CN106771376B - A method for preparing atomic force microscope tip - Google Patents
A method for preparing atomic force microscope tip Download PDFInfo
- Publication number
- CN106771376B CN106771376B CN201710127121.6A CN201710127121A CN106771376B CN 106771376 B CN106771376 B CN 106771376B CN 201710127121 A CN201710127121 A CN 201710127121A CN 106771376 B CN106771376 B CN 106771376B
- Authority
- CN
- China
- Prior art keywords
- sample
- needle tip
- tip
- feedback system
- thorn
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 54
- 230000005684 electric field Effects 0.000 claims abstract description 12
- 238000013459 approach Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims description 17
- 230000010363 phase shift Effects 0.000 claims description 11
- 238000010079 rubber tapping Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims 1
- 238000007689 inspection Methods 0.000 claims 1
- 239000000523 sample Substances 0.000 description 93
- 238000010586 diagram Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000002156 adsorbate Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000617527 Ennomos alniaria Species 0.000 description 1
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002717 carbon nanostructure Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000313 electron-beam-induced deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000007737 ion beam deposition Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
Classifications
-
- 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
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Length Measuring Devices With Unspecified Measuring Means (AREA)
Abstract
本发明涉及原子力显微镜领域，一种制备原子力显微镜针尖的方法，实现所述方法的装置主要包括电阻、悬臂、针尖、样品、样品与针尖之间的间隙处、刺状物、电流反馈系统、光电反馈系统、压电驱动器、电源U，由电源U、电阻、电流反馈系统、悬臂、针尖、间隙处和样品连接组成电流反馈回路，悬臂与样品之间连接有光电反馈系统，电流反馈系统电连接压电驱动器，压电驱动器连接悬臂，针尖固定于悬臂下面，样品位于针尖的下方，样品与针尖之间为间隙处，当针尖逼近样品表面停留时，开启电源U能在间隙处形成一高电场，从而使得针尖的前端生长出几百纳米长的刺状物，利用第一样品和第二样品先后使用，生长出垂直于样品表面的符合实验要求的刺状物。
The invention relates to the field of atomic force microscope, a method for preparing the tip of an atomic force microscope, the device for realizing the method mainly includes a resistor, a cantilever, a tip, a sample, a gap between the sample and the tip, a thorn, a current feedback system, a photoelectric Feedback system, piezoelectric driver, power supply U, the current feedback loop is composed of power supply U, resistance, current feedback system, cantilever, needle tip, gap and sample connection, a photoelectric feedback system is connected between the cantilever and the sample, and the current feedback system is electrically connected Piezoelectric driver, the piezoelectric driver is connected to the cantilever, the needle tip is fixed under the cantilever, the sample is located under the needle tip, and there is a gap between the sample and the needle tip. When the needle tip approaches the surface of the sample and stays, turn on the power supply U to form a high electric field in the gap , so that the front end of the needle tip grows a thorn with a length of several hundred nanometers, and the first sample and the second sample are used successively to grow a thorn that is perpendicular to the surface of the sample and meets the experimental requirements.
Description
技术领域technical field
本发明涉及一种纳米结构的原子力显微镜针尖的制备领域，特别是能够在常温大气条件下直接在原来的针尖上制备符合实验需求的针尖、制备方法简单有效的一种制备原子力显微镜针尖的方法。The invention relates to the field of preparation of a nanostructured atomic force microscope tip, in particular to a simple and effective method for preparing an atomic force microscope tip that can directly prepare a tip that meets the experimental requirements on the original tip under normal temperature and atmospheric conditions.
背景技术Background technique
原子力显微镜(Atomic Force Microscope，AFM)是利用原子、分子间的相互作用力来观察物体表面微观形貌的仪器，其基本原理为：通过将一根纳米级尺度的探针固定在可灵敏操控的微米级弹性悬臂上，当针尖与样品非常接近时，针尖尖端的原子与样品表面原子之间的作用力会使所述微米级弹性悬臂弯曲，偏离原来的位置；同时，有一束激光照射到悬臂上，并反射到激光监测器中，弹性悬臂的弯曲导致了激光的偏向，由此得到光斑的偏移量，根据该偏移量以及其振动频率、作为反馈信号，经过特定的反馈系统输入计算机中，计算机能够以此来重建三维图像，从而获得样品表面的形貌及成分信息。Atomic Force Microscope (AFM) is an instrument that uses the interaction force between atoms and molecules to observe the microscopic topography of the object surface. The basic principle is: by fixing a nanoscale probe on a sensitively manipulated On the micron-scale elastic cantilever, when the needle tip is very close to the sample, the force between the atoms at the tip of the needle tip and the surface atoms of the sample will cause the micron-scale elastic cantilever to bend and deviate from its original position; at the same time, a beam of laser light hits the cantilever and reflected into the laser monitor, the bending of the elastic cantilever leads to the deflection of the laser, thus obtaining the offset of the spot, according to the offset and its vibration frequency, as a feedback signal, it is input into the computer through a specific feedback system In this process, the computer can use this to reconstruct the three-dimensional image, so as to obtain the topography and composition information of the sample surface.
