WO2019090799A1 - 一种微米直径的锥形毛移动和转移纳米线的方法 - Google Patents

一种微米直径的锥形毛移动和转移纳米线的方法 Download PDF

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WO2019090799A1
WO2019090799A1 PCT/CN2017/111168 CN2017111168W WO2019090799A1 WO 2019090799 A1 WO2019090799 A1 WO 2019090799A1 CN 2017111168 W CN2017111168 W CN 2017111168W WO 2019090799 A1 WO2019090799 A1 WO 2019090799A1
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nanowire
nanowires
copper mesh
tapered hair
diameter
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French (fr)
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张振宇
崔俊峰
王博
郭东明
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Dalian University of Technology
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Dalian University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/10—STM [Scanning Tunnelling Microscopy] or apparatus therefor, e.g. STM probes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
    • G01Q30/02—Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0061—Methods for manipulating nanostructures
    • B82B3/0076—Methods for manipulating nanostructures not provided for in groups B82B3/0066 - B82B3/0071
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014—Type of force applied
    • G01N2203/0016—Tensile or compressive
    • G01N2203/0017—Tensile
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/026—Specifications of the specimen
    • G01N2203/0286—Miniature specimen; Testing on microregions of a specimen
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/026—Specifications of the specimen
    • G01N2203/0298—Manufacturing or preparing specimens
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206—Modifying objects while observing
    • H01J2237/2062—Mechanical constraints

Definitions

  • a micron-diameter tapered hair moving and transferring nanowires method involving nanowire movement, transfer and fixation has important effects on subsequent testing and characterization, particularly involving scanning electron microscopy and transmission electron microscopy in situ nanometers. Testing and characterization of mechanics.
  • Nano-precision surface fabrication methods are an effective way to meet this demanding processing requirement.
  • To develop new nano-precision surface fabrication processes and methods it is necessary to study the mechanism of atomic-scale damage generation and evolution, material removal mechanism, and stress-induced damage formation.
  • Transmission electron microscopy in situ nanomechanics is a scientific method to study this basic principle. In the past, due to the limitations of experimental conditions, it is difficult to test and characterize the in-situ nanomechanics of transmission electron microscopy.
  • the two methods of fixing nanowires generally use chemical vapor deposition or physical vapor deposition, which easily contaminate the nanowires, so that subsequent in situ testing and characterization are affected, even impossible, and it is difficult to obtain atomic scale.
  • High resolution transmission electrical mirroring In addition, in the process of moving and transferring nanowires, these two methods easily generate defects such as holes, interstitial atoms, stacking faults, and dislocation loops inside the nanowires, which enables scanning and transmission electricity obtained at the micro-nano scale. Mirroring is difficult to extend to macro materials.
  • the present invention employs a micron-diameter tapered hair moving and transferring nanowires method, using tapered hair to achieve nano Movement and transfer of rice noodles.
  • a micron-diameter tapered hair moving and transferring nanowires the nanowires having a diameter of 60-150 nm, the tapered hairs of the human eyebrows, the eyelashes, the wolf and the sheep, and the diameter range of 1-100 ⁇ ,
  • the tip has a radius of curvature of 0.8-3 ⁇ and a length of 4-10 mm.
  • the plastic film on the copper mesh for the transmission electron microscope is burned off with a fire, and the copper mesh is left, and the diameter of the hole is 50-100 ⁇ .
  • the nanowires are then taken up in an ultrasonically dispersed nanowire of acetone liquid using a sonicated copper mesh.
  • the copper mesh and the tapered hair distributed with the nanowires are respectively placed on the moving platforms of two different optical microscopes to realize the millimeter and micron-scale movement of the tapered hair, thereby realizing the movement and transfer operation of the nanowires.
  • a small drop of conductive silver glue is drawn from the tip of the tapered hair and dropped on both ends of the nanowire.
  • the radius of the conductive silver paste behind the drop is 4-8 ⁇ .
  • the present invention provides a method of moving and transferring nanowires using micron-diameter tapered hair using a moving platform of two optical microscopes.
