CN109841549B - Method for lossless transfer of self-supporting low-dimensional material - Google Patents
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Abstract
The invention relates to the technical research field of low-dimensional functional material science and material testing analysis, in particular to a method for accurately positioning, cutting and nondestructively transferring a self-supporting low-dimensional material aiming at foils, films, two-dimensional materials and the like. Most self-supporting low-dimensional materials needing to be transferred have the thickness ranging from a few nanometers to hundreds of micrometers, the in-plane size ranging from millimeters to micrometers, are extremely easy to damage in the sampling processing process and the transferring process, have extremely low specific gravity, are easily influenced by external environments (such as airflow, static electricity and the like) greatly and are difficult to accurately control and position. The method introduces the technical means of femtosecond laser cutting, microgravity, electrostatic introduction, microscopic positioning and the like, can effectively solve the problems, particularly aims at transferring the material to a tiny easily damaged device, can be perfectly applied, and greatly expands the research and application of the self-supporting low-dimensional functional material.
Description
Technical Field
The invention relates to the technical research field of low-dimensional functional material science and material testing analysis, in particular to a method for accurately positioning, cutting and nondestructively transferring a self-supporting low-dimensional material aiming at foils, films, two-dimensional materials and the like. Particularly, when the target vector is transferred to a fragile tiny target vector, the unique advantages can be fully realized.
Background
Commonly used low dimensional materials such as: the low-dimensional material has rapid development in recent years due to unique spatial structure, electrical property and thermal property, and has wide application prospect in the fields of microelectronics, biological detection and batteries. When the self-supporting low-dimensional material is transferred to a tiny vulnerable chip for testing and researching the intrinsic electrical and thermal properties of the material, a method of firstly transferring and then carrying out electron beam exposure, electrode deposition, RIE etching and wet etching or focused ion beam etching is usually adopted. However, the method has the disadvantages of expensive instruments, complicated steps, fragile and easily damaged electrode chip carriers of only a few hundred nanometers, strong specialty requirement, easy damage of some samples in the etching process due to the fact that the carriers are transferred first and then etched, no universality, limited electrode patterns and shapes and not too complex, and obvious defects in performance exploration. Therefore, it is important to invent a method of first manufacturing a chip and then performing a lossless transfer.
Disclosure of Invention
The invention aims to provide a method for transferring a self-supporting low-dimensional material onto a carrier in a nondestructive manner, which can accurately position, cut and transfer materials with the size from centimeter to submicron in a nondestructive manner, avoids expensive and time-consuming methods such as focused ion beam etching and the like, and has the characteristics of simplicity, effectiveness, easiness in popularization and the like.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method of non-destructive transfer of a self-supporting low dimensional material, the method comprising the steps of:
(1) transferring the low-dimensional material deposited on the substrate to the hollowed-out rigid support sheet by using Van der Waals force;
(2) cutting and processing the low-dimensional material into a required shape by using a femtosecond laser fine processing device;
(3) transferring the cut material to the upper part of the carrier by using a microscopic positioning device;
(4) the sample was cut with a laser to detach it from the rigid support sheet.
The method for lossless transfer of the self-supporting low-dimensional material comprises the steps that the substrate is Si or SiO2Or a polyimide.
The method for nondestructively transferring the self-supporting low-dimensional material adopts the rigid supporting sheet for supporting, has enough mechanical property, is not easy to deform in the transferring process, and the size of the rigid supporting sheet depends on the size of the low-dimensional material and the size of a target carrier to be transferred and is larger than the overall size of the carrier.
The method for nondestructively transferring the self-supporting low-dimensional material utilizes a femtosecond laser fine processing device to cut the low-dimensional material in a centimeter to submicron scale, and the device comprises: the device comprises a laser convergence and microscopic observation system, a laser light source, a common light source, an air pump, an air floatation damping platform, a sample stage mechanical numerical control moving system, a CCD camera, a laser convergence module mechanical moving system, a motion controller and a computer, and has the following specific structure:
the laser light source and the ordinary light source are respectively connected to the laser convergence and microscopic observation system in a coaxial light mode through interfaces through optical cables, and the laser light source and the ordinary light source manually select and switch the light sources; the laser convergence and microscopic observation system is connected with the input end of the CCD camera, and the output end of the CCD camera and the input end of the motion controller are connected with the computer through a USB line to carry out microscopic observation positioning and numerical control programming; the laser gathering and microscopic observation system is arranged on the laser gathering module mechanical moving system, the output end of the motion controller is connected with the sample table mechanical numerical control moving system, the sample table mechanical numerical control moving system is arranged on the air floatation damping platform, and the air inlet end of the air floatation damping platform is connected with the air pump.