原子力显微镜可以在不同模式下工作，这些模式主要有接触模式、轻敲模式、侧向力模式等。在接触模式中，针尖从样品表面划过，从悬臂的偏转可以直接分析出表面的高度图。在轻敲模式或侧向力模式中，有信号源以某个外部参考频率驱动悬臂振动，在扫描样品的过程中悬臂振动的频率会改变，振幅、相位和共振等参数与探针和样品间的作用力相关，这些参数相对信号源提供的外部参考的振动的变化可以反映样品的性质。其中，作为轻敲模式的一项扩展技术，相移模式通过检测驱动悬臂探针振动的信号源的相位角与悬臂探针实际振动的相位角之差(即信号源和实际振动的相移)的变化来成像。AFM can work in different modes, these modes mainly include contact mode, tapping mode, lateral force mode and so on. In contact mode, the tip is drawn across the sample surface, and a height map of the surface can be directly analyzed from the deflection of the cantilever. In tapping mode or lateral force mode, a signal source drives the cantilever to vibrate at some external reference frequency, the frequency of the cantilever vibration changes during the scanning of the sample, and parameters such as amplitude, phase and resonance are related to the distance between the probe and the sample. The change of these parameters relative to the vibration of the external reference provided by the signal source can reflect the properties of the sample. Among them, as an extended technology of the tapping mode, the phase shift mode detects the difference between the phase angle of the signal source driving the vibration of the cantilever probe and the phase angle of the actual vibration of the cantilever probe (that is, the phase shift between the signal source and the actual vibration) changes to image.
原子力显微镜(AFM)相对于扫描电子显微镜优势明显，第一，原子力显微镜能够提供真正的三维表面图，而扫描电子显微镜只能提供二维图像；第二，原子力显微镜不需要对样品的任何特殊处理，如镀铜或碳，这种处理对样品会造成不可逆转的伤害；第三，原子力显微镜在常压下甚至在液体环境下都可以良好工作，可以用来研究生物宏观分子，甚至活的生物组织，就像盲人摸象一样，在物体的表面慢慢抚摸，原子的形状能够很直观的表现。而电子显微镜需要运行在高真空条件下。Atomic force microscopy (AFM) has obvious advantages over scanning electron microscopy. First, AFM can provide a true three-dimensional surface map, while scanning electron microscopy can only provide two-dimensional images. Second, AFM does not require any special treatment of the sample , such as copper or carbon, this treatment will cause irreversible damage to the sample; third, the atomic force microscope can work well under normal pressure or even in a liquid environment, and can be used to study biological macromolecules, even living organisms Tissue is like a blind man touching an elephant, slowly stroking the surface of an object, and the shape of atoms can be expressed intuitively. Electron microscopes, on the other hand, need to operate under high vacuum conditions.
原子力显微镜针尖通常是硅材料Si或Si3N4制成，根据不同的需要其外部镀有不同的金属层。传统的原子力显微镜探针针尖受到磨损时，其曲率半径会变大、扫描得到样品的图像分辨率会降低，因此原子力显微镜的成像受其探针的影响非常之大，因此原子力显微镜针尖是消耗品，在使用过程中尤其是高精度实验后极易损耗，更换针尖既费时又费力，且耽误实验进度，目前硅针尖尖端生长刺状物的方法有：离子或电子束沉积、聚焦离子束刻蚀、化学气相沉积碳纳米管或金属纳米管等。但是这些方法的缺陷有：一是成本较高，二是需要在真空腔内进行并对真空的要求高，三是不能在原位进行，需要中断实验进程，使得不能方便及时地更换新的针尖，延误实验进度，所述一种制备原子力显微镜针尖的方法能解决这一问题。The tip of atomic force microscope is usually made of silicon material Si or Si 3 N 4 , and its exterior is coated with different metal layers according to different needs. When the probe tip of the traditional atomic force microscope is worn, its radius of curvature will become larger, and the image resolution of the scanned sample will be reduced. Therefore, the imaging of the atomic force microscope is greatly affected by its probe, so the tip of the atomic force microscope is a consumable , in the process of use, especially after high-precision experiments, it is very easy to wear and tear. It is time-consuming and laborious to replace the needle tip, and it will delay the progress of the experiment. At present, the methods for growing thorns on the tip of the silicon needle tip include: ion or electron beam deposition, focused ion beam etching , chemical vapor deposition of carbon nanotubes or metal nanotubes, etc. However, the defects of these methods are as follows: first, the cost is high; second, it needs to be carried out in a vacuum chamber and has high requirements for vacuum; third, it cannot be carried out in situ, and the experimental process needs to be interrupted, making it impossible to replace the new needle tip in a convenient and timely manner. , to delay the progress of the experiment, the method for preparing the tip of the atomic force microscope can solve this problem.
