CN112578669A - Two-dimensional material transfer method and intelligent transfer system - Google Patents
Two-dimensional material transfer method and intelligent transfer system Download PDFInfo
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Abstract
本发明提出一种二维材料转移方法及智能转移系统，以解决现有大面积二维材料转移过程中存在转移效率低、转移精度不高以及二维材料剥离不均匀的技术问题。本发明方法为：在载玻片下表面涂布粘性随温度反向变化的材料，粘取待转移二维材料；然后将待转移二维材料与二维材料受体准确定位；最后将载玻片放置在二维材料受体表面，加热载玻片将待转移二维材料转移到二维材料受体上。本发明系统包括底座、二维材料转移台、二维材料放置台以及光学成像单元，其中，二维材料转移台包括三维机械臂、涂有PDMS的载玻片、微位移台、二维材料受体放置台及包浆印刷工艺的加热片；光学成像单元包括支架、高倍显微镜高清CDD相机以及计算机。
The present invention provides a two-dimensional material transfer method and an intelligent transfer system to solve the technical problems of low transfer efficiency, low transfer precision and uneven peeling of two-dimensional materials in the existing large-area two-dimensional material transfer process. The method of the invention is as follows: coating the lower surface of the glass slide with a material whose viscosity changes inversely with temperature, and sticking the two-dimensional material to be transferred; then accurately positioning the two-dimensional material to be transferred and the two-dimensional material receptor; The sheet is placed on the surface of the 2D material receptor, and the glass slide is heated to transfer the 2D material to be transferred onto the 2D material receptor. The system of the present invention includes a base, a two-dimensional material transfer stage, a two-dimensional material placement stage, and an optical imaging unit, wherein the two-dimensional material transfer stage includes a three-dimensional robotic arm, a slide glass coated with PDMS, a micro-displacement stage, a two-dimensional material receiving Body placement table and heating film for paste printing process; optical imaging unit includes bracket, high-power microscope HD CDD camera and computer.
Description
Technical Field
The invention relates to a two-dimensional material transfer method and a two-dimensional material intelligent transfer system.
Background
Two-dimensional materials typically include graphene, black phosphorus, molybdenum disulfide, tungsten disulfide, BN, etc., whose relatively rare spatial structure and electrical and thermal properties are of particular interest to industry and academia. Two-dimensional materials are often used in laboratories for some relevant experiments due to their excellent physicochemical properties, and the precision and quality of such material plane transfer are extremely important for the final experimental results.
In the prior art, the number and types of related products for two-dimensional material transfer are extremely rare. At present, a common laboratory method for transferring a two-dimensional planar material is to directly stick the material down by a researcher with an adhesive tape, and then transfer the material onto a transferred object. Thus, not only is the amount of material transferred very limited, but the material transferred is not uniform, and it is difficult to ensure that the results of the experiment achieve the expected results. The coarse transfer easily results in a great waste of the two-dimensional material prepared in the laboratory, the experiment cost is difficult to control, and the exact experiment result is difficult to obtain because the amount of each transfer is difficult to maintain at a certain constant number.
In addition, laboratories often transfer two-dimensional materials by an etching method, in which a metal substrate on which a single layer of two-dimensional material is grown is coated with methyl methacrylate, the two-dimensional material is transferred to a target position by a method of etching away metal with hydrochloric acid, and then the methyl methacrylate on the surface of the two-dimensional material is removed with acetone, which causes cracks on the surface of the two-dimensional material which are difficult to avoid, and the methyl methacrylate is difficult to completely remove. When the two-dimensional material is stripped, the traditional copper sheet is generally adopted for heating, and the material is easily stripped unevenly due to uneven heating.
Disclosure of Invention
The invention aims to solve the technical problems of low transfer efficiency, low transfer precision and uneven peeling of a two-dimensional material in the conventional large-area two-dimensional material transfer process, and provides a two-dimensional material transfer method and an intelligent transfer system.
In order to achieve the purpose, the invention adopts the technical scheme that: a two-dimensional material transfer method, characterized by comprising the steps of:
2, accurately positioning a two-dimensional material to be transferred and a two-dimensional material receptor;
and 3, placing the glass slide on the surface of a two-dimensional material receptor, heating the glass slide, and transferring the two-dimensional material to be transferred to the two-dimensional material receptor.
