CN114392985B - A method of cleaning near-local electrodes of three-dimensional atom probes using Tesla coils - Google Patents
A method of cleaning near-local electrodes of three-dimensional atom probes using Tesla coils Download PDFInfo
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- 238000011086 high cleaning Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
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Abstract
本发明属于材料领域，具体的说是一种利用特斯拉线圈清理三维原子探针近局域电极的方法，该方法包括如下步骤：S1：首先将三维原子探针近局域电极从三维原子探针设备上取下，然后使用夹持器械将三维原子探针近局域电极固定在清理工作台上；S2：其次将特斯拉线圈尖端对准近局域电极微孔，留有1‑3mm的距离；S3：检查特斯拉线圈、三维原子探针近局域电极正常后，给特斯拉线圈接通电源；通过方法步骤的设计,实现了利用特斯拉线圈尖端产生高压电火花对三维原子探针近局域电极表面脏污进行熔融处理，实现表面高效率清洁的功能，解决了聚焦离子束清洁成本高降低使用寿命的问题，提高了三维原子探针近局域电极清洁的效率。
The invention belongs to the field of materials. Specifically, it is a method for cleaning the near-local electrode of a three-dimensional atom probe using a Tesla coil. The method includes the following steps: S1: First, remove the near-local electrode of the three-dimensional atom probe from the three-dimensional atom probe. Remove it from the probe equipment, and then use a clamping instrument to fix the near-local electrode of the three-dimensional atom probe on the cleaning workbench; S2: Next, align the tip of the Tesla coil with the microhole of the near-local electrode, leaving 1- 3mm distance; S3: After checking that the Tesla coil and the near-local electrode of the three-dimensional atom probe are normal, power on the Tesla coil; through the design of the method steps, the tip of the Tesla coil is used to generate high-voltage electricity. The spark melts the dirt on the surface of the near-local electrode of the three-dimensional atom probe to achieve high-efficiency cleaning of the surface. It solves the problem of high cost and reduced service life of focused ion beam cleaning, and improves the cleaning of the near-local electrode of the three-dimensional atom probe. s efficiency.
Description
技术领域Technical field
本发明涉及材料领域，具体是一种利用特斯拉线圈清理三维原子探针近局域电极的方法。The invention relates to the field of materials, specifically a method for cleaning the near-local electrode of a three-dimensional atom probe using a Tesla coil.
背景技术Background technique
三维原子探针是一种材料科学领域的分析仪器，其具备原子级空间分辨率，可用于分析材料中的三维微观特征。三维原子探针技术是基于“场蒸发”原理，在针尖样品上施加电压或激光脉冲，将针尖表面原子蒸发成离子通过近局域电极并收集，过程中要求电极表面清洁度高，才可以获得高质量的数据。然而，在收据采集过程中，三维原子探针针尖样品往往会发生断裂，粘附在电极表面上，造成近局域电极表面污染，影响数据质量。The three-dimensional atom probe is an analytical instrument in the field of materials science. It has atomic-level spatial resolution and can be used to analyze three-dimensional microscopic features in materials. Three-dimensional atom probe technology is based on the principle of "field evaporation". A voltage or laser pulse is applied to the tip sample to evaporate the atoms on the tip surface into ions and collect them through a near-local electrode. The process requires high electrode surface cleanliness to obtain High quality data. However, during the collection process, the three-dimensional atom probe tip sample often breaks and adheres to the electrode surface, causing near-local electrode surface contamination and affecting data quality.
特斯拉线圈是串联谐振变压器，可以获得上百万伏特的高频电压，可以通过特斯拉线圈人工制造出电火花进行表面脏污熔融处理。现有的利用聚焦离子束清理三维原子探针近局域电极的方法对电极内环的形状缺陷清理效果较好，但却会大大降低近局域电极的使用寿命同时清理成本较大；因此，针对上述问题提出一种利用特斯拉线圈清理三维原子探针近局域电极的方法。The Tesla coil is a series resonant transformer that can obtain high-frequency voltages of millions of volts. It can artificially create electric sparks through the Tesla coil to melt surface contamination. The existing method of using focused ion beam to clean the near-local electrode of a three-dimensional atom probe has a good cleaning effect on the shape defects of the inner ring of the electrode, but it will greatly reduce the service life of the near-local electrode and increase the cleaning cost; therefore, In order to solve the above problems, a method of using Tesla coil to clean the near-local electrode of a three-dimensional atom probe is proposed.