The method for nondestructively transferring the self-supporting low-dimensional material comprises the following steps in the process of microscopic positioning transfer:
(1) transferring the rigid supporting sheet to the upper part of the carrier by adopting a method of combining vacuum adsorption or magnetic adsorption with a sliding table;
(2) introducing non-contact external microgravity to the material or applying directional electrostatic force between the sample and the target carrier;
(3) and (5) microscopically observing the combination condition of the two-dimensional material and the target carrier.
The method for nondestructively transferring the self-supporting low-dimensional material comprises the steps of separating the low-dimensional material from the rigid supporting sheet by laser cutting, and then removing the rigid supporting sheet by adopting a method of combining vacuum adsorption or magnetic adsorption with a sliding table after the material is ensured to be successfully attached to a carrier, so as to prevent the transferred sample from being displaced due to electrostatic force when the rigid supporting sheet is removed.
In the method for transferring the self-supporting low-dimensional material without damage, a vacuum suction nozzle with a customized caliber is adopted for vacuum adsorption in the process of micro-positioning transfer, and a rigid supporting sheet is sucked up; the magnetic adsorption adopts a tiny electromagnet, the rigid support sheet adopted at the moment is made of a magnetic material, and the magnetic property of the electromagnet suction head is manually controlled, so that the rigid support sheet is stably transferred in the transfer process and cannot be vibrated and dislocated in the moving process.
In the method for the lossless transfer of the self-supporting low-dimensional material, the introduction of microgravity during the microscopic positioning transfer process considers that the influence on the property structure of the material is avoided and the material is easy to remove; the method of using electrostatic force considers that the surface of the carrier is insulated, the electrostatic force can not be conducted away quickly, and the electrostatic force is transferred as soon as possible after the carrier is introduced, so that the electrostatic force is prevented from dissipating.
In the method for transferring the self-supporting low-dimensional material without damage, the resolution ratio of a microscope is less than 5 mu m in the microscopic positioning transfer process, a sliding table comprises translation in three directions of X-Y-Z and rotation in the plane, and the repeated positioning precision is less than 1 mu m.
The design idea of the invention is as follows:
firstly, the method aims at the problems in the process of firstly transferring and then manufacturing a chip in the current international research method for the electrical, thermal, magnetic and other properties of the low-dimensional material. The present invention seeks to create a low dimensional material transfer method that can be adapted to already prepared target carriers. The invention adopts a method of converging laser processing to replace mechanical cutting, adopts hollow rigid support sheet transfer, and introduces microgravity and electrostatic force to the material, so that the material can vertically fall in a small range, or introduces electrostatic force to the carrier to directionally attract a sample, so as to realize that the sample and the carrier are attached together under the condition that the sample and the carrier are not subjected to macroscopic force, and can realize accurate cutting, positioning and nondestructive transfer of the self-supporting low-dimensional material by combining accurate positioning.
Based on the main design and guidance ideas, the invention successfully realizes the transfer of the self-supporting low-dimensional material to a vulnerable carrier, ensures that the material and the carrier are intact, and can accurately transfer the material at a fixed point.
The invention has the following advantages and beneficial effects:
1. the transfer method is suitable for most self-supporting low-dimensional materials and has good universality.
2. The transfer method can transfer the sample with the smallest size which can reach the submicron level. The material transfer device can be accurately positioned and transferred, and the small-size accurate positioning transfer is beneficial to reducing the influence of irrelevant environments in the material research process and improving the research reliability.
3. According to the transfer method, the material is cut by the femtosecond laser cutting method, so that the damage of the shearing force of mechanical cutting to the edge of the material can be avoided, the material is not modified in the transfer process, the accuracy of the material performance research is ensured, and the precision which cannot be achieved by mechanical cutting can be achieved by using converged laser.
4. The transfer method has great advantages when the carrier to be transferred is a damaged material, and the method can ensure that the material and the carrier are not influenced by macroscopic force and are not damaged in the process of transferring the material.
5. The transfer method provided by the invention provides two introduction forms of micro-gravity and electrostatic force micro-external field force aiming at the properties of different materials, and has wider applicability.
