CN105019030A - Highly-matched crystal orientation stacked structure of graphene and hexagonal boron nitride and preparation method of highly-matched crystal orientation stacked structure - Google Patents
Highly-matched crystal orientation stacked structure of graphene and hexagonal boron nitride and preparation method of highly-matched crystal orientation stacked structure Download PDFInfo
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Abstract
The invention provides a highly-matched crystal orientation stacked structure of graphene and hexagonal boron nitride and a preparation method of the highly-matched crystal orientation stacked structure. The method includes the steps that a primary stacked structure of the graphene and the hexagonal boron nitride is formed; the primary stacked structure is subjected to heat treatment to obtain the highly-matched crystal orientation stacked structure of the graphene and the hexagonal boron nitride. On the basis that the graphene rotates on a hexagonal boron nitride crystal during heat treatment, crystal orientation match of the graphene and the hexagonal boron nitride is facilitated, and a graphene and boron nitride stacked structure with perfectly-matched crystal orientation is obtained. The method avoids the uncertainty existing in a mechanical alignment mode in the prior art; besides, boundary crystal orientation of the graphene and boundary crystal orientation of the hexagonal boron nitride are unrelated, and even if graphene and hexagonal boron nitride with irregular boundary can achieve high match. Besides, according to the method, the machining and control technology is mature, and the method is suitable for the stacked structure of the grapheme and the hexagonal boron nitride and can extend to preparation of other similar structures, such as a graphene and graphite system.
Description
Technical field
The present invention relates to field of nanometer technology, height crystal orientation coupling stacked structure particularly relating to a kind of Graphene/hexagonal boron nitride and preparation method thereof.
Background technology
Graphene has many excellent properties as Two-dimensional Carbon material, (Science306 is prepared by the scientist of Univ Manchester UK since 2004,666 (2004)), since, the numerous characteristics of Graphene is gradually by people are understood.Graphene can suspend or be attached on substrate by Van der Waals for, and Graphene property list on various substrates reveals significant difference, and this illustrates the importance of substrate to the thin material of this atom level.
Hexagonal boron nitride has the surface of atomically flating, and surface does not almost hang valence link and doping electric density is extremely low, and showing it can as the great potential of the substrate of Graphene.People observe up to 60,0000cm in the grapheme material of hexagonal boron nitride as substrate
2v
-1s
-1mobility and quantum hall effect.Hexagonal boron nitride is the same with Graphene is also polynuclear plane, and lattice parameter and Graphene have the difference of 1.8%, and this difference causes Graphene/hexagonal boron nitride stacked structure to have Moire fringe to be formed on the surface of Graphene.This Moire fringe has larger impact to being with of Graphene, and its electrical properties shows peculiar superlattice dirac point, and in addition, to the performance of the other sides such as Graphene as Raman trait, interface friction etc. have obvious impact.Meanwhile, the size of Moire fringe is closely related with the relative crystal orientation of Graphene and hexagonal boron nitride, and research finds to only have crystal orientation close to the Morie fringe that just can obtain having large-size during coupling, and the structure of this crystal orientation coupling is a kind of well material.Numerous characteristics such as the superlattice dirac point in electrology characteristic showing as Graphene is easy to observe, and this kind of structural table reveals larger interface friction and fabulous thermostability, is conducive to the device that processability is stable.Although the structure with matched well has many excellent properties, but its preparation method is more difficult.The method that current people develop mainly comprises mechanical transfer method and epitaxial growth method.
Graphene/usual the crystal orientation of hexagonal boron nitride stacked structure adopting mechanical transfer method to obtain is random, and relative angle during very difficult control transfer is to reach crystal orientation coupling.The method controlling relative angle during transfer is only limitted to Graphene and the boron nitride with regular borders, then can not with using the method for the Graphene of irregularity boundary and boron nitride, therefore, mechanical transfer method has larger limitation, especially for mechanical transfer to the Graphene on boron nitride surface, owing to polluting and fold, the crystal orientation after transfer is then difficult to change again.