发明内容Contents of the invention
为了弥补现有技术的不足，解决现有的利用聚焦离子束清理三维原子探针近局域电极的方法具有降低电极使用寿命的缺点,清理成本较大的问题，本发明提出一种利用特斯拉线圈清理三维原子探针近局域电极的方法。In order to make up for the shortcomings of the existing technology and solve the problems that the existing method of cleaning the near-local electrode of the three-dimensional atom probe using focused ion beam has the shortcomings of reducing the service life of the electrode and high cleaning cost, the present invention proposes a method using Tes A method of cleaning the near-local electrode of a three-dimensional atom probe by pulling a coil.
本发明解决其技术问题所采用的技术方案是：本发明所述的一种利用特斯拉线圈清理三维原子探针近局域电极的方法，包括该方法包括如下步骤：The technical solution adopted by the present invention to solve the technical problem is: a method of using a Tesla coil to clean the near-local electrode of a three-dimensional atom probe according to the present invention, including the following steps:
S1：首先将三维原子探针近局域电极从三维原子探针设备上取下，然后使用夹持器械将三维原子探针近局域电极固定在清理工作台上；S1: First, remove the near-local electrode of the three-dimensional atom probe from the three-dimensional atom probe device, and then use a clamping instrument to fix the near-local electrode of the three-dimensional atom probe on the cleaning workbench;
S2：其次将特斯拉线圈尖端对准近局域电极微孔，留有1-3mm的距离；S2: Secondly, align the tip of the Tesla coil with the microhole of the near-local electrode, leaving a distance of 1-3mm;
S3：检查特斯拉线圈、三维原子探针近局域电极正常后，给特斯拉线圈接通电源；S3: After checking that the Tesla coil and the near-local electrode of the three-dimensional atom probe are normal, power on the Tesla coil;
S4：将特斯拉线圈旋转出电火花，对近局域电极表面清理10-20秒，随后给特斯拉线圈断电；S4: Rotate the Tesla coil to generate electric sparks, clean the near-local electrode surface for 10-20 seconds, and then cut off the power to the Tesla coil;
S5：将清理后的三维原子探针近局域电极放入扫描电镜下观察，观察其表面是否被清理干净，是否存在凸出的针尖等脏污，清理干净后放入三维原子探针设备中；S5: Place the cleaned near-local electrode of the three-dimensional atom probe under a scanning electron microscope to observe whether the surface is cleaned and whether there are protruding needle tips and other dirt. After cleaning, place it into the three-dimensional atom probe equipment. ;
S6：将清理干净后的三维原子探针近局域电极放入三维原子探针预真空舱中加热10-20分钟后，进行等离子清洗7-9小时，清理完毕后三维原子探针近局域电极可正常使用。S6: Place the cleaned near-local electrode of the three-dimensional atom probe into the pre-vacuum chamber of the three-dimensional atom probe and heat it for 10-20 minutes, then perform plasma cleaning for 7-9 hours. After cleaning, the near-local electrode of the three-dimensional atom probe is The electrodes can be used normally.
优选的，所述S2中的特斯拉线圈使用230V的交流电进行工作。Preferably, the Tesla coil in S2 uses 230V alternating current to work.
优选的，所述S2中的特斯拉线圈使用0.18A大小的电流工作。Preferably, the Tesla coil in S2 operates with a current of 0.18A.
优选的，所述S2中的三维原子探针近局域电极垂直于特斯拉线圈固定。Preferably, the near-local electrode of the three-dimensional atom probe in S2 is fixed perpendicular to the Tesla coil.
优选的，所述S1中的清理工作台的上方安装有水平隔板。Preferably, a horizontal partition is installed above the cleaning workbench in S1.
