CN109765235A - A kind of anisotropic rapid detection method of two-dimension nano materials - Google Patents
A kind of anisotropic rapid detection method of two-dimension nano materials Download PDFInfo
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- CN109765235A CN109765235A CN201910177288.2A CN201910177288A CN109765235A CN 109765235 A CN109765235 A CN 109765235A CN 201910177288 A CN201910177288 A CN 201910177288A CN 109765235 A CN109765235 A CN 109765235A
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Abstract
The present invention provides a kind of anisotropic rapid detection method of two-dimension nano materials comprising following steps: prepares two-dimension nano materials sample；The two-dimension nano materials sample prepared is fixed on the objective table of optical microscopy；The two-dimension nano materials sample surfaces are humidified；Image Acquisition is carried out to the two-dimension nano materials sample surfaces using optical microscopy, obtains drop in the distribution situation of the two-dimension nano materials sample surfaces；According to drop in the distribution situation of the two-dimension nano materials sample surfaces, the anisotropy of the two-dimension nano materials sample is determined.Experimental facilities needed for the present invention is simple and easy to operate, quick, the short zigzag direction and armchair direction that can be detected out two-dimensional nano piece for tens seconds is only needed, in addition, the detection method accuracy rate is high, and it has broad application prospects to two-dimensional nano piece sample without any damage.
Description
Technical field
The present invention relates to test chemical technical fields, and in particular to a kind of anisotropic quick inspection of two-dimension nano materials
Survey method.
Background technique
Two-dimentional black phosphorus has attracted the extensive concern of researcher as a kind of novel two-dimensional semiconductor material.Particularly,
It is compared with other materials with high symmetry, black phosphorus has unique intra-face anisotropy, not from its crystal structure
Symmetry, i.e., along two mutually perpendicular directions in black phosphorus face: armchair direction and Z-shaped direction, crystal structure difference
It shows and folds shape and mentioned ridge-shaped, lead to the difference of the bond distance of covalent bond and bond angle between the atom in the two directions, so that black
Significant difference is presented along different crystallographic directions in the properties such as physics, chemistry, mechanics and the calorifics of phosphorus.
It is existing mainly to pass through it in optics, electronics, calorifics, mechanics for the two-dimentional anisotropic detection method of black phosphorus
The characterization of aspect carrys out indirect analysis, and such as in optics aspect, the anisotropy of black phosphorus is embodied in the distinguishable light absorption of degree of polarization
The many aspects such as spectrum, extinction spectra, transmitted spectrum, reflectance spectrum, photoluminescence spectrum and optogalvanic spectra；It is black in terms of electronics
The effective mass of the electrons and holes of phosphorus shows apparent anisotropy, is macroscopically being presented as the load along different crystal orientations
Flow the difference of transport factor and conductivity；In terms of calorifics, the anisotropic thermal conductivity of black phosphorus is mainly derived from anisotropy
Phonon distribution, can be composed by raman microspectroscopy and time domain heat reflection spectrum measure；In terms of mechanics, the anisotropy master of black phosphorus
Its Young's modulus and resonance frequency are embodied in along the difference of different directions, atomic force microscope and mechanical test etc. can be passed through
Means are analyzed；And more intuitively detection method is that Raman spectrum detects, the characteristic peaks that Raman vibrates have certain each
Anisotropy, B in face2gAnd Ag 2(zigzag) direction zigzag there is bigger peak value, and Ag 1Peak intensity armchair (handrail
Chair) direction is bigger, but needs sufficiently complex data processing and analytic process, and can cause to damage to two-dimentional black phosphorus nanometer sheet
It is bad.
To sum up, existing to be directed to the anisotropic detection method of two-dimension nano materials, not only need very accurate valuable detection
Test equipment, and complicated data processing and analysis, but also exist and a degree of damage is caused to two-dimensional nano piece.