Epitaxial growth method is namely at boron nitride surface extending and growing graphene, generally utilize plasma activated chemical vapour deposition, although the Graphene that the method obtains/hexagonal boron nitride stacked structure has perfect crystal orientation coupling, but deposition and nucleation process in easily cause uneven, the Graphene grown has more defect, inevitably has a negative impact to the performance of material.
Therefore, at present in the urgent need to there is a kind of preparation method of height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride.
Summary of the invention
Object of the present invention height crystal orientation coupling stacked structure aiming to provide a kind of Graphene/hexagonal boron nitride and preparation method thereof, stacked structure coupling prepared by the method is within 1 °, tolerance range is high, and the Graphene of arbitrary orientation can be mated with hexagonal boron nitride crystal orientation
According to an aspect of the present invention, provide a kind of preparation method of height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride, comprising: the preliminary stacked structure forming Graphene/hexagonal boron nitride; Preliminary stacked structure is heat-treated, to obtain the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride.
Further, before the heat treatment, the manipulation technology based on scan-probe is adopted to operate the Graphene in preliminary stacked structure, to make preliminary stacked structure pre-matching.
Further, thermal treatment comprises heating operation, and the Heating temperature of heating operation is 600 DEG C ~ 800 DEG C, and soaking time is 10 ~ 40 minutes.
Further, thermal treatment is for carry out high temperature annealing to preliminary stacked structure, and temperature rise rate during high temperature annealing and rate of temperature fall are 5 ~ 15 DEG C/min; Be preferably 10 DEG C/min.
Further, the step forming the preliminary stacked structure of Graphene/hexagonal boron nitride comprises: on hexagonal boron nitride crystal, form graphene layer, and introduce defect on graphene layer; Expand defect to obtain mutually discrete Graphene block, thus obtain multiple preliminary stacked structure.
Further, electron beam lithography and reactive ion oxygen lithographic technique is adopted to introduce defect on graphene layer.
Further, the rounded hole of defect, circular opening is of a size of 50 ~ 800nm.
Further, adopt hydrogen plasma anisotropic etching to expand the defect on graphene layer.
Further, the condition of hydrogen plasma anisotropic etching is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.
According to a further aspect in the invention, Graphene/this stacked structure of hexagonal boron nitride stacked structure providing a kind of height crystal orientation coupling is prepared from by any one preparation method above-mentioned.
The present inventor finds, when thermal treatment, Graphene can rotate on hexagonal boron nitride crystal, the crystal orientation that this rotation is conducive to both is mated, and inventors herein proposes a kind of method preparing the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride based on this phenomenon.Namely the method heat-treats preliminary Graphene/hexagonal boron nitride stacked structure, by this operation, Graphene is mated with hexagonal boron nitride crystal orientation, obtains the Graphene/boron nitride stacked structure with highly perfect crystal orientation coupling.
Employing present method avoids the difficulties such as the existing uncertainty of mechanical registeration mode of the prior art, and the crystal orientation, border of this preparation method and Graphene and hexagonal boron nitride has nothing to do, even if the Graphene on random border and hexagonal boron nitride also can carry out perfect matched, namely can by the Graphene of arbitrary orientation and hexagonal boron nitride crystal orientation matched.In addition, processing of the present invention, manipulation technology are more ripe, anneal convenient and easy, there is universality, be not only applicable to the stacked structure of Graphene/hexagonal boron nitride, can also extend in the lamination layer structure being applied to other similar matched of preparation, as Graphene/graphite system.
According to hereafter by reference to the accompanying drawings to the detailed description of the specific embodiment of the invention, those skilled in the art will understand above-mentioned and other objects, advantage and feature of the present invention more.