本发明的有益之处在于：The benefits of the present invention are:
1.本发明通过方法步骤的设计,实现了利用特斯拉线圈产生高压电火花对三维原子探针近局域电极表面脏污进行熔融处理，实现电极表面高效率清洁的功能，解决了聚焦离子束清洁成本高、降低电极使用寿命的问题，提高了三维原子探针近局域电极清洁的效率；1. Through the design of the method steps, the present invention realizes the function of using the Tesla coil to generate high-voltage electric sparks to melt the dirt on the near-local electrode surface of the three-dimensional atom probe, achieving high-efficiency cleaning of the electrode surface, and solving the problem of focusing. The problems of high ion beam cleaning cost and reduced electrode service life have improved the efficiency of near-local electrode cleaning of three-dimensional atom probes;
2.本发明通过方法步骤的设计,实现了利用三维原子探针预真空舱中等离子清洗去除三维原子探针近局域电极表面被高频电火花清理的颗粒物的功能，解决了超高频电压清理不彻底的问题，提高了三维原子探针近局域电极的清洁效果及清洁效率。2. Through the design of the method steps, the present invention realizes the function of using plasma cleaning in the pre-vacuum chamber of the three-dimensional atom probe to remove the particles cleaned by high-frequency electric sparks on the near-local electrode surface of the three-dimensional atom probe, and solves the problem of ultra-high frequency voltage The problem of incomplete cleaning is improved, and the cleaning effect and cleaning efficiency of the near-local electrode of the three-dimensional atom probe are improved.
附图说明Description of the drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其它的附图。In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings in the following description are only These are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without exerting any creative effort.
图1为本发明的清理三维原子探针近局域电极的方法步骤示意图；Figure 1 is a schematic diagram of the steps of the method for cleaning the near-local electrode of a three-dimensional atom probe according to the present invention;
图2为本发明的三维原子探针近局域电极清理前后的示意图；Figure 2 is a schematic diagram of the near-local electrode of the three-dimensional atom probe of the present invention before and after cleaning;
图3为本发明的三维原子探针近局域电极清理前后的扫描电镜图。Figure 3 is a scanning electron microscope image of the near-local electrode of the three-dimensional atom probe of the present invention before and after cleaning.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
实施例一Embodiment 1
请参阅图1-3所示，一种利用特斯拉线圈清理三维原子探针近局域电极的方法，该方法包括如下步骤：Please refer to Figure 1-3, a method of cleaning the near-local electrode of a three-dimensional atom probe using a Tesla coil. The method includes the following steps:
S1：首先将三维原子探针近局域电极从三维原子探针设备上取下，然后使用夹持器械将三维原子探针近局域电极固定在清理工作台上；S1: First, remove the near-local electrode of the three-dimensional atom probe from the three-dimensional atom probe device, and then use a clamping instrument to fix the near-local electrode of the three-dimensional atom probe on the cleaning workbench;
S2：其次将特斯拉线圈尖端对准近局域电极微孔，留有1mm的距离；S2: Secondly, align the tip of the Tesla coil with the microhole of the near-local electrode, leaving a distance of 1mm;
S3：检查特斯拉线圈、三维原子探针近局域电极正常后，给特斯拉线圈接通电源；S3: After checking that the Tesla coil and the near-local electrode of the three-dimensional atom probe are normal, power on the Tesla coil;
S4：将特斯拉线圈旋转出电火花，对近局域电极表面清理10秒，随后给特斯拉线圈断电；S4: Rotate the Tesla coil to produce electric sparks, clean the near-local electrode surface for 10 seconds, and then cut off the power to the Tesla coil;
S5：将清理后的三维原子探针近局域电极放入扫描电镜下观察，观察其表面是否被清理干净，是否存在凸出的针尖等脏污，清理干净后放入三维原子探针设备中；S5: Place the cleaned near-local electrode of the three-dimensional atom probe under a scanning electron microscope to observe whether the surface is cleaned and whether there are protruding needle tips and other dirt. After cleaning, place it into the three-dimensional atom probe equipment. ;
S6：将清理干净后的三维原子探针近局域电极放入三维原子探针预真空舱中加热10分钟后，进行等离子清洗7小时，清理完毕后三维原子探针近局域电极可正常使用。S6: Place the cleaned near-local electrode of the three-dimensional atom probe into the pre-vacuum chamber of the three-dimensional atom probe and heat it for 10 minutes, then perform plasma cleaning for 7 hours. After cleaning, the near-local electrode of the three-dimensional atom probe can be used normally. .
