CN104984813B - It is a kind of using adjusting the method that pH value carries out nano bismuth telluride grading - Google Patents
It is a kind of using adjusting the method that pH value carries out nano bismuth telluride grading Download PDFInfo
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Abstract
It is a kind of using the method that pH value carries out nano bismuth telluride grading is adjusted, the present invention relates to the method for nano bismuth telluride grading.It is to solve the Bi that the preparation method of existing bismuth telluride nanometer sheet is obtained2Te3The big technical problem of nanometer chip size heterogeneity, yardstick dispersiveness.This method：First, in nitrogen atmosphere, bismuth telluride powder is added in the hexane solution of n-BuLi and is soaked, then remove liquid, bismuth telluride is stood in glove box；2nd, to water is added in bismuth telluride, stirring or ultrasonically treated obtains Bi2Te3Suspension；3rd, by Bi2Te3Suspension adjusts pH value to 7, centrifugation, then gradually reduces pH value, then separates, and obtains varigrained Bi2Te3Nanometer sheet, completes nano bismuth telluride grading.This method is convenient, environmentally friendly, isolate various sizes of two-dimentional Bi cheaply2Te3, and epigranular, can be used in electronics device.
Description
Technical field
The present invention relates to the method for nano bismuth telluride grading.
Background technology
The current surface metal state of topological insulator and the property of built-in electrical insulation state have caused greatly concern, because
For their this thundering physical properties make it have in the field such as low-loss spintronics devices and quantum computer
The prospect of being widely applied.Bismuth telluride (Bi2Te3) it is one of topological insulator, it is the insulation state that there is energy gap, surface inside it
It is the metallic state without energy gap, spin polarization and linear dispersion relation.Bi2Te3Crystal belongs to hexaplanar, and space group is D5 3d
(R3M), every layer is formed by five atom covalence links.Layered arrangement along c-axis is as follows:---Te—Bi—Te—Bi—
Te---Te—Bi—Te—Bi—Te---.Act on forming crystal structure with van der Waals between layers.Dimension is to determine
Determine one of important parameter of material property, the topological insulator Bi of two-dimensional nano2Te3Crystal defect can be reduced, is reduced remaining
Body conductance, improves skin effect, and pyroelectric effect is improved by suppressing thermal conductivity.For a good thermoelectric material, very
High zt is essential, and the research of nanosizing makes Bi2Te3ZT be worth to very big raising.So nanosizing
Bi2Te3Bigger application prospect is had in thermo-electric device field.Two dimension Bi is prepared at present2Te3Method have molecular beam epitaxy, machine
Tool is peeled off and chemical solution synthesis etc., these preparation methods not only apparatus expensive, and resulting two-dimensional topology insulator chi
Very little heterogeneity, surface topography is difficult to control, and low yield makes it be limited in application aspect.Application No.
The Chinese patent of 201410080171.X discloses a kind of method for preparing bismuth telluride nanometer sheet, and the method is by bismuth telluride and carbonic acid
After lithium is stirred vigorously in phenmethylol, hydro-thermal process is then centrifuged for separating, and obtains bismuth telluride nanometer sheet, but still exist and receive
Rice chip size heterogeneity, the big problem of yardstick dispersiveness.
The content of the invention
The present invention is to solve the Bi of existing preparation2Te3The big technology of nanometer chip size heterogeneity, yardstick dispersiveness is asked
Topic, and a kind of method that nano bismuth telluride grading is carried out using pH value is provided.