Accompanying drawing explanation
Hereinafter describe specific embodiments more of the present invention with reference to the accompanying drawings by way of example, and not by way of limitation in detail.Reference numeral identical in accompanying drawing denotes same or similar parts or part.It should be appreciated by those skilled in the art that these accompanying drawings may not be drawn in proportion.In accompanying drawing:
Graphene is transferred to according to an embodiment of the present invention the structural representation that hexagonal boron nitride obtains by Fig. 1;
Fig. 2 is the structural representation according to introducing artifacts after the employing beamwriter lithography of an embodiment of the present invention and reactive ion oxygen etching on Graphene;
Fig. 3 is the preliminary stacked structure schematic diagram with the Graphene/hexagonal boron nitride of discrete Graphene according to obtaining after adopting hydrogen plasma anisotropic etching in an embodiment of the present invention;
Fig. 4 is the atomic force microscope figure of Fig. 3;
Fig. 5 to Fig. 7 is according to the process schematic preparing the height crystal orientation coupling stacked structure of Graphene/boron nitride of a kind of exemplary embodiments of the present invention; Wherein, Fig. 5 to Fig. 6 is the manipulation process schematic diagram of scan-probe, and arrow in Fig. 5 display Graphene carries out the position handled and direction; Fig. 6 to Fig. 7 illustrates the procedure chart that rotation that high temperature annealing causes makes Graphene mate further with hexagonal boron nitride crystal orientation; And
Fig. 8 is the atomic force microscope figure of the matched stacked structure of the Graphene/hexagonal boron nitride obtained after high temperature annealing in Fig. 7.
Embodiment
In order to the stacked structure crystal orientation matching degree solving Graphene/hexagonal boron nitride that preparation method of the prior art obtains is not high, or the problem of stacked structure existing defects, the invention provides a kind of preparation method of height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride.This preparation method comprises: the preliminary stacked structure forming Graphene/hexagonal boron nitride; Preliminary stacked structure is heat-treated, to obtain the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride.
When thermal treatment, Graphene can rotate on hexagonal boron nitride crystal, the crystal orientation that this rotation is conducive to both is mated, a kind of method preparing the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride is inventors herein proposed based on this phenomenon, namely preliminary Graphene/hexagonal boron nitride stacked structure is heat-treated, by this operation, Graphene is mated with hexagonal boron nitride crystal orientation, obtain the Graphene/boron nitride stacked structure with highly perfect crystal orientation coupling.
In one embodiment of the invention, the step forming the preliminary stacked structure of Graphene/hexagonal boron nitride comprises: on hexagonal boron nitride crystal, form graphene layer, and introduce defect on graphene layer; Expand defect to obtain mutually discrete Graphene block, thus obtain multiple preliminary stacked structure.Generally first substrate is set, as silica/silicon substrate, hexagonal boron nitride crystal is arranged on substrate, Graphene is transferred on hexagonal boron nitride crystal.Specifically referring to Fig. 1 to Fig. 4, is the procedure chart that discrete Graphene forms the preliminary stacked structure of Graphene/hexagonal boron nitride on hexagonal boron nitride in Fig. 1 to Fig. 4.
Particularly, first adopt plant and instrument as scotch tape by hexagonal boron nitride crystal mechanically peel on nano level silica/silicon substrate, afterwards by Graphene mechanical transfer on hexagonal boron nitride crystal, obtain structure as shown in Figure 1.What obtain after transfer is Graphene/hexagonal boron nitride stacked structure that crystal orientation matching degree is lower.In order to remove the impurity of some absorption physical property, first this structure is annealed 10 hours as 340 DEG C.
Similar with the situation that graphite layers is stacking, when stacked structure more mates close to crystal orientation, the thermostability of this stacked structure is better.Therefore, need the Graphene to low crystal orientation matching degree/hexagonal boron nitride stacked structure to heat-treat, in heat treatment process, make Graphene and hexagonal boron nitride crystal orientation that height crystal orientation occurs mate.Thus the present invention creatively have employed heat treated mode and makes Graphene/hexagonal boron nitride stacked structure reach height crystal orientation coupling, and then obtains the perfect Graphene/boron nitride stacked structure of crystal orientation coupling within 1 °.The crystal orientation, border of the method and Graphene and hexagonal boron nitride has nothing to do, namely can by the Graphene of arbitrary orientation and hexagonal boron nitride crystal orientation matched, and simple to operate, and temperature is easy to control.
When preparing the preliminary stacked structure of Graphene/hexagonal boron nitride, consider size and performance issue, need to carry out discrete to whole preliminary stacked structure, namely on hexagonal boron nitride, form multiple discrete Graphene block, form the preliminary stacked structure of multiple discrete Graphene/hexagonal boron nitride.
In a preferred embodiment of the invention, electron beam lithography and reactive ion oxygen lithographic technique is adopted to introduce defect on graphene layer.Graphene after Fig. 2 shows beamwriter lithography and reactive ion oxygen etching has the structure iron of artifacts.As can be seen from Figure 2, the rounded hole of defect, circular opening is of a size of tens to hundreds of nanometer.
After Graphene forms defect, in order to obtain discrete Graphene block, the present invention adopts the mode expanding defect area to reach the fracture of graphene layer.In a specific embodiment, adopt hydrogen plasma anisotropic etching to expand the defect on graphene layer.Particularly, the condition of hydrogen plasma anisotropic etching is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.Fig. 3 is that after adopting hydrogen plasma anisotropic etching, remaining part presents discrete Graphene block, is of a size of hundreds of nanometer to several microns.Fig. 4 be discrete in Fig. 3 after the atomic force microscope figure of Graphene block.
As can be seen from Fig. 3 and Fig. 4, the Graphene block after discrete is irregular diamond shaped, and the limit of these Graphene blocks is generally zig-zag (zigzag) structure.Visible, adopt hydrogen plasma anisotropic etching not only can obtain the Graphene block with neat border, and can be used for processing other the various graphene nano-patterns obtaining atomically flating zig-zag borderline structure, this is for research Graphene size confinement effect, marginality and construct various device to comprise single electron quantum dot device, field effect transistor device etc. be all a kind of effective means.
The discrete Graphene block obtained after above-mentioned processing does not mate with the crystal orientation between hexagonal boron nitride, and this have impact on the performance of Graphene each side, as thermostability etc.In order to obtain the Graphene/hexagonal boron nitride stacked structure of height crystal orientation coupling, the present invention adopts heat treatment mode and then impels Graphene to rotate to reach and hexagonal boron nitride crystal orientation matched.Fig. 5 to Fig. 7 is the procedure chart of the Graphene/boron nitride stacked structure of preparation height crystal orientation coupling.
In order to obtain having the Graphene/hexagonal boron nitride stacked structure of Perfect Matchings degree more, when mating according to stacked structure crystal orientation, interface friction is maximum, in a preferred embodiment of the invention, before step is heat-treated to Graphene block, the manipulation technology based on scan-probe is adopted to operate the Graphene in preliminary stacked structure, to make the preliminary stacked structure pre-matching of Graphene/hexagonal boron nitride.Wherein, Fig. 5 to Fig. 6 is the manipulation process schematic diagram of scan-probe, and the position that the display of arrow in Fig. 5 is handled Graphene and direction, make Graphene rotate by handling scan-probe, thus makes that its crystal orientation is close mates with hexagonal boron nitride crystal orientation.
The manipulation technology based on scan-probe is adopted to operate Graphene block, roughly as follows: mainly by nanolithographic (nanolithography) functional realiey of atomic force microscope, the silicon needle point (elastic constant: 20 ~ 80N/m, needle point radius-of-curvature: ~ 20nm) that employing standard p adulterates handles sample.By the script able to programme of gated sweep probe, needle point is set at the height of material surface and tangential movement route.Based on the operation of scan-probe by needle point and sample contacts with promotes to realize, the rotation of the different directions of manipulation object can be realized by the active position of change needle point and direction.When Graphene block rotates under the promotion of needle point, when close coupling, frictional force is significantly greater than the situation away from coupling, and therefore, when it rotates, Graphene finally can be parked in the crystal orientation closest to mating with boron nitride.
In a preferred embodiment of the invention, thermal treatment comprises heating operation, and the Heating temperature of heating operation is 600 DEG C ~ 800 DEG C, and soaking time is 10 ~ 40 minutes.In this temperature range, heating contributes to the Graphene/hexagonal boron nitride stacked structure of higher crystal orientation coupling.Otherwise, if thermal treatment temp is higher than 800 DEG C, then Graphene/boron nitride stacked structure can be caused to occur Texturized, affect interface friction and the thermostability of this stacked structure, be unfavorable for the stability of follow-up prepared device.If thermal treatment temp is lower than 600 DEG C, then can reduce crystal orientation matching degree.
In a preferred embodiment of the invention, in step s3, high temperature annealing is adopted to heat-treat Graphene in preliminary stacked structure.Fig. 6 to Fig. 7 shows the procedure chart that rotation that high temperature annealing causes makes Graphene mate further with hexagonal boron nitride crystal orientation; Fig. 8 is the atomic force microscope figure of the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride in Fig. 7.As can be seen from the clear Moire fringe in Fig. 8, the relative angle of Graphene/hexagonal boron nitride controls within 1 °, illustrates that this stacked structure height crystal orientation is mated.Temperature rise rate during high temperature annealing and rate of temperature fall are 5 ~ 15 DEG C/min.Preferred temperature rise rate and rate of temperature fall are 10 DEG C/min.
High temperature annealing refers to and metal is slowly heated to certain temperature, keeps enough time, then with a kind of metal heating processing technology of Reasonable Speed cooling (normally Slow cooling is controlled cooling model sometimes).The present invention preferably adopts high temperature annealing, mainly considers that this processing mode can obtain the stacked structure of higher crystal orientation coupling.
According to a further aspect in the invention, provide the Graphene/hexagonal boron nitride lamination layer structure of a kind of height crystal orientation coupling, this lamination layer structure is prepared from by any one preparation method above-mentioned.The height crystal orientation coupling stacked structure of the Graphene/boron nitride adopting method of the present invention to prepare, not only can provide controlled building method for research superstructure, and in electricity, optics, tribology, all show many special performances, as stacked structure thermostability is very high, be conducive to all kinds of devices that processability is stable.
Beneficial effect of the present invention is further illustrated below in conjunction with embodiment:
Embodiment 1
1) get the hexagonal boron nitride crystal that thickness is 20nm, by its mechanically peel to thickness be 300nm silica/silicon substrate on.Then use the method for mechanical transfer to be transferred on hexagonal boron nitride by the single-layer graphene being of a size of 5 μm, form stepped construction as shown in Figure 1.
2) adopt electron beam lithography and reactive ion oxygen lithographic technique on graphene layer, prepare the circular opening that diameter is 300nm, as shown in Figure 2.Adopt hydrogen plasma etching enlarged rounded hole defect, thus obtain the preliminary stacked structure with the Graphene/hexagonal boron nitride of isolated Graphene fritter, as shown in Figure 3.Reaction conditions is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.
3) manipulation technology based on scan-probe is adopted to operate the Graphene in preliminary stacked structure, to make the preliminary stacked structure pre-matching of Graphene/hexagonal boron nitride, as shown in Figure 5 to Figure 6.When Graphene block rotates under the promotion of needle point, when frictional force significantly becomes large, Graphene finally can be parked in the crystal orientation closest to mating with boron nitride.
4) by step 3) in stacked structure after pre-matching carry out the high temperature anneal, be warming up to 700 DEG C with 10 DEG C/min, be incubated 30 minutes, be then reduced to room temperature with 10 DEG C/min.Microscope photograph after the high temperature anneal as shown in Figure 7.
Embodiment 2
1) get the hexagonal boron nitride crystal that thickness is 20nm, by its mechanically peel to thickness be 300nm silica/silicon substrate on.Then use the method for mechanical transfer to be transferred on hexagonal boron nitride by the single-layer graphene being of a size of 5 μm, form stepped construction as shown in Figure 1.
2) adopt electron beam lithography and reactive ion oxygen lithographic technique on graphene layer, prepare the circular opening that diameter is 100nm, as shown in Figure 2.Adopt hydrogen plasma etching enlarged rounded hole defect, thus obtain the preliminary stacked structure with the Graphene/hexagonal boron nitride of isolated Graphene fritter, as shown in Figure 3.Reaction conditions is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.
3) manipulation technology based on scan-probe is adopted to operate the Graphene in preliminary stacked structure, to make the preliminary stacked structure pre-matching of Graphene/hexagonal boron nitride, as shown in Figure 5 to Figure 6.When Graphene block rotates under the promotion of needle point, when frictional force significantly becomes large, Graphene finally can be parked in the crystal orientation closest to mating with boron nitride.
4) by step 3) in stacked structure after pre-matching carry out the high temperature anneal, be warming up to 600 DEG C with 5 DEG C/min, 10 minutes, be then reduced to room temperature with 5 DEG C/min.
Embodiment 3
1) get the hexagonal boron nitride crystal that thickness is 20nm, by its mechanically peel to thickness be 300nm silica/silicon substrate on.Then use the method for mechanical transfer to be transferred on hexagonal boron nitride by the single-layer graphene being of a size of 5 μm, form stepped construction as shown in Figure 1.
2) adopt electron beam lithography and reactive ion oxygen lithographic technique on graphene layer, prepare the circular opening that diameter is 700nm, as shown in Figure 2.Adopt hydrogen plasma etching enlarged rounded hole defect, thus obtain the preliminary stacked structure with the Graphene/hexagonal boron nitride of isolated Graphene fritter, as shown in Figure 3.Reaction conditions is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.
3) manipulation technology based on scan-probe is adopted to operate the Graphene in preliminary stacked structure, to make the preliminary stacked structure pre-matching of Graphene/hexagonal boron nitride, as shown in Figure 5 to Figure 6.When Graphene block rotates under the promotion of needle point, when frictional force significantly becomes large, Graphene finally can be parked in the crystal orientation closest to mating with boron nitride.
4) by step 3) in stacked structure after pre-matching carry out the high temperature anneal, be warming up to 800 DEG C with 15 DEG C/min, be incubated 40 minutes, be then reduced to room temperature with 15 DEG C/min.
Embodiment 4
Its operation steps is all identical with embodiment 1, when difference is high temperature annealing intensification different with cooling mechanism, be warming up to 900 DEG C with 20 DEG C/min in embodiment 4, be incubated 5 minutes, be then reduced to room temperature with 20 DEG C/min.
Embodiment 5
Its operation steps is all identical with embodiment 1, and difference is not adopt step 3), namely based on the manipulation technology of scan-probe, the Graphene in preliminary stacked structure is not operated.
Calculate the coupling angle of the stacked structure of the Graphene/hexagonal boron nitride prepared in embodiment 1 to 5.Calculation formula is as follows:
Wherein, a is the wavelength that the lattice parameter 0.246nm of Graphene, δ get that 1.8%, λ is Morie fringe, and atomic force microscope can be adopted to measure its numerical value; Φ represents the angle between Graphene and boron nitride crystal orientation, and Φ numerical value, more close to 0 °, illustrates that matching degree is higher.Concrete numerical value refers to table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| λ | 14nm | 13nm | 12nm | 10nm | 7nm |
| Φ | 0° | 0.5° | 1° | 1.5° | 2° |
As can be seen from Table 1, the Φ value of the Graphene adopting heat treating method of the present invention to prepare/hexagonal boron nitride stacked structure is all lower, illustrates that the stacked structure adopting method of the present invention to prepare has higher crystal orientation matching degree, especially in embodiment 1 to 3.
So far, those skilled in the art will recognize that, although multiple exemplary embodiment of the present invention is illustrate and described herein detailed, but, without departing from the spirit and scope of the present invention, still can directly determine or derive other modification many or amendment of meeting the principle of the invention according to content disclosed by the invention.Therefore, scope of the present invention should be understood and regard as and cover all these other modification or amendments.
Claims (10)
1. a preparation method for the height crystal orientation coupling stacked structure of Graphene/hexagonal boron nitride, comprising:
Form the preliminary stacked structure of Graphene/hexagonal boron nitride;
Described preliminary stacked structure is heat-treated, to obtain the height crystal orientation coupling stacked structure of described Graphene/hexagonal boron nitride.
2. preparation method according to claim 1, is characterized in that, before described thermal treatment, adopts the manipulation technology based on scan-probe to operate the Graphene in described preliminary stacked structure, to make described preliminary stacked structure pre-matching.
3. preparation method according to claim 1 and 2, is characterized in that, described thermal treatment comprises heating operation, and the Heating temperature of described heating operation is 600 DEG C ~ 800 DEG C, and soaking time is 10 ~ 40 minutes.
4. preparation method according to any one of claim 1 to 3, is characterized in that, described thermal treatment is for carry out high temperature annealing to described preliminary stacked structure, and temperature rise rate during described high temperature annealing and rate of temperature fall are 5 ~ 15 DEG C/min; Be preferably 10 DEG C/min.
5. preparation method according to claim 1, is characterized in that, the step forming the preliminary stacked structure of described Graphene/hexagonal boron nitride comprises:
Hexagonal boron nitride crystal forms graphene layer, and introduce defect on described graphene layer;
Expand described defect to obtain mutually discrete Graphene block, thus obtain multiple described preliminary stacked structure.
6. preparation method according to claim 5, is characterized in that, adopts electron beam lithography and reactive ion oxygen lithographic technique to introduce defect on described graphene layer.
7. the preparation method according to any one of claim 5 to 6, is characterized in that, the rounded hole of described defect, described circular opening is of a size of 50 ~ 800nm.
8. according to the preparation method according to any one of claim 5 to 7, it is characterized in that, adopt hydrogen plasma anisotropic etching to expand the defect on described graphene layer.
9. preparation method according to claim 8, is characterized in that, the condition of described hydrogen plasma anisotropic etching is: temperature is 400 DEG C, and hydrogen pressure is 0.4torr, and power is 10W, and etch rate is 3nm/ minute.
10. Graphene/hexagonal boron nitride stacked structure of height crystal orientation coupling, it is characterized in that, described stacked structure is the preparation method according to any one of claim 1 to 9 be prepared from.
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| CN112919454A (en) * | 2021-01-29 | 2021-06-08 | 南京大学 | Method for controlling stacking angle of double-layer graphene |
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| CN103502507A (en) * | 2011-05-03 | 2014-01-08 | 韩国科学技术院 | Method for manufacturing high quality graphene using continuous heat treatment chemical vapor deposition method |
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| CN103502507A (en) * | 2011-05-03 | 2014-01-08 | 韩国科学技术院 | Method for manufacturing high quality graphene using continuous heat treatment chemical vapor deposition method |
| CN102392225A (en) * | 2011-07-22 | 2012-03-28 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene nanoribbon on insulating substrate |
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| CN110828550A (en) * | 2019-10-21 | 2020-02-21 | 浙江大学 | Boron nitride/graphene heterojunction device |
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