  • Nanowires have a diameter of 60-150 nm.
  • the diameter of the nanowire exceeds 150 nm, the electron beam is difficult to penetrate, and it is difficult to obtain an atomic-scale high-resolution transmission electron image; the diameter of the nanowire is less than 60 nm, which is very difficult to operate and find under an optical microscope.
  • the choice of nanowires with diameters ranging from 60-150 nm is a combination of operational and atomic imaging.
  • the tapered hair is a human eyebrow, an eyelash, a wolf and a sheep, having a diameter ranging from 1-100 ⁇ , a tip radius of 0.8-3 ⁇ , and a length of 4-10 mm. These four materials are relatively easy to obtain, from the human body and the writing brush. In addition, these hairs are tapered, which is very beneficial for manipulating nanowires. These four hairs range in diameter from 1-100 ⁇ for easy manipulation of the nanowires. The tapered hair is easily inserted obliquely under the optical microscope to the lower portion of the nanowire, thereby realizing the operation of the nanowire.
  • the tip has a radius of curvature of 0.8-3 ⁇ , which is very beneficial for utilizing the electrostatic attraction between the tapered hair and the nanowire.
  • the length is 4-10 mm, so that the tapered hair has both rigidity and flexibility, so that the operation and transfer of the nanowire can be realized.
  • the plastic film on the copper mesh for the transmission electron microscope is burned off by fire, leaving a copper mesh having a diameter of 50-100 ⁇ .
  • the tapered hairs can be inserted into the lower part of the nanowires, so that the nanowires can be more accurately moved, extracted, and transferred. Therefore, it is necessary to remove a plastic film covered by the copper mesh surface. Since the plastic film is very thin, the plastic film can be quickly removed by fire, and it is very clean, not It will pollute subsequent operations. Since the length of the nanowires is generally on the order of micrometers, the pore size is selected to be 50-100 ⁇ , which can place the nanowires without being transferred into the pores of the copper mesh.
  • the nanowires were ultrasonically dispersed in acetone at a ratio of l-2 min.
  • Acetone has strong decontamination and dispersing ability, and the effect of ultrasound will be more obvious. Therefore, ultrasonic dispersion with acetone can be performed for a short period of time, which is l-2 min.
  • the copper mesh was clamped with a pair of tweezers, and ultrasonicated in an acetone solution for 0.5-1 min, and then the nanowire was taken in the acetone liquid of the ultrasonic dispersion nanowire by the ultrasonicized copper mesh. After the acetone solution was evaporated, the nanowires were distributed in the copper. Net surface. Ultrasonic cleaning of the copper mesh with tweezers in acetone is used to clean away traces and contamination from the burning of the copper mesh. Nanowires were removed from the dispersed nanowire in acetone solution using a cleaned copper mesh to leave more uniform distribution of nanowires on the copper network.
  • the copper mesh and the tapered hair distributed with the nanowires are respectively placed on the moving platforms of two different optical microscopes, and the tapered hairs are bonded to the tips of the tapered rods with conductive silver glue, and the other flat ends are used.
  • the conductive silver glue is fixed on the moving platform of the microscope.
  • the copper mesh is placed on a moving platform of an optical microscope, and an optical microscope is used to find and manipulate the nanowires.
  • the tapered hair is connected to the moving platform of another optical microscope, mainly using the macroscopic and microscopic movement functions of the mobile platform of another optical microscope to realize the precise movement, extraction, transfer and other operations of the nanowire.
  • the millimeter and micron-scale combined movement functions of the optical microscope enable the operation of the nanowires.
  • the millimeter and micron-scale movement of the tapered hair is realized by the coarse adjustment and fine adjustment knob of the moving platform of the optical microscope, thereby realizing the movement and transfer operation of the nanowire.
  • the coarse adjustment knob of the optical microscope mainly realizes the millimeter-level rapid movement of the tapered hair, and the fine adjustment knob realizes the micro-scale movement of the tapered hair, thereby realizing the operation of the nanowire.
  • the tapered hair was inserted obliquely into the lower part of the nanowire, and the nanowires were picked up to make the electrostatic attraction of the nanowires and the copper mesh. It becomes smaller, and then the nanowires are extracted from the surface of the copper mesh under the electrostatic attraction of the tapered hairs and the nanowires.
  • Replace the copper mesh with a scanning electron microscope or a transmission electron microscope In situ mechanical testing of the microdevice, placing the nanowires at the stretching site.
  • Use a tip of a tapered hair to poke a drop of conductive silver glue, gently drop it on one end of the nanowire, and lick another droplet onto the other end.
  • the size of the conductive silver gel after dropping is 4-8 ⁇ . It does not pollute the nanowires and has good bonding strength after curing.
  • the conductive silver paste After being placed in the air for 2-4 h, the conductive silver paste is solidified, and the in-situ nanometer mechanical test and characterization of the scanning electron microscope or the transmission electron microscope can be performed. After standing in the air for 2-4 h, the conductive silver paste is solidified, the nanowires are firmly fixed on the micro device, and there is no physical and chemical vapor deposition pollution and damage to the nanowires caused by the ion beam and the electron beam, ie It can be tested and characterized by in-situ nanomechanics by scanning electron microscopy or transmission electron microscopy. Advantageous effects of the invention
  • the effect and benefit of the present invention is that the movement and transfer of the nanowires are realized by using the micron-diameter tapered hair, and is fixed by the conductive silver glue, thereby avoiding the pollution caused by the operation of the conventional focused ion beam and the electron beam on the nanowire. damage.
  • FIG. 1 is a scanning electron micrograph of a micron-diameter tapered sheep.
  • FIG. 3 is an optical micrograph of a nanowire transferred under a light microscope.
  • a micron-diameter tapered hair moving and transferring nanowires method the use of tapered hair to achieve movement and transfer of nanowires, characterized by:
  • the diameter of the nanowire is 60-150 nm
  • tapered hair is human eyebrows, eyelashes, wolf and sheep, diameter range of 1-100 ⁇ , tip radius of curvature of 0.8-3 ⁇ , length of 4-10 mm;
  • the nanowires were ultrasonically dispersed in acetone with a mean of 1.5-2 min.
  • the copper mesh after the film removal was clamped with a pair of tweezers, and ultrasonically cleaned in an acetone solution for 40-60 s to remove traces and contamination after the fire. Then, the copper mesh was taken out, and the nanowires were taken up in the acetone-dispersed nanowire solution with a tweezers, and placed in the air. After the acetone was evaporated, the nanowires were distributed on the copper mesh.
  • a copper mesh with nanowires was placed on a moving platform of an optical microscope.
  • the micron-diameter tapered hair is bonded to the tip end of the tapered plastic slender rod with conductive silver glue, and the other end is fired into a flat end, and is fixed on the moving platform of another optical microscope with conductive silver glue.
  • the nanowires were found in the eyepiece of the microscope and the focus was sharp.
  • a moving platform of another optical microscope combined with coarse adjustment and fine adjustment, the millimeter- and micro-scale movement of the micron-diameter tapered hair is gradually inserted into the lower portion of the nanowire with a tapered hair.
  • the fine adjustment knob of the mobile platform After inserting, use the fine adjustment knob of the mobile platform to realize the micron-level upward movement of the tapered hair, and pick up one end of the nanowire to separate the copper mesh. After one end of the nanowire is provoked, its electrostatic attraction with the copper mesh gradually decreases with the decrease of the contact area. Finally, only one end of the contact is contacted, and the tapered hair is continued to move upward, and the nanowire is separated from the copper mesh, as shown in Fig. 3. As shown, the movement, extraction and transfer operations of the micron-diameter tapered hair to the nanowire are achieved. After the nanowires are separated from the copper mesh, the microdevices for testing by scanning electron microscopy or transmission electron microscopy are placed in the position of the copper mesh.
  • a drop of conductive silver glue is placed on the moving platform of the micro device, and a small drop of conductive silver glue is taken with the tip of the tapered hair, and is accurately dropped onto one end of the nanowire by a moving platform, so that one end of the conductive silver glue and the nanowire Contact, thereby causing the conductive silver glue to drip.
  • a small drop of conductive silver paste is taken with the tip of the tapered hair, and is accurately dropped onto one end of the nanowire by a moving platform, so that one end of the conductive silver glue and the nanowire Contact, thereby causing the conductive silver glue to drip.
  • the radius of the conductive silver paste after the drop is 5-8 ⁇ .
  • the conductive silver paste is allowed to stand in the air for 3-4 hours to achieve curing.
  • the cured microdevice was loaded into the PI 95 TEM Picolndenter transmission electron microscopy in-situ mechanical test system.
  • the system was inserted into the FEI Tecnai F20 field emission transmission electron microscope and subjected to TEM nanomechanical tensile test.
  • the operating voltage of the transmission electron microscope was 200 kV. .
  • the loading rate is 10 nm/s, and a tensile load is applied to the nanowires.
  • the diameter of the nanowire is 80-100 nm
  • the breaking force of the tensile fracture is 110 ⁇
  • the breaking strength of the nanowire is 12 GPa.
  • the dynamic stretching process of the nanowires was recorded by the in-situ mechanical testing system, from which the key atomic-scale high-resolution transmission electron image of the fracture enthalpy can be extracted, thereby realizing the in-situ mechanical tensile test and characterization experiment of the nanowire by TEM. .

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Abstract

一种微米直径的锥形毛移动和转移纳米线的方法，纳米线的直径为60-150nm，锥形毛的直径为1-100μm，尖端曲率半径为0.8-3μm，长度为4-10mm；去掉透射电镜用的铜网上的塑料薄膜，留下铜网，孔的直径为50-100μm；用超声后的铜网在超声分散纳米线的丙酮液体中捞取纳米线；将分布有纳米线的铜网和锥形毛分别放在两个不同的光学显微镜的移动平台上，实现锥形毛的毫米和微米级移动，从而实现对纳米线的移动和转移操作。用锥形毛尖端蘸取一小滴导电银胶，分别滴在纳米线的两端，滴落后的导电银胶的半径为4-8μm。所述方法采用微米直径的锥形毛实现了纳米线的移动和转移，并用导电银胶固定，避免了传统聚焦离子束和电子束对纳米线的操作造成的污染和损伤。

Description

一种微米直径的锥形毛移动和转移纳米线的方法 技术领域
[0001] 一种微米直径的锥形毛移动和转移纳米线的方法， 涉及纳米线的移动、 转移和 固定， 对后续的测试与表征具有重要的影响， 特别涉及扫描电镜和透射电镜原 位纳米力学的测试与表征。
背景技术
[0002] 高性能装备要求高性能零件表面具有纳米级平面度、 亚纳米级粗糙度， 这种苛 刻的超精密加工要求已经接近物理加工的极限， 需要研发新的超精密加工工艺 与装备来解决。 纳米精度表面制造方法是满足这种苛刻加工要求的有效方法。 要研发新的纳米精度表面制造工艺与方法， 就要对原子尺度损伤产生和演变机 制、 材料去除机理、 应力诱导损伤形成机制进行研究。 透射电镜原位纳米力学 是研究这种基本原理的科学方法， 过去由于实验条件的限制， 难以进行透射电 镜原位纳米力学的测试与表征。 其中一个重要的原因是采用聚焦离子束和电子 束对纳米线进行切割、 焊接、 转移、 移动等操作， 会对纳米线造成污染和损伤 。 这两种方法固定纳米线的吋候一般采用化学气相沉积或者物理气相沉积， 容 易污染纳米线， 从而使得随后的原位测试与表征受到重要的影响， 甚至无法进 行， 也很难获得原子尺度的高分辨透射电镜像。 此外， 这两种方法在移动和转 移纳米线的过程中， 容易在纳米线内部产生空穴、 填隙原子、 层错和位错环等 缺陷， 这使得在微纳尺度获得的扫描和透射电镜像很难扩展到宏观材料。
[0003] 为了消除传统的聚焦离子束和电子束在移动、 转移、 切割、 焊接、 固定纳米 线的过程中对纳米线造成的污染和损伤， 亟待研发一种新型的纳米线的移动、 转移和固定方法， 为后续的扫描电镜和透射电镜原位纳米力学测试和表征带来 便利， 从而消除传统的聚焦离子束和电子束对纳米线的操作带来的污染和损伤 技术问题
[0004] 本发明采用一种微米直径的锥形毛移动和转移纳米线的方法， 用锥形毛实现纳 米线的移动和转移。
问题的解决方案
技术解决方案
[0005] 本发明的技术方案：
[0006] 一种微米直径的锥形毛移动和转移纳米线的方法， 纳米线的直径为 60-150 nm ， 锥形毛为人的眉毛、 眼睫毛、 狼毫和羊毫， 直径范围为 1-100 μηι， 尖端曲率半 径为 0.8-3 μηι， 长度为 4-10 mm。 用火烧掉透射电镜用的铜网上的塑料薄膜， 留 下铜网， 孔的直径为 50-100 μηι。 然后用超声后的铜网在超声分散纳米线的丙酮 液体中捞取纳米线。 将分布有纳米线的铜网和锥形毛分别放在两个不同的光学 显微镜的移动平台上， 实现锥形毛的毫米和微米级移动， 从而实现对纳米线的 移动和转移操作。 用锥形毛尖端蘸取一小滴导电银胶， 分别滴在纳米线的两端 ， 滴落后的导电银胶的半径为 4-8 μηι。 本发明提供一种利用两个光学显微镜的移 动平台， 用微米直径的锥形毛实现移动和转移纳米线的方法。
[0007] 纳米线的直径为 60-150 nm。 纳米线的直径超过 150 nm， 电子束很难穿透， 难 以获得原子尺度的高分辨透射电镜像； 纳米线的直径小于 60 nm， 在光学显微镜 下非常难操作和寻找。 选择纳米线的直径范围为 60-150 nm， 是考虑操作和原子 成像的综合结果。
[0008] 锥形毛为人的眉毛、 眼睫毛、 狼毫和羊毫， 直径范围为 1-100 μηι， 尖端曲率半 径为 0.8-3 μηι， 长度为 4-10 mm。 这四种材料均较为容易获得， 来自人体和毛笔 。 此外， 这些毛均为锥形， 对于操作纳米线非常有好处。 这四种毛的直径范围 为 1-100 μηι， 便于精确操作纳米线。 锥形毛易于在光学显微镜下斜插入到纳米线 的下部， 从而实现对纳米线的操作。 尖端曲率半径为 0.8-3 μηι， 对于利用锥形毛 和纳米线之间的静电引力非常有好处。 长度为 4-10 mm， 是为了使得锥形毛既有 一定的刚度， 又有柔韧性， 从而可以实现对纳米线的操作和转移。
[0009] 用火烧掉透射电镜用的铜网上的塑料薄膜， 留下铜网， 孔的直径为 50-100 μηι 。 为了转移纳米线， 就要使得锥形毛能够插入到纳米线的下部， 从而对纳米线 进行较为精确的移动、 提取、 转移操作， 因此需要去掉铜网上面覆盖的一层塑 料膜。 由于塑料膜很薄， 用火烧的方法能迅速去除塑料膜， 而且非常干净， 不 会对后续的操作造成污染。 由于纳米线的长度一般在微米量级， 因此选择孔径 为 50-100 μηι， 既能放置纳米线， 又不至于调入铜网的孔中。
[0010] 将纳米线在丙酮中进行超声分散， 吋间为 l-2 min。 丙酮具有较强的去污和分散 能力， 加上超声的作用， 效果会更明显， 因此用丙酮进行超声分散， 吋间较短 即可， 为 l-2 min。
[0011] 用镊子夹住铜网， 在丙酮溶液中超声 0.5-1 min， 然后用超声后的铜网在超声分 散纳米线的丙酮液体中捞取纳米线， 丙酮溶液蒸发后， 纳米线分布于铜网表面 。 用镊子夹住铜网在丙酮中进行超声清洗， 是为了清洗掉火烧铜网留下的痕迹 和污染。 用清洗后的铜网在分散纳米线的丙酮溶液中捞取纳米线， 是为了在铜 网上留下较多的均匀分布的纳米线。
[0012] 将分布有纳米线的铜网和锥形毛分别放在两个不同的光学显微镜的移动平台上 ， 锥形毛用导电银胶粘接于锥形杆的尖端， 另外的扁平端用导电银胶固定于显 微镜的移动平台上。 铜网放在光学显微镜的移动平台上， 利用光学显微镜寻找 和操作纳米线。 锥形毛与另一台光学显微镜的移动平台相连， 主要是利用另一 台光学显微镜的移动平台的宏观和微观的移动功能， 实现对纳米线的精确移动 、 提取、 转移等操作， 利用另一台光学显微镜的毫米和微米级组合移动功能实 现对纳米线的操作。
[0013] 利用光学显微镜的移动平台的粗调和微调旋钮， 实现锥形毛的毫米和微米级移 动， 从而实现对纳米线的移动和转移操作。 光学显微镜的粗调旋钮， 主要是实 现锥形毛的毫米级的快速移动， 微调旋钮实现锥形毛的微米级移动， 从而实现 对纳米线的操作。
[0014] 在铜网放置的光学显微镜中观察纳米线， 借助锥形毛进行移动和转移操作， 用 扫描电镜或者透射电镜用的原位力学测试微装置替换铜网， 将纳米线放到微装 置的合适位置， 用锥形毛尖端蘸取一小滴导电银胶， 分别滴在纳米线的两端， 滴落后的导电银胶的半径为 4-8 μηι。 在光学显微镜下找到纳米线， 并进行聚焦， 利用另一台光学显微镜的移动平台， 实现锥形毛斜着插入到纳米线的下部， 将 纳米线挑起， 使得纳米线与铜网的静电引力变小， 然后在锥形毛与纳米线的静 电引力下， 将纳米线提取离幵铜网表面。 将铜网换成扫描电镜或者透射电镜的 原位力学测试的微装置， 将纳米线放在拉伸部位处。 用锥形毛的尖端蘸一滴导 电银胶， 轻轻滴在纳米线的一端， 蘸另一小滴， 滴在另一端。 导电银胶滴下后 的尺寸半径为 4-8 μηι。 既不污染纳米线， 同吋固化后具有良好的粘接强度。
[0015] 在空气中放置 2-4 h， 导电银胶固化， 即可进行扫描电镜或者透射电镜的原位纳 米力学测试与表征。 在空气中静置 2-4 h， 导电银胶固化， 纳米线被牢牢固定在 微装置上， 而且没有物理和化学气相沉积的污染和离子束以及电子束造成的对 纳米线的损伤， 即可进行扫描电镜或者透射电镜原位纳米力学测试与表征。 发明的有益效果
有益效果
[0016] 本发明的效果和益处是采用微米直径的锥形毛实现了纳米线的移动和转移， 并 用导电银胶固定， 避免了传统聚焦离子束和电子束对纳米线的操作造成的污染 和损伤。
对附图的简要说明
附图说明
[0017] 图 1是微米直径的锥形羊毫的扫描电镜显微照片。
[0018] 图 2是微米直径的锥形狼毫扫描电镜显微照片。
[0019] 图 3是用狼毫在光学显微镜下转移纳米线的光学显微照片。
本发明的实施方式
[0020] 以下结合附图和技术方案， 进一步说明本发明的具体实施方式。
[0021] 一种微米直径的锥形毛移动和转移纳米线的方法， 用锥形毛实现纳米线的移动 和转移， 其特征在于：
[0022] ( 1) 纳米线的直径为 60-150 nm;
[0023] (2) 锥形毛为人的眉毛、 眼睫毛、 狼毫和羊毫， 直径范围为 1-100 μηι， 尖端 曲率半径为 0.8-3 μηι, 长度为 4-10 mm;
[0024] (3) 用火烧掉透射电镜用的铜网上的塑料薄膜， 留下铜网， 孔的直径为 50-10
0 μηΐ; [0025] (4) 将纳米线在丙酮中进行超声分散， 吋间为 l-2 min;
[0026] (5) 用镊子夹住铜网， 在丙酮溶液中超声 0.5-1 min， 然后用超声后的铜网在 超声分散纳米线的丙酮液体中捞取纳米线， 丙酮溶液蒸发后， 纳米线分布于铜 网表面；
[0027] (6) 将分布有纳米线的铜网和锥形毛分别放在两个不同的光学显微镜的移动 平台上， 锥形毛用导电银胶粘接于锥形杆的尖端， 另外的扁平端用导电银胶固 定于显微镜的移动平台上；
[0028] (7) 利用光学显微镜的移动平台的粗调和微调旋钮， 实现锥形毛的毫米和微 米级移动， 从而实现对纳米线的移动和转移操作；
[0029] (8) 在铜网放置的光学显微镜中观察纳米线， 借助锥形毛进行移动和转移操 作， 用扫描电镜或者透射电镜用的原位力学测试微装置替换铜网， 将纳米线放 到微装置的测试位置， 用锥形毛尖端蘸取一小滴导电银胶， 分别滴在纳米线的 两端， 滴落后的导电银胶的半径为 4-8 μηι;
[0030] (9) 在空气中放置 2-4 h， 导电银胶固化， 即可进行扫描电镜或者透射电镜的 原位纳米力学测试与表征。
实施例
[0031] 选择直径为 80-100 nm的碳化硅单晶纳米线作为操作对象， 分别用人的眉毛， 羊毫毛笔的羊毫， 如图 1所示， 狼毫毛笔的狼毫， 如图 2所示， 作为微米直径的 锥形毛。 这三种锥形毛的直径范围为 2-100 μηι， 尖端曲率半径为 1-3
μηι， 长度为 6-10 mm。 选择 200目的带有塑料薄膜的透射电镜样品制备用的直径 为 3
mm的铜网， 用打火机烧掉铜网上的塑料薄膜， 露出铜网上的通孔， 直径为 90-10 Ο μηι。 将纳米线在丙酮中超声分散， 吋间为 1.5-2 min。 用镊子夹住去膜后的铜网 ， 在丙酮溶液中超声清洗 40-60 s,去掉火烧后的痕迹和污染。 然后取出铜网， 用 镊子夹住铜网在丙酮分散的纳米线溶液中捞取纳米线， 在空气中放置， 丙酮蒸 发后， 纳米线分布于铜网上。 将带有纳米线的铜网放置在光学显微镜的移动平 台上。 将微米直径的锥形毛用导电银胶粘接于锥形塑料细长杆的尖端， 另一端 用火烧成扁平端， 用导电银胶固定在另一台光学显微镜的移动平台上。 在光学 显微镜的目镜中找到纳米线， 并调焦清晰。 用另一台光学显微镜的移动平台， 结合粗调和微调， 实现微米直径的锥形毛的毫米和微米级移动， 逐渐用锥形毛 斜插入纳米线的下部。 插入后， 用移动平台的微调旋钮实现锥形毛的微米级向 上移动， 将纳米线一端挑起， 离幵铜网。 纳米线一端挑起后， 其与铜网静电引 力随着接触面积的减小而逐步减小， 最后只有一端的一点接触， 继续上移锥形 毛， 纳米线即离幵铜网， 如图 3所示， 从而实现了微米直径的锥形毛对纳米线的 移动、 提取和转移操作。 纳米线离幵铜网后， 将扫描电镜或者透射电镜的测试 用的微装置， 放在铜网的位置。 在光学显微镜下聚焦， 使得纳米线所要放置的 位置清晰。 然后用另一台光学显微镜的移动平台， 用微调旋钮实现纳米线的微 米级的逐步逼近， 将纳米线的一端放置在微装置的测试位置， 然后逐步利用微 移动的微调功能， 放平纳米线， 这样随着纳米线与微装置的接触面积逐步增大 ， 两者间的静电引力也逐步增大， 放平后， 即可后移锥形毛， 使得锥形毛与纳 米线脱离， 从而实现了纳米线的转移操作。 随后， 滴一滴导电银胶在微装置的 移动平台上， 用锥形毛的尖端蘸取一小滴导电银胶， 用移动平台准确滴到纳米 线的一端， 使得导电银胶与纳米线的一端接触， 从而使得导电银胶滴落。 重复 这个操作， 在纳米线的另一端滴落一小滴导电银胶。 滴落后的导电银胶的半径 为 5-8 μηι。 导电银胶在空气中静置 3-4 h， 实现固化。
将固化后的微装置装入 PI 95 TEM Picolndenter透射电镜原位力学测试系统中， 将系统插入 FEI Tecnai F20场发射透射电镜中， 进行透射电镜纳米力学拉伸测试 ， 透射电镜的操作电压为 200 kV。 采用位移控制模式， 加载速率是 lO nm/s , 对 纳米线施加拉伸载荷。 纳米线的直径为 80-100 nm， 拉断吋的断裂力为 110 μΝ， 纳米线的断裂强度为 12 GPa。 纳米线的动态拉伸过程被原位力学测试系统录下 视频， 从中可以提取出断裂吋的关键原子尺度高分辨透射电镜像， 从而实现了 纳米线的透射电镜原位力学拉伸测试和表征实验。

Claims

权利要求书 [权利要求 1] 一种微米直径的锥形毛移动和转移纳米线的方法， 用锥形毛实现纳米 线的移动和转移， 其特征在于：
( 1) 纳米线的直径为 60-150 nm;
(2) 锥形毛为人的眉毛、 眼睫毛、 狼毫和羊毫， 直径为 1-100 μηι， 尖端曲率半径为 0.8-3 μηι， 长度为 4-10 mm;
(3) 去掉透射电镜用的铜网上的塑料薄膜， 留下铜网， 铜网上的孔 的直径为 50- 100 μηΐ;
(4) 将纳米线在丙酮中进行超声分散， 吋间为 l-2 min;
(5) 用镊子夹住铜网， 在丙酮溶液中超声 0.5-1 min， 然后用超声后 的铜网在超声分散纳米线的丙酮液体中捞取纳米线， 丙酮溶液蒸发后 ， 纳米线分布于铜网表面；
(6) 将分布有纳米线的铜网和锥形毛分别放在两个不同的光学显微 镜的移动平台上； 锥形毛用导电银胶粘接于锥形杆的尖端， 扁平端用 导电银胶固定于显微镜的移动平台上；
(7) 利用光学显微镜的移动平台的粗调和微调旋钮， 实现锥形毛的 毫米和微米级移动， 从而实现对纳米线的移动和转移操作；
(8) 在铜网放置的光学显微镜中观察纳米线， 借助锥形毛进行移动 和转移操作， 用扫描电镜或透射电镜用的原位力学测试微装置替换铜 网， 将纳米线放到原位力学测试微装置的测试位置， 用锥形毛尖端蘸 取导电银胶， 分别滴在纳米线的两端， 滴落后的导电银胶的半径为 4- 8 μηΐ;
(9) 在空气中放置 2-4 h， 导电银胶固化， 即进行扫描电镜或透射电 镜的原位纳米力学测试与表征。
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CN101039870A (zh) * 2004-10-14 2007-09-19 国际商业机器公司 可编程分子操纵处理
CN101949957A (zh) * 2010-09-10 2011-01-19 东华大学 一种采用半导体纳米线作为探针精确移动纳米线的方法
WO2016112171A1 (en) * 2015-01-07 2016-07-14 Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Tip enhanced laser assisted sample transfer for biomolecule mass spectrometry
CN107219243A (zh) * 2017-05-05 2017-09-29 大连理工大学 一种透射电镜原位纳米力学拉伸测试样品粘接方法

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