A kind of method that nano bismuth telluride grading is carried out using pH value of the invention, is carried out according to the following steps：
First, in the glove box of nitrogen atmosphere, bismuth telluride powder is added to the hexane solution equipped with n-BuLi
In container, bismuth telluride powder is dipped into liquid, after sealing is placed 36~72 hours, liquid is removed, solid is stayed in spacious
In mouth container, continue to place 24~48h in glove box；
2nd, the container that will be equipped with bismuth telluride takes out from glove box, adds water, and stirring or ultrasonically treated obtains Bi2Te3It is outstanding
Supernatant liquid；
3rd, in Bi2Te3It is 7 that hydrochloric acid solution regulation pH value is added in suspension, is then centrifuged for isolated solid formation I and liquid
Phase thing I, solid formation I is dried, and obtains one-level Bi2Te3Nanometer sheet；Hydrochloric acid (HCl) solution regulation pH is continuously added in liquid phase thing I
Value is then centrifuged for isolated solid formation II and liquid phase thing II to 6, and solid formation II is dried, and obtains two grades of Bi2Te3Nanometer sheet；
Add hydrochloric acid (HCl) solution to adjust pH value to 5 in liquid phase thing II again, be then centrifuged for isolated solid formation III and liquid phase thing
III, solid formation III is dried, obtain three-level Bi2Te3Nanometer sheet；Hydrochloric acid solution is added to adjust pH value to 4 in liquid phase thing III, so
After be centrifugally separating to obtain solid formation IV and liquid phase thing IV, solid formation IV is dried, obtain level Four Bi2Te3Nanometer sheet, completes nanometer
Bismuth telluride grading.
Continuation hydrochloric acid reduces liquid phase thing pH value step by step, can separate and obtain smaller Bi2Te3Nanometer sheet.Step 3
In add hydrochloric acid solution to adjust pH value to 3 in liquid phase thing IV, be then centrifuged for isolated solid formation V and liquid phase thing V, will be solid
Phase thing V is dried, and obtains Pyatyi Bi2Te3Nanometer sheet.Hydrochloric acid solution is added to adjust pH value to 2 in liquid phase thing V in step 3, so
After be centrifugally separating to obtain solid formation VI and liquid phase thing VI, solid formation VI is dried, obtain six grades of Bi2Te3Nanometer sheet.In step 3
Add hydrochloric acid solution to adjust pH value to 1 in liquid phase thing VI, isolated solid formation VII and liquid phase thing VII are then centrifuged for, by solid phase
Thing VII is dried, and obtains seven grades of Bi2Te3Nanometer sheet.
The present invention is by Bi2Te3In the hexane solution of powder immersion n-BuLi, lithium ion is in Bi2Te3Middle intercalation, works as lithium
The Bi of ion insertion2Te3When powder is immersed in distilled water, Bi2Te3The gas effusion that lithium ion in layer is produced after being contacted with water,
Form individual layer Bi2Te3, highly opaque suspension is formed in water.Regulation suspension is separated into difference to different pH value
The individual layer Bi of size2Te3Piece, Bi2Te3Chip size is uniform.Using the method for the present invention can conveniently, environmental protection, isolate cheaply
Various sizes of two-dimentional Bi2Te3.This even-grained two-dimentional Bi2Te3Can be used for electronics device, in thermo-electric device.
Brief description of the drawings
Fig. 1 is the one-level individual layer Bi isolated in embodiment 12Te3；
Fig. 2 is the two grades of individual layer Bi isolated in embodiment 12Te3；
Fig. 3 is the three-level individual layer Bi isolated in embodiment 12Te3；
Fig. 4 is the level Four individual layer Bi isolated in embodiment 12Te3；
Fig. 5 is the individual layer Bi isolated in embodiment 12Te3The relation curve that changes with pH value of particle diameter.
Specific embodiment
Specific embodiment one：A kind of method that nano bismuth telluride grading is carried out using pH value of present embodiment,
Carry out according to the following steps：
First, in the glove box of nitrogen atmosphere, bismuth telluride powder is added to the hexane solution equipped with n-BuLi
In container, bismuth telluride powder is dipped into liquid, after sealing is placed 36~72 hours, liquid is removed, solid is stayed in spacious
In mouth container, continue to place 24~48h in glove box；
2nd, the container that will be equipped with bismuth telluride takes out from glove box, adds water, and stirring or ultrasonically treated obtains Bi2Te3It is outstanding
Supernatant liquid；
3rd, in Bi2Te3The HCl solution regulation pH value that 1M is added in suspension is 7, is then centrifuged for isolated solid formation I
With liquid phase thing I, solid formation I is dried, obtain one-level Bi2Te3Nanometer sheet；Hydrochloric acid solution regulation pH value is continuously added in liquid phase thing I
To 6, isolated solid formation II and liquid phase thing II are then centrifuged for, solid formation II is dried, obtain two grades of Bi2Te3Nanometer sheet；Again
Add hydrochloric acid solution to adjust pH value to 5 in liquid phase thing II, isolated solid formation III and liquid phase thing III are then centrifuged for, by solid phase
Thing III is dried, and obtains three-level Bi2Te3Nanometer sheet；Add hydrochloric acid solution to adjust pH value to 4 in liquid phase thing III, be then centrifuged for separating
Solid formation IV and liquid phase thing IV are obtained, solid formation IV is dried, obtain level Four Bi2Te3Nanometer sheet, completes nano bismuth telluride granularity
Classification.
