CN109580542A - A method of two-dimensional material thickness and stacking form are characterized using optical microscopy - Google Patents

A method of two-dimensional material thickness and stacking form are characterized using optical microscopy Download PDF

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Publication number
CN109580542A
CN109580542A CN201811363511.4A CN201811363511A CN109580542A CN 109580542 A CN109580542 A CN 109580542A CN 201811363511 A CN201811363511 A CN 201811363511A CN 109580542 A CN109580542 A CN 109580542A
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contrast
substrate
dimensional material
graphene
thickness
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许海腾
陈强
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Beijing Institute of Remote Sensing Equipment
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Beijing Institute of Remote Sensing Equipment
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
    • G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods

Abstract

The invention discloses a kind of methods using optical microscopy characterization two-dimensional material thickness and stacking form.Calculate several two-dimensional materials, 2H-MoS2、2H‑MoSe2、2H‑MoTe2、2H‑WSe2、2H‑NbSe2And 3R-WS2Contrast on SiO2 (300nm)/Si substrate.In addition to 2H-MoTe2Outside material, remaining material is when incident light is this wave band of 500nm-550nm, contrast has preferable discrimination with the variation of the number of plies, calculated result can utilize the size and the number of plies etc. of optical microscopy characterization mechanical stripping method or the TMDCs material of CVD method preparation according to this.For 2H-MoTe2Material can select SiO when incident light is 540nm2It is characterized with a thickness of the silicon wafer of 150nm or 340nm or so as substrate, to obtain more satisfactory result.2H-TaS is calculated separately2And 1T-TaS2Material is in SiO2Contrast on/Si substrate, the TaS of two kinds of stacking types2Material shows completely different variation pattern in contrast, may determine that the stacking form of two-dimensional material using this feature.

