CN103011185B - Preparation method for mica flakes having nanostructure - Google Patents
Preparation method for mica flakes having nanostructure Download PDFInfo
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- CN103011185B CN103011185B CN201110279528.3A CN201110279528A CN103011185B CN 103011185 B CN103011185 B CN 103011185B CN 201110279528 A CN201110279528 A CN 201110279528A CN 103011185 B CN103011185 B CN 103011185B
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Abstract
The present invention relates to a method for preparing mica flakes having a nanostructure by using atomic force microscope micromechanical processing. According to the present invention, a mechanical stripping method is adopted to prepare monolayer or a few layers of mica flakes, and the mica flakes can be adopted as a substrate to prepare a nanostructure on the obtained mica flake by using an atomic force microscope micromechanical processing method, wherein the nanostructure can be obtained through the following steps: placing the mica flake on a solid substrate so as to make the work of the atomic force microscope in a contact mode, and controlling acting force of contact of the atomic force microscope tip and the mica flake so as to control the obtained nanostructure on the mica flake; the method for preparing the mica flakes by using the micromechanical stripping method has characteristics of simple operation method, convenient and easy performing, and less defects; and the nanostructure prepared by using the atomic force microscope micromechanical processing method has characteristics of controllable thickness, atomic level accuracy, controllable shape and controllable position, wherein the patterned nanostructure can be prepared.
Description
Technical field
The present invention relates to utilize the preparation of atomic force microscope micromachined to there is the method for the mica sheet of nanostructure.
Background technology
The individual layer that the Graphene of take is in recent years representative or the layered crystal two-dimensional material of minority layer, because it has good performance and wide application prospect, have caused people's extensive concern.Mica, as a kind of stratified material, has perfect divisibility, is the good source of two-dimensional material.Because mica has unreactiveness, thermal insulation and electrical insulating property, be different from Graphene completely, thereby have unique significant application value in some field.The technology of preparing of the nanostructure of the two-dimensional material based on individual layer or minority layer all concentrates on the Graphene of conduction at present, the research of Graphene has represented two-dimensional material in nanostructure, unique advantage (Garaj, the S. in especially ultra-thin asymmetric nanoporous field; Hubbard, W.; Reina, A.; Kong, J.; Branton, D.; Golovchenko, J.A.Nature 2010,467, and 190).Yet, the preparation method of the nanostructure of the layered crystal two-dimensional material based on insulation individual layer or minority layer still rarely has report, and the method for preparing the nanostructure of other two-dimensional material is mainly electron beam or ion beam etching (Dekker, C.Nature Nanotechnology 2007,2,209), the complex process of aforesaid method, with high costs.Find method simple and effective, with low cost and prepare the nanostructure of two-dimensional material, especially the nanostructure of the two-dimensional material of the layered crystal based on insulation individual layer or minority layer remains a large difficult point.
It is simply effective, with low cost that the method for atomic force microscope micromachined has preparation technology, can accurately control thickness, position and the shape of the nanostructure of preparation two-dimensional material, prepare patterning nanostructure, except mica, the method is also applicable to other two-dimensional material.
Summary of the invention
The object of this invention is to provide a kind of method of utilizing the preparation of atomic force microscope micromachined to there is the mica sheet of nanostructure.
In method of the present invention, relate to and adopt mechanically peel legal system for the mica sheet of individual layer or minority layer, and available this mica sheet is substrate, utilize the method for atomic force microscope micromachined to prepare nanostructure on gained mica sheet.
The method of utilizing the preparation of atomic force microscope micromachined to there is the mica sheet of nanostructure of the present invention: mica sheet is placed in solid substrate, the work of atomic force microscope is under contact mode, the reactive force that the needle point of control atomic force microscope contacts with mica sheet, to be controlled at the nanostructure obtaining on mica sheet.
The shape of described nanostructure and the control of position are to be controlled by the size of the area of the position of the needle point scanning mica sheet of atomic force microscope and scanning mica sheet.
The nanostructure obtaining on described mica sheet is selected from nanoporous, nano wire, limit number and is more than or equal to more than one in three Polygons, circle etc.
Described mica sheet be selected from the thin slice of the mica of synthetic, the thin slice of the phlogopite of self-sow, the thin slice of the white mica of self-sow, a kind of in the thin slice of the biotite of self-sow etc.
The number of plies of described mica sheet is 1～100 layer.