Further, in step 1, the material with viscosity changing inversely with temperature is PDMS (Polydimethylsiloxane), the thickness is 100 μm to 500 μm, and the two-dimensional material to be transferred, which is adhered to the material, can be easily peeled off when being heated.
Further, in the step 1, a micron-sized automatic control three-dimensional mechanical arm is adopted to clamp the glass slide and pick up the two-dimensional material to be transferred; in step 3, the three-dimensional mechanical arm is adopted to place the glass slide on the surface of the two-dimensional material receptor,
further, in the step 2, high power microscope imaging is firstly adopted, and then the CNN artificial neural network automatic identification technology is utilized to accurately position the overlapping position of the two-dimensional material to be transferred and the two-dimensional material receptor.
Further, in the step 2, the two-dimensional material to be transferred and the two-dimensional material receptor are accurately positioned as follows:
2.1) clearly acquiring an image of a two-dimensional material receptor by adopting a high-power microscope, and establishing an xoy plane coordinate by taking the right center position of a high-power microscope lens as a zero point;
2.2) identifying the geometric midpoint of the two-dimensional material receptor, and controlling the movement of the two-dimensional material receptor by adopting a micro-displacement platform to ensure that the geometric midpoint of the two-dimensional material receptor is superposed with the zero point of the xoy plane;
2.3) moving the glass slide to a high power microscope clear identification area by the three-dimensional mechanical arm, identifying the figure and the position of the two-dimensional material to be transferred, and calculating the position of a geometric center point of the two-dimensional material to be transferred;
2.4) calculating the distance from the geometric center point of the two-dimensional material to be transferred to the zero point of the xoy plane, and moving the geometric center point of the two-dimensional material to be transferred to the zero point of the xoy plane by the three-dimensional mechanical arm along a straight line between the two points;
2.5) the high power microscope identifies the midpoint coordinate position of the two-dimensional material to be transferred for many times until the midpoint coordinate position is positioned at the zero point of the xoy plane;
2.6) the three-dimensional mechanical arm descends downwards to move the two-dimensional material to be transferred to a position 100-200 mu m above the two-dimensional material receptor, so that the two-dimensional material to be transferred and the two-dimensional material receptor clearly enter the visual field range of the high-power microscope;
2.7) adopting a micro-displacement table to control the two-dimensional material receptor to rotate on the horizontal plane by 360 degrees around the central axis, sampling every 0.5-1 degrees, defining the area of the overlapping area of the two-dimensional material to be transferred and the two-dimensional material receptor at each sampling angle as S1, defining the area of the two-dimensional material receptor as S2, and calculating the overlapping rate o (%)/of S1 and S2 at each sampling angle
o(％)＝S1/S2
Finding out the angle corresponding to the maximum overlapping rate, and then rotating the micro-displacement table to the angle to complete the accurate positioning of the two-dimensional material to be transferred and the two-dimensional material receptor.
Further, the step 2.3) is specifically as follows:
obtaining a boundary fitting function f (x, y) of a two-dimensional material receptor through MATLAB, and integrating and calculating a geometric central point (x, y):
further, in step 1, the slide is a standard slide;
in the step 3, a heating plate manufactured by the tungsten paste printing process is adopted for heating, and the heating temperature is 90-100 ℃.
Meanwhile, the invention also provides a two-dimensional material intelligent transfer system, which is characterized in that: comprises a base 6, a two-dimensional material transfer table, a two-dimensional material placing table 9 and an optical imaging unit, wherein the two-dimensional material transfer table, the two-dimensional material placing table and the optical imaging unit are arranged on the base 6;
the two-dimensional material transfer table comprises a three-dimensional mechanical arm 2, a glass slide 3 arranged at the clamping end of the three-dimensional mechanical arm 2, a micro-displacement table 5 positioned beside the three-dimensional mechanical arm 2 and a two-dimensional material receptor placing table 4 arranged on the micro-displacement table 5; the lower surface of the glass slide 3 is coated with a material 31 with viscosity changing inversely with temperature; a heating plate 41 is arranged in the middle of the two-dimensional material receptor placing table 4;
the two-dimensional material placing table 9 is positioned on the other side of the three-dimensional mechanical arm 2; the two-dimensional material placing table 9 and the two-dimensional material receptor placing table 4 are both positioned in the operable range of the three-dimensional mechanical arm 2;
the optical imaging unit comprises a bracket 8, a high power microscope 1 arranged on the bracket 8, a high definition CDD camera 7 arranged at the upper end of the high power microscope 1 and a computer 10;
the high power microscope 1 is arranged right above the two-dimensional material receptor placing table 4; the bracket 8 can control the high power microscope 1 to move up and down;
the computer 10 is used for intelligent transfer system control, receiving the image transmitted by the high-definition CDD camera 7 and performing calculation processing.