Description

A method of two-dimensional material thickness and stacking form are characterized using optical microscopy
Technical field
The present invention relates to a kind of methods for characterizing two-dimensional material thickness and stacking form, especially a kind of to use optical microphotograph The method of mirror characterization two-dimensional material thickness and stacking form.
Background technique
Two-dimensional material, the i.e. thin-film material of only one or several atomic layers thicks are a kind of emerging nano materials, due to Its unique structure and excellent performance cause the extensive concern of scientific circles.Two-dimensional material has the physical chemistry of many novelties Characteristic not only has important theoretical research value, and unique structure and excellent performance also make it possible in many necks Domain, such as electronic device, composite material, biological medicine, sensing etc. obtain great application achievements.Graphene, boron nitride, mistake Cross race metal disulfides (such as MoS2,WS2Deng) and transition group metallic oxide (such as TiO2Deng) etc. be all typical two dimension Material, wherein transition metal dichalcogenide is because its excellent property is the most noticeable.
Two chalcogenide of transition metal (Transition metal dichacogenides, abbreviation TMDCs) is a kind of Type stratified material extremely abundant, usually uses MX2It indicates, wherein M is transition metal, including IV race element (such as Ti, Zr, Hf Deng), V group element (such as V, Nb, Ta) or VI race element (Mo, W etc.)；And X is then chalcogen (such as S, Se, Te).Two Kind element is combined into TMDCs, such as MoS2、MoSe2、NbSe2Deng.These materials form stratified material in the form of X-M-X, As shown, wherein two X atomic layers are the sulphur atom of hexagonal lattice structure up and down, middle layer is transition metal, is similarly Hexagonal array arrangement.Adjacent layer is combined into various forms of body materials with faint Van der Waals force, they are in stack manner and gold It is different to belong to Atomic coordinate aspect.Metallic atom coordination in TMDCs can be triangular prism or octahedra mode.With graphite It compares, the TMDCs of body material shows diversified crystal form and stacking form.This is because for the MX of a single layer2, Structure includes three layers of atom, this three layers of atoms can be triangular prism or octahedral coordination.Most commonly tri- kinds of crystalline substances of 1T, 2H, 3R Body structure, as shown in Figure 1.For some TMDCs materials, between the stacking form between single layer and multi-layer morphology, different all With different property, this behavior has attracted academia widely to pay close attention to.For example, certain semiconductor TMDCs (such as MoS2、 WS2), (body material) is indirect band-gap semiconductor when multilayer, and when the number of plies is reduced to single layer, it is changed into direct band gap and partly leads Body.Multilayer or the molybdenum disulfide band gap of body material are 1.3eV, are indirect belt semiconductors, single layer molybdenum disulfide band gap increases to 1.8eV, and become directly band semiconductor.Direct band gap increases but also the photoluminescence performance of single layer molybdenum disulfide greatly enhances Add it a possibility that photoelectric field is applied.
The large-scale application of two-dimensional material be unable to do without the controllable preparation of large area, high quality.Large area, high quality at present Two-dimensional material field of film preparation mainly uses chemical vapour deposition technique.In traditional characterizing method, atomic force microscope and Raman Spectrum can be used to the number of plies of characterization two-dimensional material, but both characterization methods also suffer from respective disadvantage, such as former Sub- force microscope characterization speed is excessively slow, Raman spectrum accuracy is to be improved, thereby increases and it is possible to can cause to a certain degree to sample itself Damage.After preparing sample, how accurate and effective and while do not injure sample itself, to determine two-dimensional material The number of plies and stack manner be merit attention the problem of.
Summary of the invention
The present invention calculates two-dimensional material sample on the silica/silicon substrate of different-thickness, under different incident lights, It changes relative to the contrast of substrate.Then it is taken pictures using optical microscopy to sample, it is soft using Matlab or other interpreting blueprints Part obtains the actual contrast of sample photo, and contrast theory calculated value can not needed using atomic force microscope and Raman In the case where spectrometer, using information such as the number of plies of optical microscopy characterization two-dimensional material and stack manners.The two-dimentional material being related to Material mainly includes 2H-MoS2、2H-MoSe2、2H-MoTe2、2H-WSe2、2H-NbSe2、3R-WS2、TaS2。
Method proposed by the present invention using optical microscopy characterization two-dimensional material thickness and stacking form, feature exist In, comprising the following steps:
Step 1: theoretical calculation obtain different thickness, the two-dimensional material of different stacking form under specific incident light, serving as a contrast Contrast theoretical value on bottom simultaneously gives the curve graph of contrast theoretical value, the number of plies and incident wavelength；
Step 2: the optical filter for being suitable for the specific wavelength of material contrast-response characteristic described in respective two-dimensional is selected, light is utilized Learn the optics picture of two-dimensional material described in microscope photographing and specific substrate under the irradiation of specific incident light；
Step 3: the rgb value of the captured two-dimensional material and substrate picture is read, captured described two are calculated Tie up contrast actual value of the material relative to specific substrate；
Step 4: contrast actual value calculated in step 3 is compared with the curve graph in step 1, thus Obtain the thickness and stack manner information of two-dimensional material.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of two-dimensional material.
Fig. 2 is air/MoS2/SiO2The interference of light schematic diagram of tetra- layers of medium of/Si.
Fig. 3 is (a) single layer 2H-MoS2, (b) different layers of 2H-MoS2, (c) single layer 2H-MoSe2, (d) different layers of 2H-MoSe2(e) single layer 2H-MoTe2, (f) different layers of 2H-MoTe2In SiO2Contrast on (300nm)/Si substrate with The change curve of lambda1-wavelength.
Fig. 4 be incident light be 540nm when, (a) single layer MoTe2, (b) multilayer MoTe2In the SiO of different-thickness2/ Si substrate On contrast.
Fig. 5 is 2H-NbSe2、2H-WSe2And 3R-WS2In SiO2Contrast on (300nm)/Si substrate.
Fig. 6 is (a) single layer 2H-TaS2, (b) different layers of 2H-TaS2, (c) single layer 1T-TaS2, (d) different layers of 1T-TaS2In SiO2Contrast on (300nm)/Si substrate with lambda1-wavelength change curve (e) single layer 2H-TaS2It is (black Line), 1T-TaS2(red line) is in SiO2Contrast on (300nm)/Si substrate with lambda1-wavelength change curve.
Fig. 7 is (a) MoS2Optical microscope photograph, incident light 520nm, (b) using software treated picture.