实施例二Embodiment 2
请参阅图1-3所示，一种利用特斯拉线圈清理三维原子探针近局域电极的方法，该方法包括如下步骤：Please refer to Figure 1-3, a method of cleaning the near-local electrode of a three-dimensional atom probe using a Tesla coil. The method includes the following steps:
S1：首先将三维原子探针近局域电极从三维原子探针设备上取下，然后使用夹持器械将三维原子探针近局域电极固定在清理工作台上；S1: First, remove the near-local electrode of the three-dimensional atom probe from the three-dimensional atom probe device, and then use a clamping instrument to fix the near-local electrode of the three-dimensional atom probe on the cleaning workbench;
S2：其次将特斯拉线圈尖端对准近局域电极微孔，留有2mm的距离；S2: Secondly, align the tip of the Tesla coil with the microhole of the near-local electrode, leaving a distance of 2mm;
S3：检查特斯拉线圈、三维原子探针近局域电极正常后，给特斯拉线圈接通电源；S3: After checking that the Tesla coil and the near-local electrode of the three-dimensional atom probe are normal, power on the Tesla coil;
S4：将特斯拉线圈旋转出电火花，对近局域电极表面清理15秒，随后给特斯拉线圈断电；S4: Rotate the Tesla coil to produce electric sparks, clean the near-local electrode surface for 15 seconds, and then cut off the power to the Tesla coil;
S5：将清理后的三维原子探针近局域电极放入扫描电镜下观察，观察其表面是否被清理干净，是否存在凸出的针尖等脏污，清理干净后放入三维原子探针设备中；S5: Place the cleaned near-local electrode of the three-dimensional atom probe under a scanning electron microscope to observe whether the surface is cleaned and whether there are protruding needle tips and other dirt. After cleaning, place it into the three-dimensional atom probe equipment. ;
S6：将清理干净后的三维原子探针近局域电极放入三维原子探针预真空舱中加热15分钟后，进行等离子清洗8小时，清理完毕后三维原子探针近局域电极可正常使用。S6: Put the cleaned near-local electrode of the three-dimensional atom probe into the pre-vacuum chamber of the three-dimensional atom probe and heat it for 15 minutes, then perform plasma cleaning for 8 hours. After cleaning, the near-local electrode of the three-dimensional atom probe can be used normally. .
实施例三Embodiment 3
请参阅图1-3所示，一种利用特斯拉线圈清理三维原子探针近局域电极的方法，该方法包括如下步骤：Please refer to Figure 1-3, a method of cleaning the near-local electrode of a three-dimensional atom probe using a Tesla coil. The method includes the following steps:
S1：首先将三维原子探针近局域电极从三维原子探针设备上取下，然后使用夹持器械将三维原子探针近局域电极固定在清理工作台上；S1: First, remove the near-local electrode of the three-dimensional atom probe from the three-dimensional atom probe device, and then use a clamping instrument to fix the near-local electrode of the three-dimensional atom probe on the cleaning workbench;
S2：其次将特斯拉线圈尖端对准近局域电极微孔，留有3mm的距离；S2: Secondly, align the tip of the Tesla coil with the microhole of the near-local electrode, leaving a distance of 3mm;
S3：检查特斯拉线圈、三维原子探针近局域电极正常后，给特斯拉线圈接通电源；S3: After checking that the Tesla coil and the near-local electrode of the three-dimensional atom probe are normal, power on the Tesla coil;
S4：将特斯拉线圈旋转出电火花，对近局域电极表面清理20秒，随后给特斯拉线圈断电；S4: Rotate the Tesla coil to produce electric sparks, clean the near-local electrode surface for 20 seconds, and then cut off the power to the Tesla coil;
S5：将清理后的三维原子探针近局域电极放入扫描电镜下观察，观察其表面是否被清理干净，是否存在凸出的针尖等脏污，清理干净后放入三维原子探针设备中；S5: Place the cleaned near-local electrode of the three-dimensional atom probe under a scanning electron microscope to observe whether the surface is cleaned and whether there are protruding needle tips and other dirt. After cleaning, place it into the three-dimensional atom probe equipment. ;
S6：将清理干净后的三维原子探针近局域电极放入三维原子探针预真空舱中加热20分钟后，进行等离子清洗9小时，清理完毕后三维原子探针近局域电极可正常使用。S6: Put the cleaned near-local electrode of the three-dimensional atom probe into the pre-vacuum chamber of the three-dimensional atom probe and heat it for 20 minutes, then perform plasma cleaning for 9 hours. After cleaning, the near-local electrode of the three-dimensional atom probe can be used normally. .
