CN109269429A - Two-dimensional material is averaged piece diameter detection method, device and quantity acquisition methods, device - Google Patents
Two-dimensional material is averaged piece diameter detection method, device and quantity acquisition methods, device Download PDFInfo
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- CN109269429A CN109269429A CN201810620225.5A CN201810620225A CN109269429A CN 109269429 A CN109269429 A CN 109269429A CN 201810620225 A CN201810620225 A CN 201810620225A CN 109269429 A CN109269429 A CN 109269429A
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- G—PHYSICS
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/08—Measuring arrangements characterised by the use of optical techniques for measuring diameters
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Abstract
It is averaged piece diameter detection method, device and quantity acquisition methods, device the invention discloses a kind of two-dimensional material.The quantity that the present invention passes through two-dimensional material in unit volume in acquisition two-dimensional material dispersion liquid, the average quality of each two-dimensional material can be obtained in conjunction with the quality of two-dimensional material in unit volume in two-dimensional material dispersion liquid, the molal weight independently having further according to two-dimensional material minimum constitutional repeating unit is it can be concluded that constitute the quantity of the minimum constitutional repeating unit of each two-dimensional material, the average area of two-dimensional material finally can be obtained according to the average number of plies of the area of each minimum constitutional repeating unit and two-dimensional material, and then calculate the average piece diameter of two-dimensional material.This method only needs to measure the quantity of two-dimensional material in unit volume in two-dimensional material dispersion liquid, and other parameters are known or can measure and obtain by the simple prior art, therefore the two-dimensional material of the invention piece diameter detection method that be averaged is simply accurate, at low cost.
Description
Technical field
It is averaged the detection side of piece diameter the present invention relates to the technical field of two-dimensional material detection more particularly to a kind of two-dimensional material
Method and detection device, and to implement the method and used acquisition that obtain two-dimensional material quantity used by the detection method
Device.
Background technique
Since graphene in 2004 is found, this material being made of monolayer carbon atom two-dimensional tiles causes people
Extensive concern, pushed the development of two-dimensional material research and development, application.The two-dimensional materials such as graphene are that a kind of atom level is thick and very
The two-dimensional material of soft (radius-thickness ratio is much larger than 1000).In the two-dimensional size for determining the two-dimensional materials such as graphene, often
By AFM(Atomic Force Microscope, atomic force microscope), SEM(Scanning Electron
Microscope, scanning electron microscope), TEM (Transmission Electron Microscope, transmission electron microscopy
Mirror), STM(Scanning Tunneling Microscope, scanning tunneling microscope) etc. microscopic sdIBM-2+2q.p.approach method carry out
Small-scale observation determines the two-dimensional size of the two-dimensional materials such as graphene.However this method statistic effect is extremely limited,
It is difficult to reflect the true piece diameter size of a large amount of two-dimensional material powders or slurry, while needs many and diverse sample preparation during characterizing
Journey, randomness is big, and test value is expensive.Due to effective, rapid two-dimensional material size detecting method missing, greatly limit
The commercial applications paces of two-dimensional material.
At present by carrying out the laser particle analyzer of particle size detection based on static light scattering method in detection nanometer and micron
All there is preferable accuracy and reproducibility, but measured matter form need to be spherical close to three-dimensional when particle, and for two-dimentional material
Material is then difficult to be adapted to the method to be detected.Optical detection apparatus based on dynamic light scattering method, can be with real-time tracing liquid
Substance in body, while the concentration of substance in unit volume can also be extrapolated, it is one that detection does not change because of measured matter
Kind can be utilized the potential method for detecting two-dimensional material.But due to two-dimensional material in dispersion liquid random motion it is uncertain
Property, making it, there are larger problems in terms of two-dimensional material tracks accuracy.
The Chinese invention patent application of the number of being disclosed as CN104101612A discloses a kind of planar materials surface defects detection
Device, including main body frame, the linear light sorurce being mounted on main body frame and at least one detection being mounted on main body frame
Module；Main body frame includes the two root posts and the crossbeam being fixedly mounted in two root posts positioned at two sides, and crossbeam, which is equipped with, to be slided
Dynamic guide rod；Detection module includes the mounting base being slidably installed on sliding guide, is equipped in mounting base and is located at cross
The ccd image sensor and dot matrix type laser of beam two sides；Linear light sorurce mounting base, linear light sorurce are respectively equipped in two root posts
Both ends be separately mounted in two linear light sorurce mounting bases, and between linear light sorurce mounting base and linear light sorurce be equipped with for adjusting
Save the regulating mechanism of position of the linear light sorurce on the direction perpendicular to crossbeam.