Specific embodiment
Below in conjunction with the attached drawing technical solution that the present invention will be described in detail.
Firstly, calculating 2H-MoS2、2H-MoSe2、2H-MoTe2、2H-WSe2、2H-NbSe2And 3R-WS2Etc. two-dimensional materials In 300nmSiO2Contrast theoretical value on/Si substrate, then using optical microscopy shoot above-mentioned two-dimensional material it is specific enter It penetrates under light, in 300nmSiO2Optics picture on/Si substrate, then obtains contrast experiment value using matlab software, with reason By the number of plies information of value comparison you can get it the material.2H-TaS is calculated separately2And 1T-TaS2Material is in SiO2On/Si substrate Contrast, two kinds stacking type TaS2Material shows completely different variation pattern in contrast, utilizes this Feature can be used to judge the stacking form of the material.
Step 1: theoretical calculation.
With 2H-MoS2For, as shown, giving air/2H-MoS2The interference of light of four layers of medium of/silica/silicon Schematic diagram.Single-layer graphene can be equivalent to the film that a layer thickness is 0.67nm, and complex refractivity index n1 is (with lambda1-wavelength Variation) it can be written as Re (n1)-iIm (n1), wherein Re (n1) is the refractive index of medium, and Im (n1) is that incident light passes in the medium The decaying of sowing time, the i.e. absorption coefficient of medium.Silicon dioxide layer can be considered as the film that one layer of refractive index is n2, and refractive index is only There is real part and change with lambda1-wavelength and change, such as refractive index is 1.47 when incident light is 450nm, incident light 700nm When refractive index be 1.455.It, can be by its etc. since the thickness of silicon substrate is more than graphene and the several orders of magnitude of silica membrane Effect is the dielectric layer for the semo-infinite thickness that refractive index is n3.The refractive index of three layers of medium changes with the variation of lambda1-wavelength.
Firstly, for simple silica/silicon substrate, there is no any two-dimensional material, equivalent Fresnel coefficient aboveFor,
Wherein,(niFor medium refraction index, diFor dielectric thickness, λ is incidence Optical wavelength)
Then, silica/silicon substrate is equivalent to thin film, adds graphene, equivalent Fresnel coefficientFor,
Finally, the light intensity R of reflected light can be written as when incident light is by graphene/silicon dioxide/silicon thin film,
In order to calculate the reflected light light intensity of substrate, it is only necessary to regard graphene as air layer, reflectivity is directly written as n1 =1, the reflected light light intensity of substrate can be calculated from formula.
Contrast (contrast) Contrast between graphene and substrate is defined as through graphene and does not pass through graphene Reflective light intensity relative intensity, formula is as follows:
Unified choose has the Si of the SiO2 layer of one layer of 300nm thickness as substrate, has calculated separately 2H-MoS2、2H-MoSe2、 2H-MoTe2、2H-WSe2、2H-NbSe2And 3R-WS2Contrast over the substrate is made that contrast with wavelength change Curve graph.
Fig. 3 is respectively 2H-MoS2、2H-MoSe2And 2H-MoTe2In SiO2Contrast on (300nm)/Si substrate.From 3 (b) in, it can be seen that in this wave band of 500nm-550nm, MoS2Changing with the number of plies, contrast becomes larger, and distinguishes obviously, MoS can be characterized with optical microscopy under the wave band incident light2The number of plies.In the red light region of 650nm or so, although right It is become apparent than degree difference, but since in the wave band, the reflective light intensity of the reflected light intensity ratio material of substrate is much bigger, shows Material color can be very dark in visual field, is unfavorable for observing.Moreover, in red light region, few layer MoS2It will appear exciton resonance effect, It equally will affect MoS2Reflectivity therefore do not consider using the wave band as the ideal wave band of characterization.For 2H-MoSe2Material For material, in this wave band of 500nm-550nm, contrast difference is still obvious with the variation of the number of plies.
And for MoTe2Material, in entire bluish-green optical band, contrast difference is not obvious, for example works as lambda1-wavelength When for 540nm, single layer and double-deck contrast are only 5% and 2% respectively.Since contrast and the relationship of substrate are also very big, because This calculates under certain lambda1-wavelength and (chooses 540nm), MoTe2Contrast with SiO2The variation relation curve of thickness. Figure 4, it is seen that working as SiO2For the thickness of layer in 80nm and 260nm, contrast reaches maximum value, and with the number of plies Variation, contrast distinguish clearly.But this contrast at two is positive value, that is to say, that the reflective light intensity of substrate is higher than The reflective light intensity of material, material seem that color can be unfavorable for observing than darker in light microscopic.It, can be in view of this reason Select the SiO of 150nm and 340nm or so2Layer carries out MoTe as substrate2Characterization, to obtain ideal result.
Fig. 5 is respectively 2H-NbSe2、2H-WSe2And 3R-WS2Contrast on SiO2 (300nm)/Si substrate, can be with Find out, in the window area of 500-550nm, for these three materials with the variation of the number of plies, contrast also has preferable discrimination, can To use optical microscopy as characterization method.
Since TMDCs material has multiple stacking form, such as 1T type, 2H type and 3R type.Stacking form difference will affect material The properties such as the property of material, such as its dielectric constant make it in substrate to influence the features such as the refractive index of material, extinction coefficient The contrast on surface changes.2H-TaS is calculated separately2And 1T-TaS2Material is in SiO2Contrast on/Si substrate, such as Shown in Fig. 6, it can be seen that the TaS of two kinds of stacking types2Material shows completely different variation pattern in contrast, benefit With this feature, it can be determined that the stacking form of material.
Step 2 shoots the optics of two-dimensional material and specific substrate under the irradiation of specific incident light using optical microscopy Picture.
Equally by taking 2H-MoS2 as an example, single layer MoS2 is selected to shoot optical microscope photograph, the optical filter wavelength of selection is 520nm, such as Fig. 7 (a).
Step 3 calculates the contrast in photo using RGB principle.
The RGB data that picture is read using Matlab, is calculated from the formula the brightness value Y of material in picture, formula is such as Under:
Y=0.299*R+0.587*G+0.114*B
The brightness Y of substratesIt can be averaged and be obtained by the RGB data of substrate portions in figure.It can thus find out MoS2It relative to the contrast of substrate, and maps, sees that Fig. 7 (b), formula are as follows:
Contrast=(Y-Ys)/Ys。
Step 4: contrast actual value calculated in step 3 is compared with the curve graph in step 1, thus Obtain the thickness and stack manner information of two-dimensional material.
By being compared with calculated value, it can be deduced that: the red circle part in Fig. 7 (b), contrast be 10%~ 15%, it is single layer；Bright triangle in black circle, contrast are 30%~40%, for bilayer.