Further, the slide 3 is a standard slide; the material 31 with the viscosity changing reversely along with the temperature is PDMS, and the two-dimensional material to be transferred, which is adhered on the material, is easy to peel off when being heated;
the three-dimensional mechanical arm 2 is a micron-sized automatic control three-dimensional mechanical arm and can control the two-dimensional material to be transferred to accurately move; the micro-displacement table 5 is a micron-sized micro-displacement table, can adjust the position of x, y, z and r dimensions, and can control the precise movement of a two-dimensional material receptor;
the heating plate 41 is made by a paste coating printing process, and can ensure uniform heating.
Further, the high power microscope 1 has a 2000-fold magnification, a light source on the side surface, and the high definition CDD camera 7 has a resolution of 0.7 μm, which ensures the resolution of the image and thus the precision of the two-dimensional material transfer.
The invention has the beneficial effects that:
1) the two-dimensional material transfer method adopts a CNN artificial neural network recognition technology and is matched with a high power microscope to carry out closed loop feedback operation on the whole transfer process, and the two-dimensional material to be transferred and a two-dimensional material receptor are accurately positioned so as to achieve accurate transfer of the two-dimensional material. The CNN artificial neural network recognition technology can achieve efficient and reliable recognition, can realize rapid and large-scale two-dimensional material transfer on the premise of ensuring transfer precision, and is suitable for industrial large-scale production.
2) The two-dimensional material transfer method adopts PDMS with viscosity changing reversely along with temperature to coat the lower surface of the glass slide, picks up the two-dimensional material, and releases the picked-up two-dimensional material by heating, so that the two-dimensional material to be transferred is completely transferred, the waste of the two-dimensional material is avoided, and the cost can be effectively controlled.
3) The two-dimensional material transfer method adopts the PID temperature control technology to carry out accurate temperature control, and simultaneously adopts the heating plate prepared by the tungsten paste printing technology to ensure that the PDMS material is uniformly heated, and accurately controls the temperature range to be 90-100 ℃, so that the two-dimensional material adhered to the lower surface of the glass slide is easy to peel.
4) The two-dimensional material intelligent transfer system adopts the micron-sized automatic control three-dimensional mechanical arm to accurately move the two-dimensional material to be transferred and adopts the micron-sized micro-displacement table to accurately move the two-dimensional material receptor, thereby improving the transfer precision.
5) The two-dimensional material intelligent transfer system adopts the high power microscope, the optimal imaging distance of the lens in the high power microscope is 3.7cm, the enough operation space is ensured, the side surface of the high power microscope is provided with the light source for auxiliary imaging, the upper end of the high power microscope is provided with the high definition CDD camera with the minimum resolution of 0.7 mu m, the resolution ratio of the image is ensured, and the precision of the two-dimensional material transfer is ensured.
Drawings
FIG. 1 is a schematic structural diagram of a two-dimensional material intelligent transfer system according to the present invention.
Description of reference numerals:
the system comprises a 1-high power microscope, a 2-three-dimensional mechanical arm, a 3-glass slide, a 31-material with viscosity changing reversely along with temperature, a 4-two-dimensional material receptor placing table, a 41-heating plate, a 5-micro displacement table, a 6-base, a 7-high definition CDD camera, an 8-bracket, a 9-two-dimensional material placing table and a 10-computer.
Detailed Description
In order to more clearly explain the technical solution of the present invention, the following detailed description of the present invention is made with reference to the accompanying drawings and specific examples.
The invention provides an intelligent transfer system capable of conveniently transferring two-dimensional materials, which comprises a two-dimensional material transfer table and a two-dimensional material placing table 9 arranged beside the two-dimensional material transfer table. The two-dimensional material transfer table comprises a micron-scale automatically controlled three-dimensional mechanical arm 2, a standard glass slide 3, a two-dimensional material receptor placing table 4, a micro-displacement table 5, a support 8, an optical imaging unit and a base 6 for supporting all components. The two-dimensional material placing table 9 is located within the operable range of the three-dimensional robot arm 2.