Above-mentioned technical proposal is to detect to planar materials surface defect, uses static light source and mobile collection equipment
Data acquisition and data processing, one side are carried out to planar materials, do not can solve in the prior art based on static light scattering
Method can only to detected close to three-dimensional ball shape and the technical issues of cannot be detected to two-dimensional material；On the other hand, cannot
Based on dynamic light scattering method, to two-dimensional material, the uncertainty of random motion, the technology for being difficult to track in dispersion liquid are asked for solution
Topic.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of be averaged piece diameter detection method, device and quantity of two-dimensional material to obtain
Method, apparatus is taken, may be implemented to detect the average piece diameter of two-dimensional material, and is random in dispersion liquid not by two-dimensional material
Uncertainty of movement etc. influences.
It is averaged the detection method of piece diameter in order to solve the above-mentioned technical problems, the present invention provides a kind of two-dimensional material, comprising:
Two-dimensional material is added in solution and is uniformly mixed and forms two-dimensional material dispersion liquid；
Obtain the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume；
Obtain two-dimensional material quality, the averagely number of plies and the two-dimensional material in the two-dimensional material dispersion liquid unit volume
The physical parameter of minimum constitutional repeating unit；
According to the minimum repetitive structure of two-dimensional material quantity, quality, the average number of plies and two-dimensional material in the unit volume
The physical parameter of unit calculates the average piece diameter of two-dimensional material；
Wherein, the physical parameter of the minimum constitutional repeating unit of the two-dimensional material includes the minimum repetitive structure list of two-dimensional material
The area of the minimum constitutional repeating unit of molal weight, two-dimensional material that member independently has.
Further, the two-dimensional material quality in the two-dimensional material dispersion liquid unit volume is according to two be added in solution
The volume of dimension quality of materials and the two-dimensional material dispersion liquid of acquisition is calculated.
Further, the average piece diameter D of two-dimensional material is calculated according to the following formula:
(1)
Wherein, m is the quality of two-dimensional material in unit volume, NAFor Avogadro constant number, S is that two-dimensional material minimum repeats to tie
The area of structure unit, N are the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume, and M is two-dimensional material minimum weight
The molal weight that complex structure unit independently has, L are the average number of plies of two-dimensional material, and π is pi.
Further, after the average piece diameter D that two-dimensional material is calculated according to formula (1), also by by calculated two dimension
The average piece diameter D of material is modified the average piece diameter D of the calculated two-dimensional material multiplied by an adjusted coefficient K.
Further, the method for the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume is obtained are as follows:
Image is shot to dispersion liquid from least two angles using optical imaging apparatus；
Two-dimensional material is identified from the image of shooting respectively, and calculates two-dimensional material quantity contained in every image；
The quantity of the two-dimensional material contained in each image is added, and duplicate removal, meter are carried out to the two-dimensional material contained in each image
Calculate the two-dimensional material quantity obtained in unit volume.
Further, when shooting image to dispersion liquid using optical imaging apparatus, connect the dispersion liquid with flow regime
Continue through the region that is taken, the optical imaging apparatus is continuously shot acquisition video image.
Further, the solution is one of water, alcohols, ketone, aldehydes, lipid, surfactant or any group
It closes.
The present invention also provides a kind of methods for obtaining two-dimensional material quantity, comprising:
Image is shot to dispersion liquid from least two angles using optical imaging apparatus；
Two-dimensional material is identified from the image of shooting respectively, and calculates two-dimensional material quantity contained in every image；
The quantity of the two-dimensional material contained in each image is added, and duplicate removal, meter are carried out to the two-dimensional material contained in each image
Calculate the two-dimensional material quantity obtained in unit volume.
Further, when shooting image to dispersion liquid from least two angles using optical imaging apparatus, make the dispersion
Liquid continues through the region that is taken with flow regime, and the optical imaging apparatus is continuously shot acquisition dynamic image, according to continuous
The dynamic image data obtained is shot, list is calculated in the two-dimensional material number occurred in the shooting visual field in record unit time
Contained two-dimensional material number in the volume of position.
It is averaged the two-dimensional material quantity acquisition device of piece diameter the present invention also provides a kind of for detecting two-dimensional material, comprising:
Light source；
Sample memory, the side by close to sources are provided with light source channel, and sample memory at least part is by light transmission material
Material is made, for accommodating the dispersion liquid containing two-dimensional material in the sample memory；
Optical imaging apparatus, for shooting image to the dispersion liquid in the sample memory from least two angles.
Further, the optical imaging apparatus has at least two, is arranged in the angle that 0 is less than 180 degree is greater than described
Sample memory periphery.
Further, the optical imaging apparatus has one, for after being shot from an angle to dispersion liquid pre-
If being moved to another angle in the time to shoot dispersion liquid.
Further, the light source channel is in slit-shaped.
Further, the optical imaging apparatus includes optical observation unit and signal acquisition unit, the optical observation
Unit is used to receive the scattering light of two-dimensional material, and is imaged in signal acquisition unit, and the signal acquisition unit is used for light
It studies as being converted into electric signal and exporting.