利用本实施例提供的方法对三个使用工作电压相同、使用时间相近的三维原子探针近局域电极清理试验三次，利用扫描电镜、三维原子探针设备分别观察并测量记录三维原子探针近局域电极表面污染颗粒的数量和清理后近局域电极的工作电压。The method provided in this embodiment was used to conduct three near-local electrode cleaning tests on three three-dimensional atom probes with the same working voltage and similar use time. The scanning electron microscope and three-dimensional atom probe equipment were used to observe and record the near-local electrodes of the three-dimensional atom probes respectively. The number of contamination particles on the surface of the local electrode and the working voltage of the near-local electrode after cleaning.
所得试验数据见表1。The experimental data obtained are shown in Table 1.
表1Table 1
通过实施例1-3可以看出，特斯拉线圈工作时间越长，三维原子探针近局域电极清理后的工作电压越高，三维原子探针近局域电极的清理效果越好。It can be seen from Examples 1-3 that the longer the working time of the Tesla coil, the higher the working voltage of the three-dimensional atom probe's near-local electrode after cleaning, and the better the cleaning effect of the three-dimensional atom probe's near-local electrode.
所述S2中的特斯拉线圈使用230V的交流电进行工作；工作时，通过恒定的电压，使得特斯拉线圈正常稳定工作，保证清洁效率效果。The Tesla coil in S2 uses 230V alternating current to work; during operation, a constant voltage is used to make the Tesla coil work normally and stably, ensuring cleaning efficiency.
所述S2中的特斯拉线圈使用0.18A大小的电流工作；工作时，通过恒定的电流，使得特斯拉线圈正常稳定工作，保证清洁效率效果。The Tesla coil in S2 works with a current of 0.18A; when working, a constant current is used to make the Tesla coil work normally and stably, ensuring cleaning efficiency.
所述S2中的三维原子探针近局域电极垂直于特斯拉线圈固定；工作时，通过三维原子探针近局域电极垂直于特斯拉线圈，使得电极的表面可以直接的与电火花接触，高效清洁电极表面。The near-local electrode of the three-dimensional atom probe in S2 is fixed perpendicularly to the Tesla coil; during operation, the near-local electrode of the three-dimensional atom probe is perpendicular to the Tesla coil, so that the surface of the electrode can directly interact with the electric spark. contact, cleaning the electrode surface efficiently.
所述S1中的清理工作台的上方安装有水平隔板；工作时，通过水平隔板可以隔绝电火花的位置，保证电火花的传递被限制。A horizontal partition is installed above the cleaning workbench in S1; during operation, the position of the electric spark can be isolated by the horizontal partition to ensure that the transmission of electric spark is restricted.
在本说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。In the description of this specification, reference to the terms "one embodiment," "example," "specific example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one aspect of the invention. in an embodiment or example. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above embodiments. The above embodiments and descriptions only illustrate the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have other aspects. Various changes and modifications are possible, which fall within the scope of the claimed invention.
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