发明内容Contents of the invention
为了解决上述问题，本发明通过增设电流反馈系统控制针尖与样品之间的距离，利用第一样品和第二样品先后使用，生长出垂直于样品表面的符合实验要求的刺状物，能够直接在大气条件下进行操作并显著地提高原子力显微镜针尖的尖锐程度，不用更换针尖既能够在原位制备符合实验需求的针尖，既不需要一个充入了某些保护气体的密闭腔体，也不需要借助更复杂的制备工具，方法有效。In order to solve the above problems, the present invention controls the distance between the needle tip and the sample by adding a current feedback system, uses the first sample and the second sample successively, grows a thorn that meets the experimental requirements perpendicular to the sample surface, and can directly Operate under atmospheric conditions and significantly improve the sharpness of the tip of the atomic force microscope. The tip that meets the experimental requirements can be prepared in situ without changing the tip, and neither a closed cavity filled with some protective gas nor Requires more sophisticated preparation tools to be effective.
本发明所采用的技术方案是：The technical scheme adopted in the present invention is:
实现所述方法的装置主要包括电阻、悬臂、针尖、样品、样品与针尖之间的间隙处、刺状物、电流反馈系统、光电反馈系统、压电驱动器、电源U，由电源U、电阻、电流反馈系统、悬臂、针尖、间隙处和样品连接组成电流反馈回路，电源U的负极连接电阻，正极连接样品，电阻为20G欧姆镇流电阻，悬臂与样品之间连接有光电反馈系统，电流反馈系统电连接压电驱动器，压电驱动器连接悬臂，针尖固定于悬臂下面，样品位于针尖的下方，样品与针尖之间为间隙处，当针尖逼近样品表面停留时，开启电源U能在间隙处形成一高电场，从而使得针尖的前端生长出几百纳米长的刺状物；当电流反馈系统开启时，能够探测到针尖与样品之间的微弱电流，并将其与预先设定的电流值比较，电流反馈系统反馈信号输入压电驱动器，并能够控制针尖与样品之间的距离，针尖是半导体材料或具有金属镀膜，样品是导体金属镍或钴或金或铂的薄膜、半导体材料Si或GaAs，The device for realizing the method mainly includes a resistor, a cantilever, a needle tip, a sample, a gap between the sample and the needle tip, a thorn, a current feedback system, a photoelectric feedback system, a piezoelectric driver, a power supply U, and the power supply U, a resistor, The current feedback system, the cantilever, the needle tip, the gap and the sample connection form a current feedback loop. The negative pole of the power supply U is connected to the resistor, and the positive pole is connected to the sample. The resistance is a 20G ohm ballast resistor. The system is electrically connected to the piezoelectric driver, the piezoelectric driver is connected to the cantilever, the needle tip is fixed under the cantilever, the sample is located under the needle tip, and there is a gap between the sample and the needle tip. A high electric field, so that the tip of the tip grows hundreds of nanometers long thorns; when the current feedback system is turned on, it can detect the weak current between the tip and the sample, and compare it with the preset current value , the feedback signal of the current feedback system is input to the piezoelectric driver, and the distance between the needle tip and the sample can be controlled. The needle tip is a semiconductor material or has a metal coating, and the sample is a thin film of conductor metal nickel or cobalt or gold or platinum, semiconductor material Si or GaAs ,
样品有第一样品和第二样品，第一样品表面具有以阵列排布的倒锥体凹陷坑，每隔100nm有一个直径为100nm，深度为30nm的凹陷坑，第二样品表面具有以阵列排布的突起，每隔20nm有一个高为20nm，直径为10nm的突起；The samples include a first sample and a second sample. The surface of the first sample has inverted cone depressions arranged in an array. Every 100nm there is a depression with a diameter of 100nm and a depth of 30nm. The surface of the second sample has The protrusions arranged in an array have a protrusion with a height of 20 nm and a diameter of 10 nm every 20 nm;
一种制备原子力显微镜针尖的方法，包括：初次生长刺状物的方法、使刺状物生长得更长的方法、生长垂直于样品表面的刺状物的方法和检验针尖是否尖锐的方法，A method for preparing the tip of an atomic force microscope, comprising: a method for initially growing a thorn, a method for making the thorn grow longer, a method for growing a thorn perpendicular to the surface of a sample, and a method for checking whether the needle tip is sharp,