Claims (5)

1. a kind of method using optical microscopy characterization two-dimensional material thickness and stacking form, which is characterized in that including following Step:
Step 1: theoretical calculation obtain different thickness, the two-dimensional material of different stacking form under specific incident light, on substrate Contrast theoretical value and give the curve graph of contrast theoretical value, the number of plies and incident wavelength；
Step 2: selecting the optical filter for being suitable for the specific wavelength of material contrast-response characteristic described in respective two-dimensional, aobvious using optics Micro mirror shoots the optics picture of the two-dimensional material and specific substrate under the irradiation of specific incident light；
Step 3: reading the rgb value of the captured two-dimensional material and substrate picture, calculates the captured two-dimentional material Expect the contrast actual value relative to specific substrate；
Step 4: contrast actual value calculated in step 3 is compared with the curve graph in step 1, to obtain The thickness and stack manner information of two-dimensional material.
2. the method according to claim 1, wherein the substrate is silica/silicon lining in step 1 Bottom.
3. according to the method described in claim 2, it is characterized in that, in step 1, for above without any two-dimensional material Silica/silicon substrate, equivalent Fresnel coefficientFor,
Wherein,(niFor medium refraction index, diFor dielectric thickness, λ is incident light wave It is long),
Then, silica/silicon substrate is equivalent to thin film, adds graphene, equivalent Fresnel coefficient For,
Finally, when incident light is by graphene/silicon dioxide/silicon thin film, the light intensity R of reflected light is,
Regard graphene as air layer, reflectivity n1=1,
Contrast (Contrast) between graphene and substrate is defined as by graphene and not by the reflected light of graphene Strong relative intensity, formula are as follows:
4. the method according to claim 1, wherein the wavelength of the optical filter is 520nm in step 2.
5. the method according to claim 1, wherein the RGB data of picture is read, according to public affairs in step 3 Formula calculates the brightness value Y of material in picture, and formula is as follows:
Y=0.299*R+0.587*G+0.114*B
The brightness Y of substratesIt can be averaged and be obtained by the RGB data of substrate portions in figure, find out two-dimensional material relative to lining The contrast at bottom, formula are as follows:
Contrast=(Y-Ys)/Ys。
CN201811363511.4A 2018-11-16 2018-11-16 A method of two-dimensional material thickness and stacking form are characterized using optical microscopy Pending CN109580542A (en)

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CN113437630A (en) * 2021-06-07 2021-09-24 中国科学院上海光学精密机械研究所 Based on 1T-TaS2And its application in laser
CN114235752A (en) * 2021-12-17 2022-03-25 江南大学 Optical method for identifying two-dimensional material layer number in two-dimensional three-dimensional material heterojunction
CN116297337A (en) * 2022-09-09 2023-06-23 山东大学 Method for judging number of layers of two-dimensional material by using dark field optical imaging technology

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CN113437630A (en) * 2021-06-07 2021-09-24 中国科学院上海光学精密机械研究所 Based on 1T-TaS2And its application in laser
CN114235752A (en) * 2021-12-17 2022-03-25 江南大学 Optical method for identifying two-dimensional material layer number in two-dimensional three-dimensional material heterojunction
CN114235752B (en) * 2021-12-17 2024-02-09 江南大学 Optical method for identifying number of layers of two-dimensional material in two-dimensional three-dimensional material heterojunction
CN116297337A (en) * 2022-09-09 2023-06-23 山东大学 Method for judging number of layers of two-dimensional material by using dark field optical imaging technology
CN116297337B (en) * 2022-09-09 2023-10-31 山东大学 Method for judging number of layers of two-dimensional material by using dark field optical imaging technology

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Application publication date: 20190405