A standard glass slide 3 with the size of 25.4mm multiplied by 76.2mm and the thickness of 1mm is arranged at the clamping end of the three-dimensional mechanical arm 2; the lower surface of the standard glass slide 3 is coated with a material 31 with viscosity changing reversely with temperature, in the embodiment, the material 31 with viscosity changing reversely with temperature adopts PDMS material with the thickness of 100-500 μm, a transparent PDMS film is formed, the refractive index is 1.41, the two sides have weak viscosity, the material is used for sticking two-dimensional materials, the viscosity is weakened when heating, and the stuck two-dimensional materials are released by heating.
The two-dimensional material receptor placing table 4 is arranged on a micron-level high-precision micro-displacement table 5 right below the standard glass slide 3, a heating sheet 41 for coating and printing technology is arranged in the middle of the two-dimensional material receptor placing table 4, the heating range is 80-150 ℃, and the temperature when the PDMS is heated to release the two-dimensional material is 90-100 ℃. The micro-displacement stage 5 can perform position adjustment in four dimensions of x, y, z and r (rotation).
The optical imaging unit includes a high power microscope 1, a high definition CDD camera 7, and a computer 10. The high power microscope 1 is fixed on the support 8, the whole height of the support 8 is 60cm, and the up-and-down movement of the high power microscope 1 can be controlled. The high power microscope 1 has the magnification of 2000 times, the optimal imaging distance of the lens is 3.7cm, and the side surface is provided with a light source for auxiliary imaging, so that the sufficient operation space and the pattern resolution are ensured. The high-definition CDD camera 7 is arranged at the upper end of the high-power microscope 1 and is used for shooting the image amplified by the high-power microscope 1, and the minimum resolution of the image is 0.7 mu m. The computer 10 is used for controlling the whole intelligent transfer system, receiving the image transmitted by the high-definition CDD camera 7 and performing calculation processing.
The optical imaging unit adopts a CNN (Convolutional Neural Network) artificial Neural Network identification technology in the image identification process, the CNN Convolutional Neural Network is a mature deep learning framework at present, and the framework is inspired by a biological natural visual cognition mechanism and can achieve efficient and reliable identification. The CNN artificial neural network recognition technology is applied to the two-dimensional material transfer process, can realize rapid and large-scale two-dimensional material transfer on the premise of ensuring the transfer precision, and is suitable for the industrial large-scale production process.
The temperature control technology of the system adopts the PID closed-loop automatic control technology, measures the temperature of the transferred material in real time, feeds the temperature back to the system, and carries out error correction by comparing the measured temperature with a preset expected value, thereby achieving the dynamic control of the temperature of the transferred material and stabilizing the temperature of the transferred material near an ideal temperature. Meanwhile, the special tungsten paste printing process is adopted in the heating sheet 41 for heating the PDMS and the two-dimensional material, so that the heating temperature range of the two-dimensional material is larger, and the whole material is uniformly heated.
In the process of transferring the two-dimensional material, firstly, coating a material (PDMS and the like) with viscosity changing along with temperature change on a standard glass slide 3, precisely transferring the two-dimensional material adhered on the PDMS on the lower surface of the standard glass slide 3 to the physical surface of a two-dimensional material receptor by the system under the cooperation of the CNN artificial neural network automatic identification technology of an optical imaging unit and a high power microscope 1, and then heating a heating sheet 41, so that the two-dimensional material adhered on the standard glass slide 3 falls off and is transferred to the two-dimensional material receptor.
The difficulty in the overall transfer process is how to accurately and quickly transfer the stripped two-dimensional material to a two-dimensional material receiver, which is also a departure from conventional transfer methods. In the transferring process, the high power microscope 1 is matched with the CNN artificial neural network recognition technology to perform closed loop feedback operation on the whole transferring process so as to achieve accurate transferring of the two-dimensional material.
In the transferring process, because the two-dimensional material receptor and the two-dimensional material to be transferred are not in the same plane, and the two areas at the initial stage of transferring have a longer distance, a certain error is introduced into the initial recognition, and the transferring error is continuously corrected in a closed-loop feedback mode in the whole transferring process until a certain error allowable range is met.