初次生长刺状物的方法如下：选用第一样品，使用原子力显微镜轻敲模式将针尖水平移动至凹陷坑上方位置，关闭光电反馈系统，开启电流反馈系统，电流设定值为1pA，接下来开启电源U，并使电源U的输出电压在2秒时间内从0增加到V1，其中20V＜V1＜90V，保持2秒后关闭电源U，完成初次生长刺状物过程，如果在关闭电源U之前先在5秒内将输出电压值从原设定值降至0，能够使刺状物与针尖结合得更牢固；The method of growing thorns for the first time is as follows: select the first sample, use the AFM tapping mode to move the needle tip horizontally to the position above the depression, turn off the photoelectric feedback system, turn on the current feedback system, and set the current value to 1pA, then Turn on the power supply U, and make the output voltage of the power supply U increase from 0 to V 1 within 2 seconds, where 20V<V 1 <90V, keep the power supply U for 2 seconds and then turn off the power supply U to complete the initial process of growing thorns. Before the power supply U, reduce the output voltage value from the original set value to 0 within 5 seconds, which can make the thorn and the needle tip more firmly combined;
使刺状物生长得更长的方法如下：完成初次生长刺状物过程后，使用原子力显微镜轻敲模式将针尖水平移动到另一个凹陷坑上方，然后重复初次生长刺状物过程，能够使刺状物生长得更长；The method to make the spine grow longer is as follows: After the initial growth spine process is completed, use the AFM tapping mode to move the needle tip horizontally over another depression pit, and then repeat the initial growth spine process, which can make the spine The shape grows longer;
生长垂直于样品表面的刺状物的方法如下：初次生长刺状物过程结束后，将第一样品换成第二样品，原子力显微镜以轻敲模式工作，开启光电反馈系统，关闭电流反馈系统，再开启电源U，并使电源U的输出电压保持在10V到20V之间的一个值，然后针尖开始扫描样品，由于针尖与第二样品表面的突起有轻微接触，从而能使原先生长的方向任意性较大的刺状物略改变方向，并生长出垂直于样品表面的符合实验要求的刺状物；The method of growing spines perpendicular to the surface of the sample is as follows: After the initial growth process of spines is completed, the first sample is replaced with the second sample, the atomic force microscope is operated in tapping mode, the photoelectric feedback system is turned on, and the current feedback system is turned off , and then turn on the power supply U, and keep the output voltage of the power supply U at a value between 10V and 20V, and then the needle tip starts to scan the sample. Since the needle tip has a slight contact with the protrusion on the second sample surface, the original growth direction can be changed. Arbitrary large thorns change direction slightly, and grow thorns perpendicular to the surface of the sample that meet the experimental requirements;
检验针尖是否尖锐的方法如下：使用另一个表面较为平整的样品，原子力显微镜以相移模式工作，设一个初始振幅为A0，扫描距离为15nm，设定值为0.6A0，如果在平整的表面相移为负，则认为是尖锐的针尖，能达到实验要求；如果相移不为负，需要重复加电源U以在间隙处形成一个高电场的过程，直至生长出一个垂直于样品表面的符合实验要求的刺状物。The method to check whether the needle tip is sharp is as follows: Use another sample with a relatively flat surface, and the atomic force microscope works in phase shift mode. Set an initial amplitude as A0, a scanning distance of 15nm, and a set value of 0.6A0. If the phase shift is negative, it is considered to be a sharp needle tip, which can meet the experimental requirements; if the phase shift is not negative, it is necessary to repeat the process of applying the power source U to form a high electric field at the gap until a conforming experimental point perpendicular to the sample surface is grown. The spines required.
第二样品表面的突起若是向同一朝向倾斜，采用该第二样品进行单一方向行扫描，且使扫描的方向与该突起倾斜的朝向相对时能够取得更好效果，一行扫描结束后将针尖抬离第二样品，返回到行起点进行下一行的扫描，依次重复。If the protrusions on the surface of the second sample are inclined in the same direction, use the second sample to scan in a single direction, and make the scanning direction opposite to the inclined direction of the protrusions to achieve better results. Lift the needle tip away from the For the second sample, return to the start of the row to scan the next row, and repeat in turn.