Further, the optical observation unit includes the optical microscopy passed through for the scattering light of the two-dimensional material
Head.
Further, the light source is the fixed light source of wavelength, alternatively, being one section of preset wavelength and continuously adjustable light
Source.
Further, it is provided with inlet and liquid outlet on the sample memory, dispersion is connected on the inlet
Liquid propulsion device.
The present invention also provides a kind of the be averaged detection devices of piece diameter of two-dimensional material to further include including above-mentioned acquisition device
The control analytical equipment being connected with the acquisition device, the figure that the control analytical equipment is used to be exported according to the acquisition device
As data identify two-dimensional material, and calculate two-dimensional material quantity contained in every image；Being also used to will be in each image
The quantity of the two-dimensional material contained is added, and carries out duplicate removal to the two-dimensional material contained in each image, is calculated and is obtained unit volume
Interior two-dimensional material quantity.
Further, it is described control analytical equipment be also used to according in the unit volume two-dimensional material quantity, quality,
The physical parameter of the minimum constitutional repeating unit of the average number of plies and two-dimensional material calculates the average piece diameter of two-dimensional material,
In, the physical parameter of the minimum constitutional repeating unit of the two-dimensional material includes that the minimum constitutional repeating unit institute of two-dimensional material is only
The area of the minimum constitutional repeating unit of the vertical molal weight having, two-dimensional material.
Compared with prior art, the beneficial effects of the present invention are the present invention is single in two-dimensional material dispersion liquid by obtaining
The quantity of two-dimensional material in the volume of position can obtain each two in conjunction with the quality of two-dimensional material in unit volume in two-dimensional material dispersion liquid
The average quality for tieing up material, the molal weight independently having further according to two-dimensional material minimum constitutional repeating unit is it can be concluded that structure
At the quantity of the minimum constitutional repeating unit of each two-dimensional material, finally according to the area of each minimum constitutional repeating unit and
The average area of two-dimensional material can be obtained in the average number of plies of two-dimensional material, and then calculates the average piece diameter of two-dimensional material.It should
Method only needs to measure the quantity of two-dimensional material in unit volume in two-dimensional material dispersion liquid, and other parameters are known or logical
It crosses the simple prior art and can measure and obtain, therefore two-dimensional material of the invention be averaged that piece diameter detection method is simple accurately, cost
It is low, and not by two-dimensional material, the uncertainty etc. of random motion influences in dispersion liquid.
Detailed description of the invention
Fig. 1 be two-dimensional material of the invention be averaged piece diameter detection method schematic diagram；
Fig. 2 is the structural schematic diagram of the acquisition device embodiment one of two-dimensional material quantity in the present invention；
Fig. 3 is the structural schematic diagram of the acquisition device embodiment two of two-dimensional material quantity in the present invention；
Fig. 4 be two-dimensional material of the invention be averaged piece diameter detection device embodiment structural schematic diagram；
Fig. 5 is the functional block diagram of the control analytical equipment of the embodiment of the present invention；
Fig. 6 is two-dimensional material of the embodiment of the present invention under various concentration, and measurement obtains the linear relationship chart of two-dimensional material quantity.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
It should be noted that in the description of the present invention, the instruction such as term " on ", "lower", "left", "right", "inner", "outside"
Direction or the term of positional relationship be direction based on the figure or positional relationship, this is intended merely to facilitate description, and
It is not that indication or suggestion described device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore not
It can be interpreted as limitation of the present invention.
In addition it is also necessary to explanation, in the description of the present invention unless specifically defined or limited otherwise, term " peace
Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally
Connection；It can be mechanical connection, be also possible to be electrically connected；Can be directly connected, can also indirectly connected through an intermediary,
It can be the connection inside two elements.To those skilled in the art, it can understand that above-mentioned term exists as the case may be
Concrete meaning in the present invention.
The detection method of piece diameter as shown in Figure 1, two-dimensional material of the invention is averaged, comprising:
Step 1, two-dimensional material is added in solution and is uniformly mixed and form two-dimensional material dispersion liquid；
Step 2, the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume is obtained；
Step 3, two-dimensional material quality, the average number of plies and the two dimension in the two-dimensional material dispersion liquid unit volume are obtained
The physical parameter of the minimum constitutional repeating unit of material；
Step 4, according to the minimum weight of two-dimensional material quantity, quality, the average number of plies and two-dimensional material in the unit volume
The physical parameter of complex structure unit calculates the average piece diameter of two-dimensional material.
Wherein, the physical parameter of the minimum constitutional repeating unit of the two-dimensional material includes that the minimum of two-dimensional material repeats to tie
The area of the minimum constitutional repeating unit of molal weight, two-dimensional material that structure unit independently has.When preparing dispersion liquid, institute
The solution used is one of water, alcohols, ketone, aldehydes, lipid, surfactant or any combination.
In step 3, the two-dimensional material quality in the two-dimensional material dispersion liquid unit volume is according in addition solution
Two-dimensional material quality and the volume of the two-dimensional material dispersion liquid of acquisition are calculated.That is, with the two-dimensional material for preparing dispersion liquid
Quality divided by the volume of finally obtained dispersion liquid, be the two-dimensional material quality in unit volume two-dimensional material dispersion liquid,
Its numerical value is generally 1 × 10-2×10-5Between g/ml.Mole matter that the minimum constitutional repeating unit of two-dimensional material independently has
Amount and area can be obtained according to specific two-dimensional material structural formula, or detect or calculate to obtain by the prior art；And structure
It can also detect to obtain by prior art means at the average number of plies of the minimum constitutional repeating unit of two-dimensional material.Such as two dimension
The number of plies of material is distributed or the ratio of averagely element such as C, O, H, P, S contained by number of plies situation and two-dimensional material itself etc..
Specifically, according in two-dimensional material dispersion liquid in unit volume two-dimensional material quantity, in conjunction with two-dimensional material disperse
The quality of two-dimensional material can obtain the average quality of each two-dimensional material in unit volume in liquid, repeat further according to two-dimensional material minimum
The molal weight that structural unit independently has is it can be concluded that constitute the quantity of the minimum constitutional repeating unit of each two-dimensional material
N:
(11)
Wherein m is the mass value of two-dimensional material in unit volume；N is to measure contained two-dimensional material number value in unit volume；M is
The molal weight that minimum constitutional repeating unit independently has；NAFor Avogadro constant number.The present embodiment is used when calculating
Molal weight combination Avogadro constant number that minimum constitutional repeating unit independently has replaces two-dimensional material minimum weight
The molal weight that complex structure unit independently has is more convenient to calculate.Those skilled in the art with minimum it is recognised that repeated
The quality that structural unit independently has also can be implemented as the physical parameter of characterization two-dimensional material minimum constitutional repeating unit
The present invention, the molal weight M that minimum constitutional repeating unit is independently had remove as Avogadro constant number NAIt is as minimum
The mass M that constitutional repeating unit independently has '.The Mass Calculation two-dimensional material independently having with minimum constitutional repeating unit
Average piece diameter equally within protection scope of the present invention.
Then according to the quantity n for the minimum constitutional repeating unit for constituting each two-dimensional material, in conjunction with each minimum repetition
The area of structural unit and the average number of plies of two-dimensional material calculate the average piece diameter D that two-dimensional material can be obtained:
(12)
Wherein, S is the area of two-dimensional material minimum constitutional repeating unit, and L is the average number of plies of two-dimensional material, and π is pi.
In conjunction with above-mentioned formula (11) and formula (12), the final calculation formula of the average piece diameter of available two-dimensional material:
(1).
" the average piece diameter of two-dimensional material " of the present invention refers to two-dimensional material lateral dimension equivalent diameter.Described
" molal weight that minimum constitutional repeating unit independently has " refers to mole matter that minimum constitutional repeating unit can independently possess
Amount.It, should such as regular hexagon, that is, hexatomic ring that the minimum constitutional repeating unit of graphene is the side length about 0.142nm that carbon atom is constituted
The molal weight that hexatomic ring independently possesses is 24 grams/mol (i.e. 1/3 × 6 × 12 grams/mol), and area is about 0.052nm2；
Molybdenum disulfide minimum constitutional repeating unit is the equilateral triangle that sulphur and molybdenum are constituted, mole matter which independently possesses
Amount is 160.08 grams/mol.
In addition, same atom may be simultaneously adjacent minimum repetitive structure list due to this body structure of two-dimensional material
The constitution element of member will affect the molal weight that minimum constitutional repeating unit independently has, and then influence final calculating knot
Fruit；In addition, due to by the way of optical identification, being limited to the resolution ratio of optical identification when detecting two-dimensional material quantity,
The two-dimensional material that might have less than the optical identification limit exists, and is averaged piece diameter D ' to obtain more accurate two-dimensional material,
The above-mentioned two-dimensional material the being calculated piece diameter D that is averaged can be modified by adjusted coefficient K when needing:
D '=KD, i.e.,
Adjusted coefficient K can be calculated according to the molecular structure of two-dimensional material, can also be calculated with sampling statistics.
Preferably, in order to obtain the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume, used one
Kind embodiment method are as follows:
Image is shot to dispersion liquid from least two angles using optical imaging apparatus；
Two-dimensional material is identified from the image of shooting respectively, and calculates two-dimensional material quantity contained in every image；
The quantity of the two-dimensional material contained in each image is added, and duplicate removal is carried out to the two-dimensional material contained in each image,
Exactly the number of iterations for appearing in two-dimensional material in different images simultaneously is removed, to obtain the two-dimensional material in unit volume
Quantity.Such as 1000 two-dimensional materials are had identified in the image of first optical imaging apparatus shooting, and in second light
It learns in the image of imaging device shooting and has identified 1100 two-dimensional materials, the two-dimensional material wherein computed repeatedly by analysis has
900, and the total quantity of two-dimensional material is 1200 (1000+1100-900), then as single divided by the dispersion liquid volume of detection
The quantity of two-dimensional material in the volume of position.