The two-dimensional material transfer system comprises the following specific operation steps:
1) placing a two-dimensional material receptor on a two-dimensional material receptor placing table 4, pressing an adsorption key and adsorbing the two-dimensional material receptor at a central position;
2) controlling the distance from the high-power microscope 1 to the operating platform, enabling the lens of the high-power microscope 1 to be just 3.7cm above the operating platform, clearly acquiring an image on the two-dimensional material receptor placing platform 4, and establishing an xoy plane coordinate at the positive center position of the lens of the high-power microscope 1;
3) the computer 10 identifies the geometric midpoint of the two-dimensional material receptor and controls the micro-displacement table 5 to move so that the geometric midpoint of the two-dimensional material receptor is positioned at the zero point of the xoy plane;
determination of geometric center point of two-dimensional material receptor: obtaining a boundary fitting function f (x, y) of a two-dimensional material receptor through MATLAB, and calculating a geometric central point (x, y) through integration
4) Loading a standard glass slide 3 coated with PDMS on an automatically controlled three-dimensional mechanical arm 2 with the PDMS facing downwards to prepare for obtaining a two-dimensional material;
5) the three-dimensional mechanical arm 2 is turned to the position right above the two-dimensional material placing table 9, the standard glass slide 3 is controlled to descend, the two-dimensional material to be transferred is adhered and taken, and the two-dimensional material is turned to the direction on the two-dimensional material receptor placing table 4 and enters the identification area of the lens of the high power microscope 1;
6) the high power microscope 1 is lifted to a position 3.7cm away from the two-dimensional material adhered by PDMS below the standard glass slide 3, the computer 10 can clearly identify the figure and the position of the two-dimensional material at the moment, and the computer 10 calculates the position of the geometric center point of the two-dimensional material;
7) calculating the distance from the central point to the zero point of the xoy plane, and moving the geometric midpoint of the two-dimensional material to the zero point of the xoy plane by the three-dimensional mechanical arm 2 along a straight line between the two points;
8) and identifying the coordinate position of the midpoint of the two-dimensional material again, and judging whether the coordinate position is positioned at the coordinate zero point of the xoy plane. If the coordinate is at the zero point, entering the next link, otherwise, repeating the operation process of 7);
9) the three-dimensional mechanical arm 2 descends to a position 100-200 mu m above the two-dimensional material receptor, and the high power microscope 1 is adjusted again at the moment, so that the lens of the high power microscope 1 descends to a position 3.7cm above the two-dimensional material receptor, and the two-dimensional material receptor can clearly enter the visual field range of the high power microscope 1;
10) at the moment, the colors of the two-dimensional material, the two-dimensional material receptor and the overlapping area of the two-dimensional material and the two-dimensional material receptor are different and are from light to deep, the overlapping area S1 of the two-dimensional material and the two-dimensional material receptor and the overlapping area S2 of the two-dimensional material and the two-dimensional material receptor are respectively calculated, and the overlapping rate o (%) of the two areas is S1/S2;
11) controlling the micro-displacement platform 5 to rotate 360 degrees around the central axis on the horizontal plane, sampling once every 0.5-1 degrees, calculating the overlapping rate o (%) at each sampling angle, comparing an angle corresponding to the maximum overlapping rate, and finally rotating the micro-displacement platform 5 to the angle;
12) the three-dimensional mechanical arm 2 drops the two-dimensional material to the surface of the two-dimensional material receptor, the heating sheet 41 is controlled to start heating at the same time, when the surface temperature of the two-dimensional material receptor placing table 4 reaches 100 ℃, the three-dimensional mechanical arm 2 starts to move upwards, and the two-dimensional material is transferred to the surface of the two-dimensional material receptor at the moment;
13) the standard glass slide 3 with PDMS and the two-dimensional material and two-dimensional material receptor that have been successfully transferred are removed. And (3) replacing the standard glass slide 3, the two-dimensional material and the two-dimensional material receptor, and returning to the step 1) to perform the two-dimensional material transfer operation again.
The system has high automation degree, and can automatically complete the transfer of the two-dimensional material to the two-dimensional material receptor after a preset transfer task.
The above description is only for the purpose of describing the preferred embodiments of the present invention and is not intended to limit the technical solutions of the present invention, and any known modifications made by those skilled in the art based on the main technical concepts of the present invention are within the technical scope of the present invention.
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