Layer in the number of plies of described mica sheet refers to one deck mica molecular structure unit.
Mica sheet described in the present invention can obtain by the following method: the two sides of a mica splitting is bonded at respectively on adhesive tape, tear adhesive tape, one mica splitting is peeled off into two cloudlet master slices, again the two sides of peeling off the sheet mica obtaining is bonded at respectively on adhesive tape, tear adhesive tape, sheet mica is peeled off into two cloudlet master slices again; Repeat above step, can obtain the mica sheet of the required number of plies, preferably obtain the number of plies and be the mica sheet of 1～100 layer.Selecting of the mica sheet of the required number of plies is that the mica sheet on adhesive tape is transferred in solid substrate, utilizes opticmicroscope in conjunction with atomic force microscope, to characterize thickness and the number of plies of mica sheet, picks out the mica sheet of the required number of plies.
The described opticmicroscope that utilizes is after mica sheet is transferred in solid substrate in conjunction with the atomic force microscope sign thickness of mica sheet and the method for the number of plies, with opticmicroscope, record the characteristic color of mica sheet or mica sheet and the light intensity contrast ratio of solid substrate around, then utilize atomic force microscope to measure to record the thickness of mica sheet, obtain the optical signature of mica sheet and the corresponding relation of thickness, after being convenient to, according to optical signature, find easily the mica sheet of the required number of plies.
Described mica be selected from the mica of synthetic, the white mica of the phlogopite of self-sow, self-sow, a kind of in the biotite of self-sow etc.
Described adhesive tape comprises various cloth or the plastics films that scribble bala gutta.
Layer in the number of plies of described mica sheet refers to one deck mica molecular structure unit.
The material of described solid substrate is selected from one or more in silicon, magnesium, aluminium, iron, copper, nickel, zinc, gold and silver or their oxide compound or nitride, or is selected from carbon, or be selected from above-mentioned materials any two or more.
What in the inventive method, relate to utilizes mechanically peel legal system simple for the working method of mica sheet, convenient and easy, and defect is few.The thickness of the nanostructure that the atomic force microscope micromachined method relating in the inventive method prepares is controlled, precision reaches atomic level, and shape, the position of nanostructure are controlled, and can prepare the nanostructure of patterning, except mica, the present invention is also applicable to other two-dimensional material.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1. for mechanically peel is prepared the mica sheet of individual layer or minority layer, and utilize atomic force microscope micromachined to prepare the schematic diagram of nanostructure.
Fig. 2. the embodiment of the present invention 1, 2, 3, 4 mechanically peel method prepares 8 layers, 28 layers, 9 layers, the opticmicroscope of 6 layers of mica sheet and the photo of atomic force microscope, respectively as the second row in figure (Fig. 2 a-c), the first row (Fig. 2 d-f), the third line (Fig. 2 g-i), shown in fourth line (Fig. 2 j-1), wherein the solid substrate in the second row figure is 250nm silica/silicon (the silicon-dioxide of 250 nanometer thickness covers in silicon base), solid substrate in the first row figure is silicon base, solid substrate in the third line figure is 300nm silica/silicon (the silicon-dioxide of 300 nanometer thickness covers in silicon base), solid substrate in fourth line figure is 500nm silica/silicon (the silicon-dioxide of 500 nanometer thickness covers in silicon base), first row in every row figure is optical photograph above, secondary series is atomic force microscopy, the 3rd row are atomic power height maps.
Fig. 3. optics and the atomic force microscopy of the ultra-thin asymmetric nanoporous preparing on the mica sheet of 10 layers of the use atomic power micromachined method of the embodiment of the present invention 1 in the solid substrate of 250nm silica/silicon; A figure is its atomic force microscopy; B figure is its optical photograph, and b figure upper right corner illustration is the optical photograph of solid substrate, and the osculum end of the ultra-thin asymmetric nanoporous preparing is about 68 nanometers, hole depth 9.6 nanometers; C figure is the shape schematic diagram of ultra-thin asymmetric nanoporous, and nanoporous is square.
Fig. 4. when the control of the embodiment of the present invention 1,6 applies the needle point of atomic force microscope and the different reactive force of mica sheet contact, the three-dimensional Photomicrograph of atomic power of the ultra-thin asymmetric nanoporous of the different depths obtaining, when reactive force is respectively 863, receives ox (nN), 1613 and receive ox (nN), 2363 and receive ox (nN), 3112 and receive ox (nN), 3863 and receive ox (nN), obtain the nanoporous of a series of degree of depth, its degree of depth is respectively 2,4,7,8,9 stratus parent molecule structural units, as shown in Fig. 4 a-e, Fig. 4 f is the statistical graph of Fig. 4 a-e.