It in the method, can be by the way that two or more optical imaging apparatus be arranged simultaneously from different perspectives to dispersion liquid
It is shot, only first dispersion liquid can also be shot from an angle with an optical imaging apparatus, then when default
In be moved to another angle dispersion liquid shot, shooting interval requires short enough twice, to avoid two-dimensional material
Brownian movement testing result is impacted.
It is further preferred that making the dispersion liquid to flow shape when shooting image to dispersion liquid using optical imaging apparatus
State continues through the region that is taken, and the optical imaging apparatus is continuously shot acquisition video image.Due to using dynamic detection,
It so that the dispersion liquid volume that optical imaging apparatus can detecte greatly increases, and then can reduce error, improve detection accuracy.Together
When, due to using dynamic detection, the motion profile of each two-dimensional material can be identified, convenient for analyzing different optical imageries
Which two-dimensional material is identical in image captured by equipment.
The present invention is from the purpose of the images of multiple angle shot dispersion liquids, first is that caused by eliminating and mutually blocking because of two-dimensional material
Error；Second is that general optical imaging apparatus can not identify the object of the size because of two-dimensional material with a thickness of atomic level
Body, therefore when the extending direction face optical imaging apparatus of two-dimensional material, it can not be imaged in optical imaging apparatus, will cause something lost
Leakage.When shooting dispersion liquid simultaneously from two angles, then the case where can omitting, greatly reduce, and from three or more angles
When spending while shooting dispersion liquid, then two-dimensional material can be taken by always having an optical imaging apparatus, will not be omitted
Situation.
And when shooting if the dispersion liquid is made to continue through the region that is taken with flow regime, it can increase in addition to above-mentioned
Add detection volume and improve outside precision, the effect that can also be flowed by dispersion liquid, promotes two-dimensional material to change posture, to keep away
Exempt to be leaked bat.That is, even if some two-dimensional material at a time the lucky face optical imaging apparatus of its extending direction (or
Person is directed at two optical imaging apparatus simultaneously), but since mobilization changes the posture moment of two-dimensional material, at other moment
Optical imaging apparatus can take the two-dimensional material, to further increase detection accuracy.
As shown in Fig. 2, it is of the invention for detect two-dimensional material be averaged piece diameter two-dimensional material quantity acquisition device one
Embodiment characterized by comprising
Light source 1；
Sample memory 2, the side by close to sources are provided with light source channel 22, and 2 at least part of sample memory is by saturating
Luminescent material is made, for accommodating the dispersion liquid containing two-dimensional material in the sample memory；
Optical imaging apparatus, for shooting image to the dispersion liquid in the sample memory from least two angles.
The light that light source issues enters sample memory 2 by light source channel 22, and light is scattered in dispersion liquid by two-dimensional material,
The light transmission part on sample memory is scattered light through, is received by optical imaging apparatus.Optical imaging apparatus has at least two, if
It sets in the sample memory periphery, for shooting the image of dispersion liquid from different angles.In general, two optical imageries
Angle between equipment is greater than 0 and is less than 180 degree.But in order to preferably reduce error, between two optical imaging apparatus
The straight angle is preferred close to 90 degree, such as 70-110 degree.
The light transmission part of sample memory 2 is made of the high molecular material of acid and alkali-resistance, quartz, glass etc..Sample memory 2
Generally regular structure, such as cube structure, the inside dimension that dispersion liquid flows through sample memory 2 are rules and fix vertical
Cube, the size section of length are respectively 1000-100 μm, 500-50 μm, 2-20 μm.Dispersion liquid and two-dimensional material stream
When through sample memory, when light source is radiated at rough or curvature biggish two-dimensional material surface, light beam, which generates to scatter, simultaneously to be led to
It crosses the optical observation unit 3 that 2 outside of sample memory is set and signal acquisition unit 4 acquires information.Before detection, need to point
Dispersion liquid carries out blank detection according to detecting step, and impurity particle number should be less than 1 × 10 in General Decentralized liquid7A/ml, to avoid
Excessive impurity particle impacts scatter incident light.It certainly, can also in the enough situations of optical imaging apparatus resolution ratio
To relax the requirement to impurity particle number.
