10-09 2020-06-05 武汉纺织大学 Method for preparing two-dimensional bismuth-based oxygen group compound nanosheet by liquid phase stripping method and application
CN110586930A (en) * 2019-10-22 2019-12-20 广东银纳科技有限公司 Preparation method of nano titanium material for corrosion prevention
CN110586930B (en) * 2019-10-22 2022-01-14 广东银纳科技有限公司 Preparation method of nano titanium material for corrosion prevention
CN110745790A (en) * 2019-11-25 2020-02-04 东北大学 Hydrothermal preparation method of bismuth selenide nano powder
CN110745790B (en) * 2019-11-25 2022-09-20 东北大学 Hydrothermal preparation method of bismuth selenide nano powder
CN111261737A (en) * 2020-01-21 2020-06-09 广东工业大学 SnSe/Bi2Se3Nanosheet heterojunction and preparation method thereof
CN111261737B (en) * 2020-01-21 2022-08-12 广东工业大学 SnSe/Bi 2 Se 3 Nanosheet heterojunction and preparation method thereof
CN113257933A (en) * 2021-05-26 2021-08-13 哈尔滨工业大学 Bismuth selenide/gallium nitride ultraviolet-infrared broadband detector and preparation method thereof
CN113257933B (en) * 2021-05-26 2023-08-29 哈尔滨工业大学 Bismuth selenide/gallium nitride ultraviolet-infrared broadband detector and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets

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