Drawings
FIG. 1 is a flow chart of the method of the present invention; in the figure, 1-self-supporting two-dimensional material, 2-rigid supporting thin sheet, 3-converging laser, 4-target carrier to be transferred, 5-vacuum suction nozzle or magnetic suction head, 6-non-contact micro gravity or electrostatic force is introduced.
FIG. 2 is a schematic diagram of the transfer of a carbon nanotube free-standing film to suspended Si by the method of the present invention3N4Optical photograph of the electrode chip.
FIG. 3 is a schematic diagram of an experimental apparatus according to the present invention. In the figure, 7 laser convergence and microscopic observation systems; 8, a laser light source; 9 a source of ordinary light; 10 air pump; 11, an air floatation damping platform; 12, a mechanical numerical control moving system of the sample stage; 13CCD camera; 14 laser convergence module mechanical moving system; 15 a motion controller; 16 computers.
Detailed Description
In the specific implementation process, a method for transferring the self-supporting low-dimensional material to the carrier in a nondestructive mode is provided, mainly aiming at an application scene of transferring to a vulnerable carrier, the micro self-supporting low-dimensional material is transferred by introducing two micro external forces of non-contact microgravity or electrostatic force instead of applying a macro contact external force, so that the damage of the low-dimensional material and a target carrier can be effectively avoided, and meanwhile, the accurate positioning nondestructive transfer is realized by combining the mode of converging femtosecond laser cutting and microscopic positioning.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Referring to fig. 1, the flow of the method for lossless transfer of self-supporting low-dimensional material of the invention is as follows:
(S1) firstly, transferring the self-supporting two-dimensional material 1 onto a rigid supporting sheet 2, and then carrying out numerical control cutting processing on the self-supporting two-dimensional material into a required geometric shape by using a converging laser 3 processing device;
(S2), the rigid support sheet 2 is turned over to make the self-supporting two-dimensional material 1 under the rigid support sheet 2, the rigid support sheet 2 is sucked up by the vacuum suction nozzle or the magnetic suction head 5, the target carrier 4 to be transferred is placed under the rigid support sheet 2, the relative position of the sample and the carrier is observed under the optical microscope, the target carrier 4 to be transferred is positioned right under the sample by operating the sliding table, and at this time, the vacuum suction nozzle or the magnetic suction head 5 is lowered to make the rigid support sheet 2 fall on the carrier frame.
(S3) non-contact type minute gravity or electrostatic force introduction 6: if the method of micro gravity is adopted, then the liquid which is relatively volatile and does not react with the sample carrier, such as alcohol or ultrapure water, can be sprayed into the environment where the sample is located, so that the liquid falls on the sample. If an electrostatic method is used, the carrier surface is required to be insulated and the environment is dry, and before transfer, bias voltage is applied to the surface of the target carrier to inject electrons, so that charges are accumulated on the surface of the target carrier, and then transfer is performed.
(S4) the joint between the sample and the rigid support sheet 2 is cut off rapidly by the focused laser beam 3, and the rigid support sheet 2 is lifted vertically by the vacuum suction nozzle or the magnetic suction head 5, taking care not to take the sample up.
Most self-supporting low-dimensional materials needing to be transferred have the thickness ranging from a few nanometers to hundreds of micrometers, the in-plane size ranging from millimeters to micrometers, are extremely easy to damage in the sampling processing process and the transferring process, have extremely low specific gravity, are easily influenced by external environments (such as airflow, static electricity and the like) greatly and are difficult to accurately control and position. The method introduces the technical means of femtosecond laser cutting, microgravity, electrostatic introduction, microscopic positioning and the like, can effectively solve the problems, particularly aims at transferring the material to a tiny easily damaged device, can be perfectly applied, and greatly expands the research and application of the self-supporting low-dimensional functional material.
The invention is further explained or illustrated by the following examples.
Example 1
In this embodiment, the device for measuring the thermal conductivity of the self-supporting Carbon Nanotube (CNTs) film is a suspended Si film reported in the literature3N4The thickness of the electrode chip is approximately within 500nm, and the electrode chip cannot be subjected to macroscopic force and is easy to break.
The transfer method comprises the following steps: the self-supporting CNTs film is transferred to a Mo ring with the thickness of 100 microns, the outer diameter of 5mm and the inner diameter of 1.2mm, and the detailed steps of the material processing method are carried out, so that the strip-shaped CNTs film can be transferred to two suspended Si rings3N4Between the electrode chips, as shown in FIG. 2.