Light source channel on sample memory 2 is in slit by light transmission or partial light permeability, the high molecular material of acid and alkali-resistance, stone
English, glass etc. constitute shape can be by being arranged in at least two of 2 side of sample memory easy-disassembling-assembling opaque sheet metals 21
It constitutes, forms light source channel 22 between two neighboring sheet metal 21.When two sheet metals are arranged, a light source channel is formed,
Light source, which enters after sample memory 2, acquires information by corresponding optical imaging apparatus；When at least three sheet metals is arranged, shape
Enter sample memory 2 at least two light source channels 22, light source, light can be made more uniform.Those skilled in the art can be with
Understand, compared to the mode for being easy to dismount setting sheet metal, also the one side of sample sample memory 2 can be set as opening up
There are light source channel 22 and integrally formed structure, is such as set as opening the panel of narrow slit in centre, defect is that can not adjust light
The width and height of source channels, can only the sample memory 2 of every kind of model corresponding light source channel 22 is set, but it is still able to achieve
The present invention passes through for light source to generate the function of scattering light and be observed.Slit spacing is fixed between adjacent metal piece 21, such as
Between 5-500 μm.
In the present embodiment, the optical imaging apparatus includes optical observation unit 3 and signal acquisition unit 4, the light
The scattering light that observation unit 4 is used to receive two-dimensional material is learned, and is imaged in signal acquisition unit 4, the signal acquisition unit 4
For optical imagery to be converted into electric signal and is exported.The optical observation unit includes supplying the scattering light of the two-dimensional material logical
The optical microphotograph camera lens crossed.The amplification factor of optical microphotograph camera lens is any one of 4 times, 10 times, 20 times, 40 times etc., is passed through
Adjust its adjustable focal length of optical microscopy.It will be appreciated by persons skilled in the art that optical observation unit 3 can also be energy
The other structures that enough there is enlarging function and light beam is allowed to pass through.Signal acquisition unit 4 includes CCD camera or cmos camera
And corresponding supporting mechanism, record are preferably greater than 60 frames/second picture, are believed by the image that style of shooting obtains two-dimensional material
Breath.
Preferably, the light source is the fixed light source of wavelength, e.g. laser light source, and the optical wavelength generated is in 193nm-
Within the scope of 1064nm.Or light source may be one section of preset wavelength and continuously adjustable light source, the wavelength generated be
Within the scope of 193nm-1064nm.It will be appreciated by persons skilled in the art that according to different dispersion liquid and unlike material, property
The light source of appropriate wavelength, selection fixation or adjustable light source may be selected in the two-dimentional material of energy.
As shown in figure 3, for another embodiment of the acquisition device of two-dimensional material quantity in the present invention, in the present embodiment,
Optical observation unit 3 and signal acquisition unit 4 are arranged on two adjacent sides of sample memory 2, and the light with incident light
The perpendicular side of beam.Since two-dimensional material generates scattering light, the beam range after scattering is wider, in order to improve the essence of test
Degree, if several optical observation units 3, the setting of signal acquisition unit 4 is arranged in same side or is arranged at least two sides
Dry optical observation unit 3, signal acquisition unit 4.
The detection device of piece diameter as shown in figure 4, two-dimensional material of the invention is averaged, on the basis of above-mentioned acquisition device,
Increase the control analytical equipment 6 being connected with the acquisition device.Acquisition device periphery is equipped with closed frame 7, and frame 7 will enter
It penetrates grow up to be a useful person 1, sample memory 2, optical observation unit 3 and signal acquisition unit 4 of photoproduction to be located in it, and supports above-mentioned each knot
Structure.Frame 7 can be the hardened structure of box-type, realize shading and support function by dismounting mode, can also be curtain structure, pass through
Function and support function are blocked in cord realization.
Control analytical equipment 6 is mainly connect with optical imaging apparatus, the figure for being exported according to the optical imaging apparatus
As data identify two-dimensional material, and calculate two-dimensional material quantity contained in every image；Being also used to will be in each image
The quantity of the two-dimensional material contained is added, and carries out duplicate removal to the two-dimensional material contained in each image, is calculated and is obtained unit volume
Interior two-dimensional material quantity.Can also be by the parameters such as the electronics filter of picture signal, contrast on control analytical equipment 6, it will
Image Adjusting is most weak to influencing each other between the most clear, scatter spot, obtains stray light effects information at this time.
As shown in Figure 4, it is preferable that inlet and liquid outlet (not shown), institute are provided on the sample memory 2
It states and is connected with dispersion liquid propulsion device 5 on inlet.Dispersion liquid can be pushed to continue through sample by dispersion liquid propulsion device 5
Memory 2, so that dynamic detection is realized, to improve detection accuracy.Dispersion liquid propulsion device 5 is that sample memory 2 is provided such as 10-
The flow velocity of 1000ul/min, flow rate accuracy are can be controlled in as in ± 1ul/min.Dispersion liquid propulsion device 5 may include storage tank,
It connect the pump that inside storage or outside is set with storage tank, and conveys the pipe of dispersion liquid to sample memory with pump connection
Road, and the control valve being arranged on pipeline；Meanwhile the also settable flow rate detection valve on pipeline, to the stream of conveying dispersion liquid
Speed is measured in real time.Dispersion liquid propulsion device 5 is also possible to the liquid storage tank that liquid level is higher than sample memory 2.