刺状物形成原理：电场能在样品表面附近的一个相对受约束的区域保持一个较大的值，此时样品与针尖上均会形成纳米结构生长，空间上，因为其中一个电极是针尖的尖端，该电场是不均匀的，样品表面的吸附物在不均匀电场中的转移，并分解，后又自组装，从而使得针尖上形成刺状物。刺状物组成材料的来源是吸附在针尖和样品表面的大气环境中的碳氢化合物的吸附物，组成吸附物的碳氢化合物的分解，在针尖和样品表面形成碳纳米结构。通过施加电源，在样品和针尖上都会有沉积，多数情况下，沉积下来的材料是碳，由吸附的碳氢化合物分解而来。The principle of thorn formation: the electric field can maintain a large value in a relatively restricted area near the sample surface. At this time, nanostructure growth will be formed on both the sample and the needle tip, spatially, because one of the electrodes is the tip of the needle tip , the electric field is inhomogeneous, and the adsorbate on the surface of the sample transfers in the inhomogeneous electric field, decomposes, and then self-assembles, thereby forming a thorn on the needle tip. The source of the constituent material of the thorn is the adsorbate of hydrocarbons in the atmospheric environment adsorbed on the needle tip and the surface of the sample, and the decomposition of the hydrocarbons constituting the adsorbate forms a carbon nanostructure on the needle tip and the surface of the sample. By applying power, deposits are deposited on both the sample and the tip, and in most cases, the deposited material is carbon, which results from the decomposition of adsorbed hydrocarbons.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明通过增设电流反馈系统控制针尖与样品之间的距离，利用第一样品和第二样品先后使用，生长出垂直于样品表面的符合实验要求的刺状物，通过在样品与针尖之间的间隙处加上一个高电场，能够直接在大气条件下制备针尖并显著地提高原子力显微镜针尖的尖锐程度，既不需要在真空腔内进行，也不需要借助更复杂的制备工具，方法有效，能够方便及时地更换新的符合实验需求的针尖，进而继续进行实验，加快实验进程，且成本低。In the present invention, the distance between the needle tip and the sample is controlled by adding a current feedback system, and the first sample and the second sample are used successively to grow a thorn that is perpendicular to the surface of the sample and meets the experimental requirements. Adding a high electric field to the gap can directly prepare the needle tip under atmospheric conditions and significantly improve the sharpness of the AFM needle tip. It does not need to be carried out in a vacuum chamber, nor does it need to use more complicated preparation tools. The method is effective. It is possible to conveniently and timely replace a new needle tip that meets the experimental requirements, and then continue the experiment, speed up the experimental process, and have low cost.
附图说明Description of drawings
下面结合本发明的图形进一步说明：Below in conjunction with figure of the present invention further illustrate:
图1是本发明示意图；Fig. 1 is a schematic diagram of the present invention;
图2是样品与针尖之间的间隙处的放大示意图；Figure 2 is an enlarged schematic view of the gap between the sample and the needle tip;
图3是第一样品放大示意图；Fig. 3 is the enlarged schematic view of the first sample;
图4是第二样品之一放大示意图；Fig. 4 is an enlarged schematic view of one of the second samples;
图5是第二样品之二放大示意图。Fig. 5 is a second enlarged schematic view of the second sample.
图中，1.电阻，2.悬臂，3.针尖，4.样品，5.间隙处，6.刺状物，7.电流反馈系统，8.光电反馈系统，9.压电驱动器。In the figure, 1. Resistor, 2. Cantilever, 3. Needle tip, 4. Sample, 5. Gap, 6. Spike, 7. Current feedback system, 8. Photoelectric feedback system, 9. Piezoelectric driver.
具体实施方式Detailed ways
如图1是本发明示意图，实现所述方法的装置主要包括电阻(1)、悬臂(2)、针尖(3)、样品(4)、样品与针尖之间的间隙处(5)、刺状物(6)、电流反馈系统(7)、光电反馈系统(8)、压电驱动器(9)、电源U，由电源U、电阻(1)、电流反馈系统(7)、悬臂(2)、针尖(3)、间隙处(5)和样品(4)连接组成电流反馈回路，电源U的负极连接电阻(1)，正极连接样品(4)，电阻(1)为20G欧姆镇流电阻，以能防止电流反馈回路中电流过大，悬臂(2)与样品(4)之间连接有光电反馈系统(8)，电流反馈系统(7)电连接压电驱动器(9)，压电驱动器(9)连接悬臂(2)，针尖(3)固定于悬臂(2)下面，样品(4)位于针尖(3)的下方，样品(4)与针尖(3)之间为间隙处(5)；当电流反馈系统(7)开启时，能够探测到针尖(3)与样品(4)之间的微弱电流，并将其与预先设定的电流值比较，电流反馈系统(7)反馈信号输入压电驱动器(9)，并能够控制针尖(3)与样品(4)之间的距离，针尖(3)是半导体材料或具有金属镀膜，样品(4)是导体金属镍或钴或金或铂的薄膜、半导体材料Si或GaAs，样品(4)有第一样品和第二样品。Figure 1 is a schematic diagram of the present invention, the device for realizing the method mainly includes a resistor (1), a cantilever (2), a needle point (3), a sample (4), a gap between the sample and the needle point (5), a thorn Object (6), current feedback system (7), photoelectric feedback system (8), piezoelectric driver (9), power supply U, consisting of power supply U, resistance (1), current feedback system (7), cantilever (2), The needle tip (3), the gap (5) and the sample (4) are connected to form a current feedback loop. The negative electrode of the power supply U is connected to the resistor (1), and the positive electrode is connected to the sample (4). The resistor (1) is a 20G ohm ballast resistor, with It can prevent excessive current in the current feedback loop, a photoelectric feedback system (8) is connected between the cantilever (2) and the sample (4), the current feedback system (7) is electrically connected to the piezoelectric driver (9), and the piezoelectric driver (9 ) is connected to the cantilever (2), the needle point (3) is fixed under the cantilever (2), the sample (4) is located below the needle point (3), and there is a gap (5) between the sample (4) and the needle point (3); When the current feedback system (7) is turned on, it can detect the weak current between the needle tip (3) and the sample (4), and compare it with the preset current value, and the feedback signal of the current feedback system (7) is input to the piezoelectric The driver (9) can control the distance between the needle point (3) and the sample (4), the needle point (3) is a semiconductor material or has a metal coating, and the sample (4) is a film of conductor metal nickel or cobalt or gold or platinum 1. The semiconductor material Si or GaAs, the sample (4) has a first sample and a second sample.