Referring to fig. 3, an embodiment of the present invention provides an apparatus for fine processing using femtosecond laser, which mainly includes the following systems: the device comprises a laser convergence and microscopic observation system, a sample stage mechanical numerical control moving system, a microscopic observation positioning system, a computer centralized data monitoring and visualization system, a damping system and the like.
The laser light source 8 and the ordinary light source 9 are respectively connected to the laser convergence and microscopic observation system 7 through an optical cable in a coaxial light mode through a customized interface, and the laser light source 8 and the ordinary light source 9 can be manually selected to switch light sources. The laser convergence and microscopic observation system 7 is connected with the input end of the CCD camera 13, and the output end of the CCD camera 13 and the input end of the motion controller 15 are connected with the computer 16 through USB lines for microscopic observation positioning and numerical control programming. The laser convergence and microscopic observation system 7 is provided with the long-focus objective lenses with different multiples, so that observation and selection can be conveniently carried out according to different samples and processing requirements. The laser convergence and microscopic observation system 7 is arranged on a laser convergence module mechanical moving system 14, the output end of the motion controller 15 is connected with a sample stage mechanical numerical control moving system 12, the sample stage mechanical numerical control moving system 12 is arranged on an air floatation damping platform 11, and the air inlet end of the air floatation damping platform 11 is connected with an air pump 10. The motion controller of the device is used for storing and converting program commands of the computer and sending the program commands to the motor driver; the motor driver of the device is used for transmitting pulse electric signals to the stepping motor of the electric sample stage.
The laser converging and microscopic observation system of the device is provided with a coaxial optical path system, wherein the coaxial optical path system comprises a laser optical cable interface, a common optical cable interface, a laser CCD camera, a group of laser converging lenses, a common microscope eyepiece, an objective lens and a group of ultralong focal length objective lenses with different multiplying powers, and laser is converged so as to meet the requirements of processing and processing precision. The laser convergence module mechanical moving system 14 drives the laser convergence and microscopic observation system 7 to move randomly in an x, y and z three-dimensional space for focusing of a microscope and movement of light spots; the mechanical numerical control moving system 12 of the sample stage drives the sample stage to move randomly in x, y and z three-dimensional spaces, the repeated positioning precision can reach 0.1 mu m, the mechanical numerical control moving system 12 of the sample stage realizes the rotation and the tilting of the sample in the plane, and the numerical control and the real-time state monitoring of the sample are realized. The laser convergence and microscopic observation system is provided with a microscopic imaging system with adjustable magnification and a coaxial light source and is used for positioning laser spots and observing, processing and treating samples, the observation resolution can reach 0.5 mu m, the cutting resolution can reach 4 mu m, and the laser spots can reach 4 mu m. And the numerical control and real-time monitoring of the mechanical displacement are realized through computer control software, the repeated positioning precision is 0.5 mu m, and the moving speed is 1 mm/min-1000 mm/min and can be continuously adjusted.
The example results show that it is possible to transfer a self-supporting low-dimensional material of a specific shape and size onto a target carrier quickly, accurately and without damage using the method of the invention. The integrity of the material and the carrier is guaranteed. Has unique application advantages for special vulnerable carriers. The method is beneficial to promoting the development of the field of low-dimensional material performance research, reduces the research threshold, can carry out performance test research on the low-dimensional material without a plurality of image exposure machines, RIE etching machines, electrode coating machines, PECVD equipment, focused ion beam equipment and the like by only customizing a carrier and then transferring, and has certain commercial value, market and possibility.
The device and the method for preparing the in-situ electron microscope sample by using the converged femtosecond laser are described in detail above. The principles and embodiments of the present invention are described herein using specific examples, which are presented only to assist in understanding the method and core concepts of the present invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A method for the non-destructive transfer of a self-supporting low dimensional material, the method comprising the steps of:
(1) transferring the low-dimensional material deposited on the substrate to the hollowed-out rigid support sheet by using Van der Waals force;
(2) cutting and processing the low-dimensional material into a required shape by using a femtosecond laser fine processing device;
(3) transferring the cut material to the upper part of the carrier by using a microscopic positioning device;
(4) cutting the sample by laser to separate the sample from the rigid support sheet;
wherein the low-dimensional material is foil, functional film or two-dimensional material.
2. The method for the lossless transfer of self-supporting low-dimensional material as claimed in claim 1, wherein the substrate is Si, SiO2Or a polyimide.
