摘要
三维原子探针是一种先进的材料表征设备,可用来分析样品在纳米尺度空间中化学元素的分布及含量。为克服目前人工制备三维原子探针纳米针尖样品效率低、质量差的问题,该文设计了金属纳米针尖制备专用装置,分为粗抛、清洗和精抛三个部分,通过电控系统实现制备过程的自动化。使用该装置分别制备了5种金属材料(Al、Al基合金、Mo、Fe基合金、Ti合金)的纳米针尖,制备出的纳米针尖质量高,且制备效率高、成功率高。该装置可用于实验室纳米针尖的制备,也可用于材料分析与测试相关领域的实验教学工作。
[Objective]Three-dimensional atom probe tomography(APT)is an advanced material characterization technique that can enable the distribution and quantitative analyses of each element in a sample in the nanoscale space,but it has strict requirements regarding the sample size.At present,the preparation of samples for APT mainly relies on manual operation,which not only has low efficiency but also a low success rate.In view of the above problems,this paper develops a metal nano needle tip sample preparation device.[Methods]It is divided into three functional modules for rough polishing,cleaning,and fine polishing according to the principle of nano needle tip sample preparation,and the automation of the preparation process is realized using an electronic control system.Additionally,it is easy to operate.Step 1:Turn on the main power supply,manually adjust the arm up and down to move a sample away from the working table or rotate the stepper motor box to make the sample chuck upward so as to facilitate the clamping of metal samples,and then reset clamping after this process is completed,and finally adjust the height of the arm to make the tip of the metal sample close to the surface of the electrolyte.Step 2:Connect the positive pole of the DC power supply to the metal sample and the negative pole to the platinum wire ring,and submerge the metal wire ring in the electrolyte so that the electrolyte acts as the negative pole for the electrochemical reaction.Step 3:Turn on the helm switch to start calibration;the electrolyte is placed in the metal samples directly below,and,at the same time,turn on the stepper motor switch so that the metal samples begin to undergo up and down reciprocating motion,beginning the rough polishing stage.After a beep sound,turn off the stepper motor switch and wait for the metal samples to rotate on the left side of the place to turn on the pump switch to start cleaning.After cleaning,the metal sample automatically returns to the vertical position.Repeat the third step several times until the front end of the needle tip sample is not visible to the naked eye,which means the end of the rough polishing stage.Step 4:Automatically rotate to the horizontal position,starting the fine polishing stage.Disconnect the negative electrode from the rough polishing platinum wire ring and connect it to the fine polishing platinum wire ring,drop the electrolyte on the platinum wire ring to form an electrolyte film,and start the fine polishing stage.Step 5:Remove the nano needle tip sample after preparation,disconnect the power supply,rotate the sample chuck to the vertical position,and adjust the arm height to the initial state.[Results and Conclusions]Microscopic observation shows that this device can prepare high-quality nanometer tips with high efficiency and a high success rate and can basically prepare samples that meet the requirements in one go.For the preparation of nano-tip of different materials,the device parameters can be standardized and accurately controlled by setting them appropriately.Avoid the impact of human factors on the success rate of sample preparation and save manpower and material resources.The proposed device can be used to prepare nano needle tip samples in laboratories,reduce the initial sample preparation time,and improve experimental efficiency as well as for experimental teaching in the field of material analysis and testing.
作者
赵磊
吴雨菲
刘吉梓
吴森达
祖莉
吴志林
ZHAO Lei;WU Yufei;LIU Jizi;WU Senda;ZU Li;WU Zhiin(School of Mechanical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China;School of Materials Science and Engineering,Nanjing University of Science and Technology,Nanjing 210094,China;Military Representative Bureau in Nanjing,General Armament Department of PLA,Nanjing 210007,China)
出处
《实验技术与管理》
北大核心
2025年第5期169-173,共5页
Experimental Technology and Management
基金
教育部产学合作协同育人项目(220604598164438)
江苏省高校“青蓝工程”(苏教师函[2023]27号)。
关键词
三维原子探针
纳米针尖
电化学抛光
专用制样装置
three-dimensional atom probe
nano-tip
electrochemical polishing
specialized sample preparation device