Control analytical equipment 6 can also be connected with dispersion liquid propulsion device 5, to control the start and stop of dispersion liquid propulsion device 5
And fltting speed.Control analytical equipment 6 can also be connect with light source, to control opening and closing and/or the wavelength of light source.
Control analytical equipment 6 obtains in real time to be believed by optical observation unit 3 by the scattering light that signal acquisition unit 4 obtains
Number generate scatter spot, the scattering optical image data of acquisition are stored and are analyzed, and to the video data of record into
Row repeats playing, and tracks, records scattering luminous point.Analytical equipment 6 is controlled when obtaining scattering optical image data, by adjusting it
The parameters such as the scattering electronics filter of optical image signal of display, contrast, to scatter optical image the most clearly, phase between scatter spot
Most weak, the scattering optical image data of storage certain time two-dimensional material are mutually influenced, according to the image data of storage, when recording unit
The numbers of particles occurred in the interior visual field, can calculate contained two-dimensional material number in unit volume, as testing result；Statistics
Two-dimensional material number value in obtained unit volume calculates two-dimensional material and is averaged piece in conjunction with required two-dimensional material parameter value
Diameter value.
As shown in connection with fig. 5, control analytical equipment 6 can be include obtaining the scattering optical image data of acquisition device in real time simultaneously
The storage unit for storing the scattering optical image data of preset time, adjusts electronics filter, contrast of the picture signal of display etc.
Parameter obtains the best adjusting unit for clearly scattering optical image, carries out calculating to the data of storage unit acquisition and obtains two-dimentional material
Expect the computing unit of average piece diameter value.Data interaction is carried out between each unit, is integrated into same chip, naturally it is also possible to be
Each chip such as passes through the CPU interacted and realizes above-mentioned function.The control analytical equipment of the present embodiment, can be to multiple letters
The signal that number acquisition unit same time obtains carries out Algorithms Integration, obtain signal it is compound after unique consequence, specifically, respectively
The information of a signal acquisition unit respectively according to preset form collator after, by control analytical equipment 6 according to same algorithm carry out
Processing；Can also, control analytical equipment 6 calculates separately the information of each signal acquisition unit according to algorithm respectively, and finally obtains
The average value that each signal acquisition unit calculates.Particularly with the same side in sample memory, several signal acquisitions are set
When unit, the signal acquisition unit of same side can respectively be handled scattered light signal according to above two mode, with
The precision of detection is improved by average value acquisition modes.
Analytical equipment is controlled according to two-dimensional material quantity, quality, the average number of plies and the two-dimentional material in the unit volume
The physical parameter of the minimum constitutional repeating unit of material calculates the average piece diameter of two-dimensional material.Before specific calculation method refers to
Described in face.
As shown in fig.6, it is two-dimensional material of the embodiment of the present invention under various concentration, measurement obtains two-dimensional material quantity
Linear relationship chart, it is known that, two-dimensional material is under various concentration, two-dimensional material quantity and the substantially linear relationship of concentration.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (19)
- The detection method of piece diameter 1. a kind of two-dimensional material is averaged characterized by comprisingTwo-dimensional material is added in solution and is uniformly mixed and forms two-dimensional material dispersion liquid；Obtain the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume；Obtain two-dimensional material quality, the averagely number of plies and the two-dimensional material in the two-dimensional material dispersion liquid unit volume The physical parameter of minimum constitutional repeating unit；According to the minimum repetitive structure of two-dimensional material quantity, quality, the average number of plies and two-dimensional material in the unit volume The physical parameter of unit calculates the average piece diameter of two-dimensional material；Wherein, the physical parameter of the minimum constitutional repeating unit of the two-dimensional material includes the minimum repetitive structure list of two-dimensional material The area of the minimum constitutional repeating unit of molal weight, two-dimensional material that member independently has.
- The detection method of piece diameter 2. two-dimensional material according to claim 1 is averaged, which is characterized in that the two-dimensional material point Two-dimensional material quality in dispersion liquid unit volume is dispersed according to the two-dimensional material of the two-dimensional material quality and acquisition that are added in solution The volume of liquid is calculated.
- The detection method of piece diameter 3. two-dimensional material according to claim 1 is averaged, which is characterized in that count according to the following formula Calculate the average piece diameter D of two-dimensional material:(1)Wherein, m is the quality of two-dimensional material in unit volume, NAFor Avogadro constant number, S is that two-dimensional material minimum repeats to tie The area of structure unit, N are the two-dimensional material quantity in the two-dimensional material dispersion liquid unit volume, and M is two-dimensional material minimum weight The molal weight that complex structure unit independently has, L are the average number of plies of two-dimensional material, and π is pi.
- The detection method of piece diameter 4. two-dimensional material according to claim 3 is averaged, which is characterized in that counted according to formula (1) After the average piece diameter D for calculating two-dimensional material, also by by the average piece diameter D of calculated two-dimensional material multiplied by an adjusted coefficient K, The average piece diameter D of the calculated two-dimensional material is modified.
- The detection method of piece diameter 5. two-dimensional material according to claim 1 is averaged, which is characterized in that obtain the two-dimentional material Expect the method for the two-dimensional material quantity in dispersion liquid unit volume are as follows:Image is shot to dispersion liquid from least two angles using optical imaging apparatus；Two-dimensional material is identified from the image of shooting respectively, and calculates two-dimensional material quantity contained in every image；The quantity of the two-dimensional material contained in each image is added, and duplicate removal, meter are carried out to the two-dimensional material contained in each image Calculate the two-dimensional material quantity obtained in unit volume.
- The detection method of piece diameter 6. two-dimensional material according to claim 5 is averaged, which is characterized in that set using optical imagery When the standby shooting image to dispersion liquid, the dispersion liquid is set to continue through the region that is taken with flow regime, the optical imagery is set It is standby to be continuously shot acquisition video image.
- The detection method of piece diameter 7. two-dimensional material according to claim 1 is averaged, which is characterized in that the solution be water, One of alcohols, ketone, aldehydes, lipid, surfactant or any combination.
- 8. a kind of method for obtaining two-dimensional material quantity characterized by comprisingImage is shot to dispersion liquid from least two angles using optical imaging apparatus；Two-dimensional material is identified from the image of shooting respectively, and calculates two-dimensional material quantity contained in every image；The quantity of the two-dimensional material contained in each image is added, and duplicate removal, meter are carried out to the two-dimensional material contained in each image Calculate the two-dimensional material quantity obtained in unit volume.
- 9. it is according to claim 8 obtain two-dimensional material quantity method, which is characterized in that using optical imaging apparatus from When at least two angles shoot image to dispersion liquid, the dispersion liquid is made to continue through the region that is taken with flow regime, it is described Optical imaging apparatus is continuously shot acquisition dynamic image, according to the dynamic image data for being continuously shot acquisition, record unit time The two-dimensional material number occurred in the interior shooting visual field, is calculated contained two-dimensional material number in unit volume.
- 10. a kind of be averaged the two-dimensional material quantity acquisition device of piece diameter for detecting two-dimensional material characterized by comprisingLight source；Sample memory, the side by close to sources are provided with light source channel, and sample memory at least part is by light transmission material Material is made, for accommodating the dispersion liquid containing two-dimensional material in the sample memory；Optical imaging apparatus, for shooting image to the dispersion liquid in the sample memory from least two angles.
- 11. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that the optical imaging apparatus has At least two, it is less than the angle setting of 180 degree in the sample memory periphery in being greater than 0.
- 12. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that the optical imaging apparatus has One, dispersion liquid is clapped for being moved to another angle within a preset time after shooting from an angle to dispersion liquid It takes the photograph.
- 13. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that the light source channel is in slit Shape.
- 14. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that the optical imaging apparatus packet Optical observation unit and signal acquisition unit are included, the optical observation unit is used to receive the scattering light of two-dimensional material, and is believing It is imaged on number acquisition unit, the signal acquisition unit is for being converted into electric signal for optical imagery and exporting.
- 15. two-dimensional material quantity acquisition device according to claim 14, which is characterized in that the optical observation unit packet Include the optical microphotograph camera lens passed through for the scattering light of the two-dimensional material.
- 16. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that the light source is fixed for wavelength Light source, alternatively, be one section of preset wavelength and continuously adjustable light source.
- 17. two-dimensional material quantity acquisition device according to claim 10, which is characterized in that set on the sample memory It is equipped with inlet and liquid outlet, dispersion liquid propulsion device is connected on the inlet.
- The detection device of piece diameter 18. a kind of two-dimensional material is averaged, which is characterized in that including claim 10-17 any one institute The acquisition device stated, further includes the control analytical equipment being connected with the acquisition device, and the control analytical equipment is used for basis The image data of the acquisition device output identifies two-dimensional material, and calculates two-dimensional material number contained in every image Amount；The quantity for the two-dimensional material for being also used to contain in each image is added, and is gone to the two-dimensional material contained in each image Weight calculates the two-dimensional material quantity obtained in unit volume.
- The detection device of piece diameter 19. two-dimensional material according to claim 18 is averaged, which is characterized in that the control analysis Device is also used to the minimum weight according to two-dimensional material quantity, quality, the average number of plies and two-dimensional material in the unit volume The physical parameter of complex structure unit calculates the average piece diameter of two-dimensional material, wherein the minimum repetitive structure of the two-dimensional material The physical parameter of unit include the minimum constitutional repeating unit of two-dimensional material independently have molal weight, two-dimensional material most The area of small constitutional repeating unit.
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