3. The method for the non-destructive transfer of self-supporting low-dimensional materials according to claim 1, wherein a rigid support sheet is used for supporting, having sufficient mechanical properties to be not easily deformed during the transfer, and having a size larger than the external dimensions of the carrier, depending on the size of the low-dimensional material and the size of the target carrier to be transferred.
4. The method for the nondestructive transfer of the self-supporting low dimensional material according to claim 1, wherein the low dimensional material is trimmed in a centimeter to submicron scale using a femtosecond laser fine processing apparatus comprising: the device comprises a laser convergence and microscopic observation system, a laser light source, a common light source, an air pump, an air floatation damping platform, a sample stage mechanical numerical control moving system, a CCD camera, a laser convergence module mechanical moving system, a motion controller and a computer, and has the following specific structure:
the laser light source and the ordinary light source are respectively connected to the laser convergence and microscopic observation system in a coaxial light mode through interfaces through optical cables, and the laser light source and the ordinary light source manually select and switch the light sources; the laser convergence and microscopic observation system is connected with the input end of the CCD camera, and the output end of the CCD camera and the input end of the motion controller are connected with the computer through a USB line to carry out microscopic observation positioning and numerical control programming; the laser gathering and microscopic observation system is arranged on the laser gathering module mechanical moving system, the output end of the motion controller is connected with the sample table mechanical numerical control moving system, the sample table mechanical numerical control moving system is arranged on the air floatation damping platform, and the air inlet end of the air floatation damping platform is connected with the air pump.
5. The method for the non-destructive transfer of self-supporting low-dimensional materials according to claim 1, wherein the microscopic positioning transfer process comprises the following steps:
(1) transferring the rigid supporting sheet to the upper part of the carrier by adopting a method of combining vacuum adsorption or magnetic adsorption with a sliding table;
(2) introducing non-contact external microgravity to the material or applying directional electrostatic force between the sample and the target carrier;
(3) and (5) microscopically observing the combination condition of the two-dimensional material and the target carrier.
6. The method for non-destructive transfer of self-supporting low-dimensional material according to claim 5, wherein after separating the low-dimensional material from the rigid support sheet by laser cutting, after ensuring that the material has been successfully attached to the carrier, the rigid support sheet is removed again by vacuum suction or magnetic suction in combination with a slide table to prevent the transferred sample from being displaced by electrostatic force when the rigid support sheet is removed.
7. The method for the non-destructive transfer of self-supporting low-dimensional materials according to claim 5, wherein during the micro-positioning transfer, a vacuum nozzle with a customized caliber is used for vacuum suction to suck up the rigid support sheet; the magnetic adsorption adopts a tiny electromagnet, the rigid support sheet adopted at the moment is made of a magnetic material, and the magnetic property of the electromagnet suction head is manually controlled, so that the rigid support sheet is stably transferred in the transfer process and cannot be vibrated and dislocated in the moving process.
8. The method for the nondestructive transfer of self-supporting low dimensional material according to claim 5 wherein the microgravity is introduced during the microscopic positioning transfer in consideration of not affecting the material's own property structure and being easily removed; the method of using electrostatic force considers that the surface of the carrier is insulated, the electrostatic force can not be conducted away quickly, and the electrostatic force is transferred as soon as possible after the carrier is introduced, so that the electrostatic force is prevented from dissipating.
9. The method for the non-destructive transfer of self-supporting low-dimensional materials according to claim 5, wherein the resolution of the microscope is less than 5 μm during the microscopic positioning transfer, and the slide stage comprises translation in three directions of X-Y-Z and rotation in the plane, and the repetitive positioning precision is less than 1 μm.
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| CN103647012A (en) * | 2013-12-20 | 2014-03-19 | 中国科学院半导体研究所 | Chip transfer method for LED (light-emitting diode) wafer level package |
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| CN103831536B (en) * | 2014-03-05 | 2016-01-13 | 北京工业大学 | Femtosecond laser manufactures method and the device thereof of three-dimensional micro-channel in PMMA |
| CN104129783B (en) * | 2014-08-04 | 2017-02-15 | 中国科学院金属研究所 | Low cost clean nondestructive transfer method of large area of graphene |
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| CN103647012A (en) * | 2013-12-20 | 2014-03-19 | 中国科学院半导体研究所 | Chip transfer method for LED (light-emitting diode) wafer level package |
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