Fig. 5. the needle point scanning region of the control atomic force microscope of the embodiment of the present invention 1 is 120 nanometer * 120 nanometers, obtain big opening end and be about 120 nanometer * 120 nanometers, osculum end is about the ultra-thin asymmetric nanoporous of 20 nanometer * 20 nanometers, a figure is atomic force microscopy vertical view, and b figure is inverted atomic force microscopy three-dimensional plot.
Fig. 6. the needle point scanning region of the control atomic force microscope of the embodiment of the present invention 1,5 is respectively 15 nanometer * 15 nanometers, 30 nanometer * 30 nanometers, 60 nanometer * 60 nanometers, 80 nanometer * 80 nanometers, 100 nanometer * 100 nanometers, 120 nanometer * 120 nanometers, 180 nanometer * 180 nanometers, 250 nanometer * 250 nanometers, 300 nanometer * 300 nanometers, 500 nanometer * 500 nanometers, obtain the ultra-thin asymmetric nanoporous of a series of different shapeies and size, respectively as shown in Fig. 6 a, b, c, d, e, f, g, h, i, j, k.
Fig. 7. the schematic diagram of the nanostructure of the difform patterning that the needle point scanning region of the control atomic force microscope of embodiment of the present invention 12-16 and the Multiple-Scan of scanning position obtain, wherein a-e figure be respectively that array is square, the nanostructure schematic diagram of array trilateral, array circle, nano wire, right-angled intersection nano wire.
Embodiment
Embodiment 1.
1), the preparation of mica sheet
The two sides of the white mica of a slice self-sow is bonded at respectively on adhesive plaster, tear adhesive plaster, white mica described in a slice is peeled off into two white clouds master slices, again the two sides of peeling off the white clouds master slice obtaining is bonded at respectively on adhesive plaster, tear adhesive plaster, by last time peeling off the white clouds master slice obtaining, peel off into again two white clouds master slices; Repeat above step several times, can obtain the mica sheet of the required number of plies;
2), shift and find the mica sheet of the required number of plies
By step 1) adhesive plaster that obtains adheres in the solid substrate of 250nm silica/silicon, the adhesive plaster of tearing, mica sheet on adhesive plaster is transferred in the solid substrate of 250nm silica/silicon, this solid substrate is placed in to optical microphotograph Microscopic observation, can be observed the sheet mica thin slice of micro-meter scale, the color of mica sheet changes with its thickness, record the characteristic color of the mica sheet of observing or itself and the light intensity contrast ratio of solid substrate (top does not have the 250nm silica/silicon of mica) around, then by atomic force microscope, measure thickness the record of this mica sheet, to set up the optical signature of this mica sheet and the corresponding relation of thickness, according to optical signature, find the mica sheet of the required number of plies, refer to the second row in Fig. 2, the characteristic color of the mica sheet in e figure and light intensity contrast ratio and f figure, the thickness of this mica sheet in g figure (8 layers) has been set up one-to-one relationship, the mica sheet that runs into same color or optical contrast while later utilizing observation by light microscope just can be determined its thickness under the condition without atomic force microscope observation, then the corresponding relation that utilizes above-mentioned same first coupling opticmicroscope and atomic force microscope observation to determine optical signature and thickness, by the method that opticmicroscope is found separately, can find the mica sheet of 10 layers as shown in Figure 3 again,
3), utilize the preparation of atomic force microscope micromachined to there is the mica sheet of nanostructure
Use the atomic force microscope under contact mode, the needle point of atomic force microscope is used the needle point that is coated with the relatively hard materials such as silicon nitride or diamond, by step 2) mica sheet that obtains is placed in the solid substrate of 250nm silica/silicon, the work of atomic force microscope is under contact mode, the reactive force that the needle point of control atomic force microscope contacts with mica sheet, progressively strengthen reactive force, needle point scanning step 2 by atomic force microscope) mica sheet of 10 layers obtaining, to prepare ultra-thin asymmetric nanoporous.Control the needle point of atomic force microscope and the amount of force of mica sheet to control the thickness of ultra-thin asymmetric nanoporous, in control action kou power, be 3863 to receive ox, the hole depth of the ultra-thin square asymmetric nanoporous preparing is about 9.6 nanometers (9 stratus parent molecule structural unit), osculum end is about 68 nanometers, atomic force microscopy figure as shown in Figure 3 a and the optical microscopy map shown in Fig. 3 b, the 3D shape of ultra-thin asymmetric nanoporous shape schematic diagram as shown in Figure 3 c, the degree of depth of ultra-thin asymmetric nanoporous is as shown in Fig. 4 e.