Summary of the invention
The technical problem to be solved by the embodiment of the invention is that overcoming the deficiencies of existing technologies, a kind of two wieners are provided
The rapid detection method of rice material anisotropy.
The embodiment of the present invention provides a kind of anisotropic rapid detection method of two-dimension nano materials comprising following step
It is rapid:
Prepare two-dimension nano materials sample；
The two-dimension nano materials sample prepared is fixed on the objective table of optical microscopy；
The two-dimension nano materials sample surfaces are humidified；
Image Acquisition is carried out to the two-dimension nano materials sample surfaces using optical microscopy, obtains drop described
The distribution situation of two-dimension nano materials sample surfaces；
According to drop in the distribution situation of the two-dimension nano materials sample surfaces, the two-dimension nano materials sample is determined
The anisotropy of product.
The anisotropic rapid detection method of two-dimension nano materials provided in an embodiment of the present invention, makes two-dimensional nano first
Piece adsorption drop carries out Image Acquisition to its surface using optical microscopy, and according to drop on two-dimensional nano piece surface
Distribution situation, determine the anisotropy of the two-dimensional nano piece sample；Required experimental facilities is simple and easy to operate, quick,
The short zigzag direction and armchair direction that can be detected out two-dimensional nano piece for tens seconds is only needed, in addition, the detection method is quasi-
True rate is high, and has broad application prospects to two-dimensional nano piece sample without any damage.
Detailed description of the invention
Fig. 1 is the optical microscope image of two-dimentional black phosphorus nanometer sheet sample surfaces: before a, c humidification；B, after d humidification；
Fig. 2 is the optical microscope image of two-dimensional graphene nanometer sheet sample surfaces: before a, c. humidification；B, after d. humidification；
Fig. 3 is the optical microscope image of two-dimentional molybdenum sulfide nanometer sheet sample surfaces: before a, c. humidification；B, after d. humidification；
Fig. 4 is the polarization Raman spectrum test result of the black squama nanometer sheet sample of two dimension: a. Raman map；B. Raman peaks Ag 1
The image of intensity and incident angle；C. the optical microscope image after two-dimentional black squama nanometer sheet sample humidification；
Fig. 5 is the in-situ Raman spectrum in-situ test result of the two-dimentional black phosphorus nanometer sheet sample under different wetting number；
Fig. 6 is the schematic diagram that drop is distributed in two-dimentional black phosphorus nanometer sheet sample surfaces: a. side view；B. top view.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments,
The present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain this hair
It is bright, it is not intended to limit the present invention.
The embodiment of the present invention provides a kind of anisotropic rapid detection method of two-dimension nano materials comprising following step
It is rapid:
S01: two-dimension nano materials sample is prepared；
S02: the two-dimension nano materials sample prepared is fixed on the objective table of optical microscopy；
S03: the two-dimension nano materials sample surfaces are humidified；
S04: Image Acquisition is carried out to the two-dimension nano materials sample surfaces using optical microscopy, drop is obtained and exists
The distribution situation of the two-dimension nano materials sample surfaces；
S05: according to drop in the distribution situation of the two-dimension nano materials sample surfaces, the two-dimensional nano material is determined
Expect the anisotropy of sample.
Step S01 is specifically included: two-dimension nano materials being placed on adhesive tape, is bonded, is obtained repeatedly using the viscosity of adhesive tape
Two-dimensional material nanometer sheet；It is transferred to using two-dimensional material nanometer sheet dimethyl silicone polymer (PDMS) film as medium
On slide surface after cleaning up；Wherein, the micro slide can be the plate of any surfacing, such as SiO2/ Si is brilliant
Piece, coverslip etc.；The two-dimension nano materials are with anisotropic material, including two-dimentional black phosphorus, alloy, distortion 1T phase
The transition metal chalcogenide (1T '-TMDs) of structure, the IV race metal chalcogenide (GIVMCs) of orthorhombic phase and some
IV-V race semiconductor (such as Ge2As、Ge2S, GeS, GeSe, SnS, SnSe) etc..
Step S03 is specifically included: gradually being humidified using humidifier to the two-dimension nano materials sample surfaces, i.e.,
It is constantly generated by humidifier by spraying, by spraying comprising millions of very small drops, these droplets are easy by nanometer sheet institute
Absorption；Wherein, the humidifier internal solution is water or organic solvent.
Step S04 is specifically included: the mistake humidified by optical microscopy to the two-dimension nano materials sample surfaces
Cheng Jinhang video recording；Or by optical microphotograph sem observation drop the two-dimension nano materials sample surfaces distribution situation；When
When observing that elliptical bead occur in two-dimension nano materials sample surfaces, the two-dimension nano materials sample surfaces are clapped
It takes the photograph, shooting includes video recording and takes pictures.
Step S05 is specifically included: will be distributed over the long axis of the elliptical bead on the two-dimension nano materials sample surfaces
Direction is determined as zigzag (zigzag) direction of the two-dimension nano materials sample；By the short axle side of the elliptical bead
To armchair (armchair) direction for being determined as the two-dimension nano materials sample.
Specific implementation of the invention is described in detail (by taking two-dimentional black phosphorus as an example) combined with specific embodiments below,
The test process and principle of his two-dimensional material are similar, in addition do not repeat herein.
Embodiment 1
Firstly, the method using mechanical stripping carries out sample preparation to two-dimentional black phosphorus bulk crystals, that is, take a certain amount of black
Phosphorus bulk crystals are put on adhesive tape, are bonded repeatedly using the viscosity of adhesive tape, two-dimentional black phosphorus nanometer sheet are obtained, by obtained two dimension
Black phosphorus nanometer sheet uses PDMS film to be transferred to SiO as medium2The surface of/Si chip, wherein SiO2Thickness be about 300nm；So
The two-dimentional black phosphorus nanometer sheet sample prepared is fixed to immediately on the objective table of optical microscopy and is observed afterwards, using adding
Wet device gradually humidifies two-dimentional black phosphorus nanometer sheet sample surfaces, and by optical microscopy to two-dimentional black phosphorus nanometer sheet sample
The process that product surface is humidified is recorded a video；Finally, according to water droplet two-dimentional black phosphorus nanometer sheet sample surfaces distribution feelings
Condition determines the anisotropy of the two dimension black phosphorus nanometer sheet sample, that is, will be distributed on the two dimension black phosphorus nanometer sheet sample surfaces
The long axis direction of oval water droplet is determined as its direction zigzag；The short-axis direction of oval water droplet is determined as it
The direction armchair.
Comparative example 1
Firstly, the method using mechanical stripping carries out sample preparation to two-dimensional graphene bulk crystals, that is, take a certain amount of
Graphene bulk crystals are put on adhesive tape, are bonded repeatedly using the viscosity of adhesive tape, are obtained two-dimensional graphene nanometer sheet, will be made
Obtaining two-dimensional graphene nanometer sheet uses PDMS film to be transferred to SiO as medium2The surface of/Si chip, wherein SiO2Thickness about
For 300nm；The two-dimensional graphene nanometer sheet sample prepared is fixed to immediately after on the objective table of optical microscopy and is carried out
Observation, gradually humidifies two-dimensional graphene nanometer sheet sample surfaces using humidifier, and by optical microscopy to two
The process that dimension graphene nanometer sheet sample surfaces are humidified is recorded a video；And two-dimensional graphene nanometer sheet sample surfaces are added
The image of wet front and back is intercepted.
Comparative example 2
Firstly, the method using mechanical stripping carries out sample preparation to two-dimentional molybdenum sulfide bulk crystals, that is, take a certain amount of
Molybdenum sulfide bulk crystals are put on adhesive tape, are bonded repeatedly using the viscosity of adhesive tape, are obtained two-dimentional molybdenum sulfide nanometer sheet, will be made
Obtaining two-dimentional molybdenum sulfide nanometer sheet uses PDMS film to be transferred to SiO as medium2The surface of/Si chip, wherein SiO2Thickness about
For 300nm；The two-dimentional molybdenum sulfide nanometer sheet sample prepared is fixed to immediately after on the objective table of optical microscopy and is carried out
Observation, gradually humidifies two-dimentional molybdenum sulfide nanometer sheet sample surfaces using humidifier, and by optical microscopy to two
The process that dimension molybdenum sulfide nanometer sheet sample surfaces are humidified is recorded a video, and two-dimentional molybdenum sulfide nanometer sheet sample surfaces are added
The image of wet front and back is intercepted.
By Fig. 1-3, the two-dimensional graphene nanometer sheet sample of the two-dimentional black phosphorus nanometer sheet of the embodiment of the present invention 1, comparative example 1
And the two-dimentional molybdenum sulfide nanometer sheet sample surfaces of comparative example 2 optical microscope image it is found that water droplet in two-dimentional black phosphorus nanometer sheet
Ellipse is presented in sample surfaces, and water droplet is not having anisotropic two-dimensional graphene nanometer sheet sample and two-dimentional molybdenum sulfide
Nanometer sheet sample surfaces are rendered as circle, exactly embody the anisotropy of two-dimentional black phosphorus, meanwhile, by the length of oval water droplet
Axis direction is determined as its direction zigzag；The short-axis direction of oval water droplet is determined as its direction armchair.
In order to further confirm that the direction zigzag and the direction armchair of two-dimentional black phosphorus nanometer sheet, the embodiment of the present invention 1
The test of polarization Raman is carried out to the two-dimentional black phosphorus nanometer sheet (Fig. 4 c) in Fig. 1, every test is primary to rotate 30 ° of incident light angle,
Then two-dimentional black phosphorus nanometer sheet is tested in the Raman map of the light of incidence angles degree, as shown in fig. 4 a with Raman spectrum；Into one
Step, according to Raman peaks A each in Fig. 4 ag 1、B2g、Ag 2Intensity, incident angle and Raman peak intensity are drawn in polar coordinates
Image, with Ag 1For, as shown in Figure 4 b；It is tested it can be seen from Fig. 4 b by the anisotropic distribution situation of small water droplet
The anisotropic result of black phosphorus nanometer sheet and the test result of polarization Raman are identical, and illustrate two dimension provided by the present invention
The anisotropic rapid detection method of nano material, required experimental facilities is simple and easy to operate, quick, only needs short by tens
Second can be detected out the direction zigzag and the direction armchair of two-dimensional nano piece, and accuracy rate of testing result is high, very may be used
It leans on.
In order to prove that water spray will not damage two-dimentional black phosphorus nanometer sheet sample, the present invention continues will be in embodiment 1
Two-dimentional black phosphorus nanometer sheet sample carry out in-situ Raman spectrum in-situ test (Fig. 5), by two-dimentional black phosphorus nanometer sheet sample respectively into
Water wetting of row, Ji Shici water wetting, the results showed that same test point Ag 1、B2g、Ag 2Raman peak position and peak intensity not
It changes, it is sufficient to confirm that the embodiment of the present invention 1 is soaked with water droplet anisotropy to identify two-dimentional black phosphorus nanometer sheet respectively to different
The method of property is completely lossless to sample itself.
The anisotropic rapid detection method of two-dimension nano materials provided in an embodiment of the present invention, makes two-dimensional nano first
Piece adsorption drop carries out Image Acquisition to its surface using optical microscopy, and according to drop on two-dimensional nano piece surface
Distribution situation, determine the anisotropy of the two-dimensional nano piece sample；Required experimental facilities is simple and easy to operate, quick,
The short direction zigzag and the direction armchair that can be detected out two-dimensional nano piece for tens seconds is only needed, in addition, the detection method
Accuracy rate is high, and has broad application prospects to two-dimensional nano piece sample without any damage.
It is worth noting that, anisotropy wetting also involves wetability of the water droplet on two-dimentional black phosphorus nanometer sheet surface
And non-uniform Distribution, i.e. in terms of the physical factor of anisotropy wetting mainly has a following two, 1) liquid shows not in solid
Continuously distributed (precipitous solid rim)；2) chemistry is heterogeneous.Test philosophy of the invention is to be dependent on nanoscale and micron order
Surface texture (groove, parallel columns, wrinkle) can lead to the visible change of droplets wet phenomenon, specifically, significant having
In the two-dimentional black phosphorus nanometer sheet of groove structure, the anisotropy wetting of drop only relies upon the wetability of two-dimentional black phosphorus itself
Matter, water drop suspension are not directly contacted with the phosphorus atoms of bottom on the groove structure of protrusion；The groove structure of protrusion is enough
It is deep, and be rectangle (as shown in Figure 6), rather than triangle or sinusoidal profile, drop and groove structure are easily lead in this way
Centre forms air layer, that is, the groove structure protruded is the main reason for generating so big drop anisotropic elastic solid.
The above is merely preferred embodiments of the present invention, be not intended to restrict the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (8)
1. a kind of anisotropic rapid detection method of two-dimension nano materials characterized by comprising
Prepare two-dimension nano materials sample；
The two-dimension nano materials sample prepared is fixed on the objective table of optical microscopy；
The two-dimension nano materials sample surfaces are humidified；
Image Acquisition is carried out to the two-dimension nano materials sample surfaces using optical microscopy, obtains drop in two wiener
The distribution situation on rice material sample surface；
According to drop in the distribution situation of the two-dimension nano materials sample surfaces, each of the two-dimension nano materials sample is determined
Anisotropy.
2. detection method according to claim 1, it is characterised in that: the two-dimension nano materials are with anisotropic
Material.
3. detection method according to claim 1, it is characterised in that: it is described to prepare two-dimension nano materials sample, it is specific to wrap
It includes:
Two-dimension nano materials are placed on adhesive tape, is bonded repeatedly using the viscosity of adhesive tape, obtains two-dimensional material nanometer sheet；
Polydimethylsiloxanefilm film is used to be transferred on slide surface as medium the two-dimensional material nanometer sheet.
4. detection method according to claim 1, it is characterised in that: it is described to the two-dimension nano materials sample surfaces into
Row humidification, specifically includes:
The two-dimension nano materials sample surfaces are gradually humidified using humidifier.
5. detection method according to claim 4, it is characterised in that: solution used in the humidification is water or organic solvent.
6. detection method according to claim 1, it is characterised in that: described to utilize optical microscopy to the two-dimensional nano
Material sample surface carries out Image Acquisition, obtains drop in the distribution situation of the two-dimension nano materials sample surfaces, specific packet
It includes:
It is recorded a video by the process that optical microscopy humidifies the two-dimension nano materials sample surfaces.
7. detection method according to claim 1, it is characterised in that: described to utilize optical microscopy to the two-dimensional nano
Material sample surface carries out Image Acquisition, obtains drop in the distribution situation of the two-dimension nano materials sample surfaces, specific packet
It includes:
By optical microphotograph sem observation drop the two-dimension nano materials sample surfaces distribution situation；
When observing that elliptical bead occur in two-dimension nano materials sample surfaces, to the two-dimension nano materials sample surfaces into
Row shooting.
8. detection method according to claim 1, which is characterized in that it is described according to drop sample surfaces distribution feelings
Condition determines the anisotropy of the two-dimension nano materials sample, specifically includes:
The long axis direction that will be distributed over the elliptical bead on the two-dimension nano materials sample surfaces is determined as two wiener
The zigzag direction of rice material sample；The short-axis direction of the elliptical bead is determined as the two-dimension nano materials sample
Armchair direction.
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