如图2是样品与针尖之间的间隙处的放大示意图，当针尖(3)逼近样品(4)表面停留时，开启电源U能在间隙处(5)形成一高电场，从而使得针尖(3)的前端生长出几百纳米长的刺状物(6)。Figure 2 is an enlarged schematic diagram of the gap between the sample and the needle tip. When the needle tip (3) approaches the surface of the sample (4) and stops, turning on the power supply U can form a high electric field at the gap (5), thereby making the needle tip (3) ) grows hundreds of nanometer-long spines (6).
如图3是第一样品放大示意图，第一样品表面具有以阵列排布的倒锥体凹陷坑，每隔100nm有一个直径为100nm，深度为30nm的凹陷坑。Figure 3 is an enlarged schematic view of the first sample. The surface of the first sample has inverted cone depressions arranged in an array, and every 100 nm there is a depression with a diameter of 100 nm and a depth of 30 nm.
如图4是第二样品之一放大示意图，第二样品表面具有以阵列排布的突起，每隔20nm有一个高为20nm，直径为10nm的突起。Figure 4 is an enlarged schematic view of one of the second samples. The surface of the second sample has protrusions arranged in an array, and every 20 nm there is a protrusion with a height of 20 nm and a diameter of 10 nm.
如图5是第二样品之二放大示意图，第二样品表面的突起若是向同一朝向倾斜，采用该第二样品进行单一方向行扫描，且使扫描的方向与该突起倾斜的朝向相对时能够取得更好效果，一行扫描结束后将针尖(3)抬离第二样品，返回到行起点进行下一行的扫描，依次重复。Figure 5 is an enlarged schematic diagram of the second sample. If the protrusions on the surface of the second sample are inclined in the same direction, the second sample can be used to scan in a single direction, and the scanning direction is opposite to the inclined direction of the protrusions. For better results, lift the needle tip (3) away from the second sample after one row of scanning, return to the starting point of the row to scan the next row, and repeat in sequence.
一种制备原子力显微镜针尖的方法，包括初次生长刺状物(6)的方法、使刺状物(6)生长得更长的方法、生长垂直于样品(4)表面的刺状物(6)的方法和检验针尖(3)是否尖锐的方法，A method for preparing an atomic force microscope tip, comprising a method for growing a thorn (6) for the first time, a method for growing the thorn (6) longer, and growing a thorn (6) perpendicular to the surface of a sample (4) method and the method for checking whether the needle point (3) is sharp,
初次生长刺状物(6)的方法如下：选用第一样品，使用原子力显微镜轻敲模式将针尖(3)水平移动至凹陷坑上方位置，关闭光电反馈系统(8)，开启电流反馈系统(7)，电流设定值为1pA，接下来开启电源U，并使电源U的输出电压在2秒时间内从0增加到V1，其中20V＜V1＜90V，保持2秒后关闭电源U，完成初次生长刺状物(6)过程，如果在关闭电源U之前先在5秒内将输出电压值从原设定值降至0，能够使刺状物(6)与针尖(3)结合得更牢固，相比平整的样品(4)表面，针尖(3)处于凹陷坑位置时聚焦电场更强，更容易产生刺状物(6)；The method for initial growth of thorns (6) is as follows: select the first sample, use the atomic force microscope to tap the mode to move the needle tip (3) horizontally to the position above the depression, turn off the photoelectric feedback system (8), and turn on the current feedback system ( 7), the current setting value is 1pA, then turn on the power supply U, and make the output voltage of the power supply U increase from 0 to V 1 within 2 seconds, where 20V<V 1 <90V, keep 2 seconds and then turn off the power supply U , to complete the process of growing the thorn (6) for the first time, if the output voltage value is reduced from the original set value to 0 within 5 seconds before turning off the power supply U, the thorn (6) can be combined with the needle tip (3) Compared with the flat sample (4) surface, the focused electric field is stronger when the needle tip (3) is in the pit position, and it is easier to produce thorns (6);
使刺状物(6)生长得更长的方法如下：完成初次生长刺状物(6)过程后，使用原子力显微镜轻敲模式将针尖(3)水平移动到另一个凹陷坑上方，然后重复初次生长刺状物(6)过程，能够使刺状物(6)生长得更长；The method of making the spine (6) grow longer is as follows: After the initial growth of the spine (6) is completed, use the AFM tapping mode to move the needle tip (3) horizontally over another depression, and then repeat the initial The process of growing the thorn (6) can make the thorn (6) grow longer;
生长垂直于样品(4)表面的刺状物(6)的方法如下：初次生长刺状物(6)过程结束后，将第一样品换成第二样品，原子力显微镜以轻敲模式工作，开启光电反馈系统(8)，关闭电流反馈系统(7)，再开启电源U，并使电源U的输出电压保持在10V到20V之间的一个值，然后针尖(3)开始扫描样品(4)，由于针尖(3)与第二样品表面的突起有轻微接触，从而能使原先生长的方向任意性较大的刺状物(6)略改变方向，并生长出垂直于样品(4)表面的符合实验要求的刺状物(6)；The method for growing the thorns (6) perpendicular to the surface of the sample (4) is as follows: after the process of growing the thorns (6) for the first time is finished, the first sample is replaced with the second sample, and the atomic force microscope works in a tapping mode, Turn on the photoelectric feedback system (8), turn off the current feedback system (7), then turn on the power supply U, and keep the output voltage of the power supply U at a value between 10V and 20V, and then the needle tip (3) starts to scan the sample (4) , due to the slight contact between the needle tip (3) and the protrusion on the surface of the second sample, the original growth direction of the thorn (6) with a relatively random direction can be slightly changed, and grow perpendicular to the surface of the sample (4) Spikes (6) meeting the experimental requirements;