Specific embodiment two：Present embodiment and the bismuth telluride powder in step one unlike specific embodiment one
It is dipped into liquid, sealing standing time is 60 hours.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from step one unlike specific embodiment one or two, by liquid
Solid is stayed in open-top receptacle after removal, continues to place 36h in glove box.Other and specific embodiment one or two-phase
Together.
Specific embodiment four：Stirred in step 2 unlike one of present embodiment and specific embodiment one to three
Speed be 100~1000 revs/min, mixing time be 0.1~6h.Other are identical with one of specific embodiment one to three.
Specific embodiment five：Ultrasound in step 2 unlike one of present embodiment and specific embodiment one to four
The frequency for the treatment of is 25~50kHz, and sonication treatment time is 5~30min.Other phases one of with specific embodiment one to four
Together.
Specific embodiment six：Hydrochloric acid in step 3 unlike one of present embodiment and specific embodiment one to five
Concentration be 1~1.5mol/L.Other are identical with one of specific embodiment one to five.
Beneficial effects of the present invention are verified with following embodiment
Embodiment 1：A kind of method that nano bismuth telluride grading is carried out using pH value of the present embodiment, according to the following steps
Carry out：
First, in the glove box of nitrogen atmosphere, bismuth telluride powder is added to the hexane solution equipped with n-BuLi
In container, bismuth telluride powder is dipped into liquid, after sealing is placed 72 hours, liquid is removed, solid is stayed in into open appearance
In device, continue to place 24h in glove box；
2nd, the container that will be equipped with bismuth telluride takes out from glove box, adds water, stirs 30min, obtains Bi2Te3Suspension；
3rd, in Bi2Te3The HCl solution regulation pH value that 1M is added in suspension is 7, is then centrifuged for isolated solid formation I
With liquid phase thing I, solid formation I is dried, obtain one-level Bi2Te3Nanometer sheet；The HCl solution regulation of 1M is continuously added in liquid phase thing I
PH value is then centrifuged for isolated solid formation II and liquid phase thing II to 6, and solid formation II is dried, and obtains two grades of Bi2Te3Nanometer
Piece；Add hydrochloric acid (HCl) solution of 1M to adjust pH value to 5 in liquid phase thing II again, be then centrifuged for the He of isolated solid formation III
Liquid phase thing III, solid formation III is dried, and obtains three-level Bi2Te3Nanometer sheet；The HCl solution regulation of 1M is continuously added in liquid phase thing III
PH value is then centrifuged for isolated solid formation IV and liquid phase thing IV to 4, and solid formation IV is dried, and obtains level Four Bi2Te3Nanometer
Piece, completes nano bismuth telluride grading.
In the present embodiment 1, one-level Bi2Te3The atomic force microscopy of nanometer sheet is as shown in Figure 1；Two grades of Bi2Te3Nanometer
The atomic force microscopy of piece is as shown in Fig. 2 three-level Bi2Te3The atomic force microscopy of nanometer sheet is as shown in figure 3, level Four
Bi2Te3The atomic force microscopy of nanometer sheet is as shown in Figure 4.Contrast from Fig. 1~4 it is recognised that with the reduction of pH value,
The Bi for isolating2Te3The size of nanometer sheet is less and less.
Fig. 5 is the individual layer Bi isolated in embodiment 12Te3The relation curve that changes with pH value of particle diameter, can also from Fig. 5
Find out with the reduction of pH value, the Bi for isolating2Te3The size of nanometer sheet is less and less.
The method of the present embodiment, simply, efficiently, low cost has obtained various sizes of individual layer Bi2Te3Nanometer sheet.
Claims (9)
1. it is a kind of using adjusting the method that pH value carries out nano bismuth telluride grading, it is characterised in that the method is according to the following steps
Carry out：
First, in the glove box of nitrogen atmosphere, bismuth telluride powder is added to the container of the hexane solution equipped with n-BuLi
In, bismuth telluride powder is dipped into liquid, after sealing is placed 36~72 hours, liquid is removed, solid is stayed in into open appearance
In device, continue to place 24~48h in glove box；
2nd, the container that will be equipped with bismuth telluride takes out from glove box, adds water, and stirring or ultrasonically treated obtains Bi2Te3Suspend
Liquid；
3rd, in Bi2Te3It is 7 that hydrochloric acid solution regulation pH value is added in suspension, is then centrifuged for isolated solid formation I and liquid phase thing
I, solid formation I is dried, obtain one-level Bi2Te3Nanometer sheet；Hydrochloric acid solution is continuously added in liquid phase thing I and adjust pH value to 6, then
Solid formation II and liquid phase thing II are centrifugally separating to obtain, solid formation II is dried, obtain two grades of Bi2Te3Nanometer sheet；Again in liquid phase thing
Add hydrochloric acid solution to adjust pH value to 5 in II, be then centrifuged for isolated solid formation III and liquid phase thing III, solid formation III is dry
It is dry, obtain three-level Bi2Te3Nanometer sheet；Add hydrochloric acid solution to adjust pH value to 4 in liquid phase thing III, be then centrifuged for isolated solid
Phase thing IV and liquid phase thing IV, solid formation IV is dried, and obtains level Four Bi2Te3Nanometer sheet, completes nano bismuth telluride grading.
2. according to claim 1 a kind of using adjusting the method that pH value carries out nano bismuth telluride grading, its feature
It is that bismuth telluride powder in step one is dipped into liquid, sealing standing time is 60 hours.
3. according to claim 1 and 2 a kind of using the method that pH value carries out nano bismuth telluride grading is adjusted, it is special
Levy in being step one, stay in open-top receptacle solid after liquid is removed, continue to place 36h in glove box.
4. according to claim 1 and 2 a kind of using the method that pH value carries out nano bismuth telluride grading is adjusted, it is special
It is 100~1000 revs/min to levy the speed for being to stir in step 2, and mixing time is 1~6h.
5. according to claim 1 and 2 a kind of using the method that pH value carries out nano bismuth telluride grading is adjusted, it is special
It is that ultrasonically treated frequency in step 2 is 25~50kHz to levy, and sonication treatment time is 5~30min.
6. according to claim 1 and 2 a kind of using the method that pH value carries out nano bismuth telluride grading is adjusted, it is special
Levy be hydrochloric acid in step 3 concentration be 1~1.5mol/L.
7. according to claim 1 a kind of using adjusting the method that pH value carries out nano bismuth telluride grading, its feature
It is to add hydrochloric acid solution to adjust pH value to 3 in liquid phase thing IV in step 3, is then centrifuged for isolated solid formation V and liquid
Phase thing V, solid formation V is dried, and obtains Pyatyi Bi2Te3Nanometer sheet.
8. according to claim 7 a kind of using adjusting the method that pH value carries out nano bismuth telluride grading, its feature
It is to add hydrochloric acid solution to adjust pH value to 2 in liquid phase thing V in step 3, is then centrifuged for isolated solid formation VI and liquid
Phase thing VI, solid formation VI is dried, and obtains six grades of Bi2Te3Nanometer sheet.
9. according to claim 8 a kind of using adjusting the method that pH value carries out nano bismuth telluride grading, its feature
It is to add hydrochloric acid solution to adjust pH value to 1 in liquid phase thing VI in step 3, is then centrifuged for isolated solid formation VII and liquid
Phase thing VII, solid formation VII is dried, and obtains seven grades of Bi2Te3Nanometer sheet.
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