The scanning position of the needle point of control atomic force microscope and region are to be controlled at the size of preparing ultra-thin asymmetric nanoporous on mica sheet, if gated sweep region is 120 nanometer * 120 nanometers, obtain big opening end and be about 120 nanometer * 120 nanometers, osculum end is about the ultra-thin square asymmetric nanoporous of 20 nanometer * 20 nanometers, inverted atomic force microscopy three-dimensional plot shown in atomic force microscopy figure as shown in Figure 5 a, Fig. 5 b, the atomic force microscopy figure as shown in Fig. 6 f.
The ultra-thin asymmetric nanoporous of embodiment 2. preparations based on mica sheet
Preparation method is substantially with embodiment 1, and difference is: employing silicon chip is solid substrate, and the mica sheet obtaining is thereon as shown in the height map of the atomic force microscopy figure of the optical photograph of Fig. 2 a, Fig. 2 b and Fig. 2 c.
The ultra-thin asymmetric nanoporous of embodiment 3. preparations based on mica sheet
Preparation method is substantially with embodiment 1, and difference is: adopt the solid substrate of 300nm silica/silicon, the mica sheet obtaining is thereon as shown in the height map of the atomic force microscopy figure of the optical photograph of Fig. 2 h, Fig. 2 i and Fig. 2 j.
The ultra-thin asymmetric nanoporous of embodiment 4. preparations based on mica sheet
Preparation method is substantially with embodiment 1, and difference is: adopt the solid substrate of 500nm silica/silicon, the mica sheet obtaining is thereon as shown in the height map of the atomic force microscopy figure of the optical photograph of Fig. 2 k, Figure 21 and Fig. 2 m.
The ultra-thin asymmetric nanoporous of embodiment 5. preparations based on mica sheet
Preparation method is substantially with embodiment 1, difference is: gated sweep region is respectively 15 nanometer * 15 nanometers, 30 nanometer * 30 nanometers, 60 nanometer * 60 nanometers, 80 nanometer * 80 nanometers, 100 nanometer * 100 nanometers, 180 nanometer * 180 nanometers, 250 nanometer * 250 nanometers, 300 nanometer * 300 nanometers, 500 nanometer * 500 nanometers, obtain the ultra-thin asymmetric nanoporous of a series of different shapeies and size, as shown in figure a, b in Fig. 6, c, d, e, g, h, i, j, k, the shape and size of nanoporous can accurately be controlled by scanning area as can be seen here.
The ultra-thin asymmetric nanoporous of embodiment 6. preparations based on mica sheet
Preparation method is substantially with embodiment 1, difference is: strengthen gradually the reactive force of the needle point of atomic force microscope to mica sheet, reactive force is received ox to 1613 from 863 and is received ox, 2363 and receive ox, 3112 and receive ox, peel off layer by layer mica and prepare ultra-thin asymmetric nanoporous, obtain the nanoporous of a series of degree of depth, its degree of depth is respectively 2,4,7,8 stratus parent molecule structural units, respectively as shown in Fig. 4 a-d.
The ultra-thin asymmetric nanoporous of embodiment 7. preparations based on mica sheet
Preparation method is substantially with embodiment 1, and difference is: mica sheet used is 100 layers.
The ultra-thin asymmetric nanoporous of embodiment 8. preparations based on individual layer mica sheet
Preparation method is substantially with embodiment 1, and difference is: mica sheet used is individual layer.
The ultra-thin asymmetric nanoporous of embodiment 9. preparations based on mica sheet
Preparation method is substantially with embodiment 1, and difference is: mica used is selected from artificial mica synthesis.
The ultra-thin asymmetric nanoporous of embodiment 10. preparations based on mica sheet
Preparation method is substantially with embodiment 7, and difference is: mica used is selected from artificial mica synthesis.
The ultra-thin asymmetric nanoporous of embodiment 11. preparations based on individual layer mica sheet
Preparation method is substantially with embodiment 8, and difference is: mica used is selected from artificial mica synthesis.
Nanostructure and the patterning nanostructure of embodiment 12. preparations based on mica sheet
Preparation method is substantially with embodiment 1, difference is: the needle point of controlling atomic force microscope step 3) scans at previously selected different positions, obtain the nanostructure of the trilateral of array, square, circular, nano wire, right-angled intersection pattern of nanowires, as shown in Fig. 7 a-e.
Nanostructure and the patterning nanostructure of embodiment 13. preparations based on mica sheet
Preparation method is substantially with embodiment 12, and difference is: mica sheet used is 100 layers.
Nanostructure and the patterning nanostructure of embodiment 14. preparations based on individual layer mica sheet
Preparation method is substantially with embodiment 13, and difference is: mica sheet used is individual layer.
Nanostructure and the patterning nanostructure of embodiment 15. preparations based on individual layer mica sheet
Preparation method is substantially with embodiment 14, and difference is: mica used is selected from artificial mica synthesis.
Nanostructure and the patterning nanostructure of embodiment 16. preparations based on individual layer mica sheet
Preparation method is substantially with embodiment 15, difference is: the needle point of controlling atomic force microscope step 3) scans at previously selected different positions, obtain the nanostructure of the trilateral of array, square, circular, nano wire, right-angled intersection pattern of nanowires, as shown in Fig. 7 a-e.
Claims (5)
1. the preparation method of a mica sheet, it is characterized in that: the two sides of a mica splitting is bonded at respectively on adhesive tape, tear adhesive tape, one mica splitting is peeled off into two cloudlet master slices, again the two sides of peeling off the sheet mica obtaining is bonded at respectively on adhesive tape, tear adhesive tape, sheet mica is peeled off into two cloudlet master slices again; Repeat above step, obtain the mica sheet of the required number of plies; Selecting of the mica sheet of the required number of plies is that the mica sheet on adhesive tape is transferred in solid substrate, utilizes opticmicroscope in conjunction with atomic force microscope, to characterize thickness and the number of plies of mica sheet, picks out the mica sheet of the required number of plies.
2. method according to claim 1, it is characterized in that: the described opticmicroscope that utilizes is after mica sheet is transferred in solid substrate in conjunction with the atomic force microscope sign thickness of mica sheet and the method for the number of plies, with opticmicroscope, record the characteristic color of mica sheet or mica sheet and the light intensity contrast ratio of solid substrate around, then utilize atomic force microscope to measure to record the thickness of mica sheet, obtain the optical signature of mica sheet and the corresponding relation of thickness, according to optical signature, find the mica sheet of the required number of plies.
3. method according to claim 1, is characterized in that: described mica is selected from the phlogopite of the mica of synthetic, self-sow, a kind of in the biotite of the white mica of self-sow, self-sow.
4. method according to claim 1, is characterized in that: described adhesive tape comprises cloth or the plastics film that scribbles bala gutta.
5. method according to claim 1, it is characterized in that: the material of described solid substrate is selected from one or more in silicon, magnesium, aluminium, iron, copper, nickel, zinc, gold and silver or their oxide compound or nitride, or be selected from carbon, or be selected from above-mentioned materials any two or more.
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| CN104445235B (en) * | 2014-12-05 | 2016-06-01 | 武汉理工大学 | The preparation method of a kind of two-dimensional nano white mica |
| CN106976887A (en) * | 2017-04-19 | 2017-07-25 | 合肥工业大学 | A kind of a large amount of methods for preparing two-dimensional nano mica sheet of utilization liquid phase ultrasound |
| WO2019071499A1 (en) * | 2017-10-12 | 2019-04-18 | 深圳先进技术研究院 | Method for preparing mica film |
| CN110455317A (en) * | 2019-07-05 | 2019-11-15 | 华南师范大学 | A kind of high-temperature flexible sensor and preparation method thereof |
| CN111716548B (en) * | 2020-06-08 | 2021-11-12 | 安徽锐光电子科技有限公司 | Thick mica sheet stripping device for mica sheet production and using method thereof |
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| CN101143708A (en) * | 2007-08-17 | 2008-03-19 | 中国科学技术大学 | Method for preparing ultra-thin two-dimension graphite sheet |
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