检验针尖(3)是否尖锐的方法如下：使用另一个表面较为平整的样品，原子力显微镜以相移模式工作，设一个初始振幅为A0，扫描距离为15nm，设定值为0.6A0，如果在平整的表面相移为负，则认为是尖锐的针尖(3)，能达到实验要求；如果相移不为负，需要重复加电源U以在间隙处(5)形成一个高电场的过程，直至生长出一个垂直于样品(4)表面的符合实验要求的刺状物(6)。The method to check whether the needle tip (3) is sharp is as follows: Use another sample with a relatively flat surface, and the atomic force microscope works in phase shift mode. Set an initial amplitude as A0, a scanning distance of 15nm, and a set value of 0.6A0. If the phase shift of the surface is negative, it is considered to be a sharp needle tip (3), which can meet the experimental requirements; if the phase shift is not negative, it is necessary to repeat the process of applying the power source U to form a high electric field at the gap (5) until the growth Produce a thorn (6) that is perpendicular to the surface of the sample (4) and meets the experimental requirements.
以上所述的，仅为本发明的较佳实施例，并非用以限定本发明的范围，本发明的上述实施例还可以做出各种变化。凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰，皆落入本发明专利的权利要求保护范围。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various changes can be made to the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and description of the application for the present invention fall within the protection scope of the claims of the patent of the present invention.
本发明未详尽描述的均为常规技术内容。What is not described in detail in the present invention is conventional technical content.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127121.6A CN106771376B (en) | 2017-02-24 | 2017-02-24 | A method for preparing atomic force microscope tip |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127121.6A CN106771376B (en) | 2017-02-24 | 2017-02-24 | A method for preparing atomic force microscope tip |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106771376A CN106771376A (en) | 2017-05-31 |
| CN106771376B true CN106771376B (en) | 2023-08-29 |
Family
ID=58962346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710127121.6A Active CN106771376B (en) | 2017-02-24 | 2017-02-24 | A method for preparing atomic force microscope tip |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106771376B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110967527A (en) * | 2018-09-30 | 2020-04-07 | 中国计量科学研究院 | Preparation device for scanning probe tip |
| CN109507454A (en) * | 2018-11-07 | 2019-03-22 | 中北大学 | A kind of preparation method measuring crystal face active force atomic-force microscope needle-tip |
| CN110658360B (en) * | 2019-09-16 | 2020-08-18 | 浙江大学 | Method and device for preparing superfine atomic force microscope metal probe |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6075585A (en) * | 1994-04-12 | 2000-06-13 | The Board Of Trustees Of The Leland Stanford, Jr. University | Vibrating probe for a scanning probe microscope |
| KR20040081597A (en) * | 2003-03-14 | 2004-09-22 | 한국기계연구원 | Processing method of carbon nanotube |
| JP2006260780A (en) * | 2005-03-15 | 2006-09-28 | Japan Atomic Energy Agency | Ionization method of needle-like sample surface layer by using both ultrashort pulse laser convergence and high voltage application, and analytical method of needle-like sample surface layer using it |
| CN101630536A (en) * | 2008-07-18 | 2010-01-20 | 中国科学院沈阳自动化研究所 | Preparation method of carbon nanotube AFM probe based on electromagnetic field |
| CN102012439A (en) * | 2010-10-12 | 2011-04-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing silicon-based self-sharpening AFM (antifrictional metal) probe |
| CN102768292A (en) * | 2012-07-25 | 2012-11-07 | 天津大学 | Ultrahigh vacuum fast scanning microscopy method based on carbon nanotube probe |
| CN104071746A (en) * | 2014-07-21 | 2014-10-01 | 厦门大学 | Preparation method of metal probe applicable to AFM (Atomic Force Microscope) |
| CN106226560A (en) * | 2016-08-02 | 2016-12-14 | 河南师范大学 | The PSTM of solid-state potential barrier needle point contact mode |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7735147B2 (en) * | 2005-10-13 | 2010-06-08 | The Regents Of The University Of California | Probe system comprising an electric-field-aligned probe tip and method for fabricating the same |
-
2017
- 2017-02-24 CN CN201710127121.6A patent/CN106771376B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6075585A (en) * | 1994-04-12 | 2000-06-13 | The Board Of Trustees Of The Leland Stanford, Jr. University | Vibrating probe for a scanning probe microscope |
| KR20040081597A (en) * | 2003-03-14 | 2004-09-22 | 한국기계연구원 | Processing method of carbon nanotube |
| JP2006260780A (en) * | 2005-03-15 | 2006-09-28 | Japan Atomic Energy Agency | Ionization method of needle-like sample surface layer by using both ultrashort pulse laser convergence and high voltage application, and analytical method of needle-like sample surface layer using it |
| CN101630536A (en) * | 2008-07-18 | 2010-01-20 | 中国科学院沈阳自动化研究所 | Preparation method of carbon nanotube AFM probe based on electromagnetic field |
| CN102012439A (en) * | 2010-10-12 | 2011-04-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing silicon-based self-sharpening AFM (antifrictional metal) probe |
| CN102768292A (en) * | 2012-07-25 | 2012-11-07 | 天津大学 | Ultrahigh vacuum fast scanning microscopy method based on carbon nanotube probe |
| CN104071746A (en) * | 2014-07-21 | 2014-10-01 | 厦门大学 | Preparation method of metal probe applicable to AFM (Atomic Force Microscope) |
| CN106226560A (en) * | 2016-08-02 | 2016-12-14 | 河南师范大学 | The PSTM of solid-state potential barrier needle point contact mode |
Non-Patent Citations (1)
| Title |
|---|
| 用于扫描探针电子能谱仪的 扫描隧道显微镜;郦盟;真空科学与技术学报;第第36卷卷(第第36卷期);第1320-1324页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106771376A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tseng | Advancements and challenges in development of atomic force microscopy for nanofabrication | |
| US7441444B2 (en) | AFM cantilevers and methods for making and using same | |
| CN110658360B (en) | Method and device for preparing superfine atomic force microscope metal probe | |
| CN106771376B (en) | A method for preparing atomic force microscope tip | |
| EP3047335B1 (en) | Scanning probe nanolithography system and method | |
| CN206671365U (en) | A kind of sample for being used to prepare atomic-force microscope needle-tip | |
| CN101630536B (en) | Method for preparing carbon nano-tube AFM probe based on electromagnetic field | |
| CN103336149B (en) | Based on atomic force microscopy micro-cantilever and the application of nano particle dot array Quantum Transport | |
| CN106383250A (en) | Scanning tunneling microscope probe with use of two-dimensional atomic crystal material | |
| CN206540931U (en) | A kind of current feedback circuit for preparing atomic-force microscope needle-tip | |
| CN104880578B (en) | The measuring method of driver move distance in a kind of device and its application method and the device for measuring micro-nano metallic fiber surface topography | |
| Pumarol et al. | Controlled deposition of gold nanodots using non-contact atomic force microscopy | |
| Foubert et al. | Mechanical and optical manipulation of porphyrin rings at the submicrometre scale | |
| US10352963B2 (en) | Dynamic sweep-plow microcantilever device and methods of use | |
| JP2002214112A (en) | Scanning probe microscope | |
| Kim et al. | 100× 100 thermopiezoelectric cantilever array for SPM nano-data-storage application | |
| CN1654943A (en) | A nano-scale processing method for conducting indentations | |
| CN105510637A (en) | Micro-nano thermoelectric in-situ detection device and method based on scanning probe microscope | |
| Magonov et al. | Advancing characterization of materials with atomic force microscopy-based electric techniques | |
| Ruiz-Perez et al. | Scanning Probe Microscopy: Tipping | |
| RU2426190C1 (en) | Method of producing nano-sized structures | |
| Ruiz-Perez et al. | Scanning Probe Microscopy: Tipping the Path Toward Atomic Visions | |
| US20240175896A1 (en) | Method for Producing a Substrate Comprising Multiple Tips for Scanning Probe Microscopy | |
| Micro et al. | Graphene | |
| CN201083670Y (en) | Transmission electron microscope one-dimensional nano material test slide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Jin Xiongjun Inventor after: Zhao Yongjian Inventor after: Fang Xiaohua Inventor after: Zhang Xiangping Inventor before: Zhao Yongjian Inventor before: Fang Xiaohua Inventor before: Zhang Xiangping |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |