CN1977159A - Method for manipulating microscopic particles and analyzing the composition thereof - Google Patents
Method for manipulating microscopic particles and analyzing the composition thereof Download PDFInfo
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- CN1977159A CN1977159A CNA2004800379489A CN200480037948A CN1977159A CN 1977159 A CN1977159 A CN 1977159A CN A2004800379489 A CNA2004800379489 A CN A2004800379489A CN 200480037948 A CN200480037948 A CN 200480037948A CN 1977159 A CN1977159 A CN 1977159A
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Abstract
Description
技术领域technical field
本发明涉及一种从样品表面,特别是半导体样品表面移走和分析微小颗粒的方法。The present invention relates to a method for removing and analyzing microscopic particles from the surface of a sample, especially a semiconductor sample.
背景技术Background technique
在半导体工业生产过程中,不可避免的颗粒污染将使产量降低。因为半导体业一直在集中精力极大地减小构图线宽的特征尺寸,所以,会使性能降低的颗粒最小尺寸也迅速减少。一般认为,合理估计半导体晶片上的“致命缺陷”尺寸应该大于最小特征尺寸的三分之一。In the production process of the semiconductor industry, the inevitable particle pollution will reduce the yield. As the semiconductor industry has been concentrating on dramatically reducing the feature size of patterned linewidths, the minimum particle size that degrades performance has also rapidly decreased. It is generally believed that a reasonable estimate of the size of a "fatal defect" on a semiconductor wafer should be greater than one third of the smallest feature size.
尽管半导体制造是在具有严格颗粒标准的洁净室中进行的,然而由于存在物体移动、人员进出、气体凝聚以及房间老化等原因,仍然不可避免地会造成污染。控制并除去这些颗粒是一项持续的过程。多数情况下,只有了解来源才能更好地除去颗粒。许多颗粒或缺陷很小,无法用普通的光学检查显微镜发现,因此需要采取分辨率更高的方法,使用如扫描电子显微镜(SAM)、透射电子显微镜(TEM)、扫描俄歇微探针(SAM)、或者聚焦离子束仪器等带电粒子显微镜。Although semiconductor manufacturing takes place in cleanrooms with stringent particle standards, contamination is unavoidable due to movement of objects, people entering and exiting, gas condensation, and room aging. Controlling and removing these particles is an ongoing process. In most cases, particle removal can only be improved by knowing the source. Many particles or defects are too small to be found with ordinary optical inspection microscopes, thus requiring higher resolution methods such as Scanning Electron Microscopy (SAM), Transmission Electron Microscopy (TEM), Scanning Auger Microprobe (SAM ), or charged particle microscopes such as focused ion beam instruments.
只根据颗粒的图像常常无法找到颗粒的来源,我们还需要更多的信息。基本成分在鉴别缺陷过程中有很高的应用价值。使用上述的带电粒子显微镜可以通过许多方法做这项工作。然而,多数分析方法受到颗粒周围背景信号的限制。Images of particles alone often fail to locate the source of the particles, and more information is needed. Basic components have high application value in the process of identifying defects. There are a number of ways to do this using the charged particle microscope described above. However, most analytical methods are limited by the background signal surrounding the particle.
生产能力也是半导体制造中的关键因素。现有的分析半导体晶片上的颗粒成分的方法通常需要将晶片从生产线上取下,然后使用下述方法进行离线分析,这将极大地降低产量。Throughput is also a key factor in semiconductor manufacturing. Existing methods for analyzing the composition of particles on semiconductor wafers typically require the wafers to be removed from the production line and then analyzed offline using the methods described below, which greatly reduces throughput.
由于颗粒与电子穿透深度的相对尺寸关系的变化,以及样品中周围材料特性的不同,使利用电子束对样品表面的颗粒进行鉴别变得非常复杂。随着电子束与大块固体材料相互作用,它将发散并充满水滴状的空间,且损失能量。一次光束与这个空间里的原子相互作用,产生该元素特有的低能量的俄歇电子和X射线。Particle identification on the surface of a sample using an electron beam is complicated by variations in the relative size relationship of the particle to the electron penetration depth, as well as by differences in the properties of the surrounding materials in the sample. As the electron beam interacts with the bulk of solid material, it diverges and fills the droplet-like space, losing energy. The primary beam interacts with the atoms in this space, producing low-energy Auger electrons and X-rays characteristic of that element.
产生的X射线取决于元素的原子序数、作用过程中电子的能量以及其它因素。当采用传统的能量分散型X射线分光光度法(EDS)鉴别未知的颗粒时,电子束的能量必须足够大,以在所有可能的相关元素上产生内壳层X射线,对于半导体业来说,这可能包含诸如钨等高原子序数的元素。可是,这个能量可能使穿透深度远大于所要鉴别的颗粒,以至于在样品表面产生X射线。这些X射线与从颗粒发出的信号相互干涉,使唯一地鉴别颗粒材料非常困难。传统的解决办法包括解析不同元素的X射线或降低激发电子束的能量。The X-rays produced depend on the atomic number of the element, the energy of the electrons involved, and other factors. When using traditional energy-dispersive X-ray spectrophotometry (EDS) to identify unknown particles, the energy of the electron beam must be large enough to generate inner-shell X-rays on all possible elements of interest. For the semiconductor industry, This may contain high atomic number elements such as tungsten. However, this energy may cause the penetration depth to be much greater than the particle to be identified, so that X-rays are generated at the sample surface. These X-rays interfere with the signal emanating from the particles, making unique identification of the particle material very difficult. Traditional solutions include resolving X-rays of different elements or lowering the energy of the excited electron beam.
例如,通过基准晶体或者波长分散型X射线光谱法(WDS)来测量X射线衍射的强度和衍射角可以检测并分析颗粒中由电子束产生的X射线。人们选定晶体原子间距以偏转(以高分辨率)给定能量的X射线,可使不同元素的X射线分开。此方法具有比EDS更高的能量分辨率,但是它的产量较低。另外,在多数情况下,颗粒可能与样品表面的成分一样,则这种方法就不能唯一地测定颗粒的成分。For example, measuring the intensity and diffraction angle of X-ray diffraction by reference crystals or wavelength-dispersive X-ray spectroscopy (WDS) can detect and analyze X-rays generated by electron beams in particles. The interatomic spacing of the crystal is chosen to deflect (with high resolution) X-rays of a given energy, allowing the X-rays of different elements to be separated. This method has higher energy resolution than EDS, but its yield is lower. In addition, in most cases, the particles may have the same composition as the sample surface, so this method cannot uniquely determine the composition of the particles.
其它的方法包括降低一次电子束的能量,以保证激活的空间小于所探测的颗粒的体积。一次电子束能量的降低使特征X射线具有较低的能量(M或L壳层X射线而不是K壳层)。传统冷却的基于半导体的探测器产生并收集电子空穴对,以测量电离辐射能量(根据不同的探测材料,每个电子空穴对产生几eV的能量)。降低X射线的能量,就减少了空穴对的数量,导致对颗粒材料的灵敏度降低。另外,这些探测器的分辨率由电子空穴产生过程中的统计量决定,降低探测到的X射线的能量通常会导致对所探测元素的鉴别不明确。已有技术中使用X射线微热量计方法来探测这些微弱的X射线信号,通过传递到探测器的热量而不是产生的电子空穴对进行测量。此方法可测量到很低的X射线能量,但是微热量计非常昂贵,需要进行复杂的冷却,并且与其它方法相比速度较慢。同时,电子束必须小于所探测颗粒的最小尺寸,因而此方法实际上无法探测小的、不对称的颗粒。Other methods include reducing the energy of the primary electron beam to ensure that the volume of activation is smaller than the volume of the particle being detected. The reduction in primary electron beam energy results in characteristic X-rays with lower energy (M or L shell X-rays instead of K shell). Conventional cooled semiconductor-based detectors generate and collect electron-hole pairs to measure ionizing radiation energy (a few eV per electron-hole pair, depending on the detector material). Reducing the energy of the X-rays reduces the number of hole pairs, resulting in reduced sensitivity to particulate materials. In addition, the resolution of these detectors is determined by the statistics of the electron-hole generation process, and reducing the energy of the detected X-rays often leads to ambiguous identification of the detected elements. Existing techniques use X-ray microcalorimetry methods to detect these weak X-ray signals, measuring the heat transferred to the detector rather than the electron-hole pairs generated. This method can measure very low X-ray energies, but microcalorimeters are expensive, require complex cooling, and are slow compared to other methods. Also, the electron beam must be smaller than the smallest particle size to be detected, so detection of small, asymmetric particles is practically impossible with this method.
扫描俄歇微探针分析也使用电子束照射所探测的颗粒,但是它不探测产生的X射线,而是探测材料原子发出的俄歇电子。这些俄歇电子从外壳发出,且具有相对较低的能量。来自材料的俄歇电子能量会产生一个表征材料中每种元素的构图,俄歇转换形态和精确的能量提供了材料中元素的化学结合信息(如相位和组成信息)。这些电子的逃离深度很小(几纳米),所以俄歇分析主要用于分析样品的表面。这有益于分析直径较小的颗粒(<10纳米)。如要分析较大的颗粒,可使用离子束溅射穿透颗粒来产生深度分布并进行周期性的测量,但是由于SAM中的离子研磨作用,不可避免地造成对周围样品的破坏,且其需要对颗粒所在位置周围的样品进行背景分析。对轻元素而言,俄歇分析通常比标准的EDS分析灵敏,使其更适合鉴别有机材料。然而,为了提高统计精度,通常需要用高电子束电流。这将放大热机漂移和样品电荷漂移的影响。这意味着以“点模式”操作SAM,电子束位于颗粒上,随着时间的延长,存在电子束点漂移到颗粒周围的样品上的风险。为了使电子束留在颗粒上,使用电子束的光栅图样可更耐漂移,但是来自周围材料的信号会对结果产生显著的污染。在任何情况下,俄歇分析结果的背景污染都是一个严重的问题,需要对周围材料的俄歇分析来唯一地识别出来自颗粒的信号。背景分析将降低产量并损坏样品。Scanning Auger microprobe analysis also uses an electron beam to irradiate the probed particles, but instead of detecting the X-rays produced, it detects the Auger electrons emitted by the atoms of the material. These Auger electrons are emitted from the outer shell and have relatively low energy. The Auger electron energy from the material produces a pattern that characterizes each element in the material, and the Auger transition morphology and precise energy provide chemical binding information (such as phase and composition information) of the elements in the material. The escape depth of these electrons is very small (a few nanometers), so Auger analysis is mainly used to analyze the surface of the sample. This is beneficial for the analysis of smaller diameter particles (<10 nm). If you want to analyze larger particles, you can use ion beam sputtering to penetrate the particles to generate depth distribution and measure periodically, but due to the ion grinding effect in SAM, it will inevitably cause damage to the surrounding samples, and it requires Background analysis is performed on the sample surrounding the particle location. For light elements, Auger analysis is generally more sensitive than standard EDS analysis, making it more suitable for identifying organic materials. However, in order to increase the statistical accuracy, it is usually necessary to use high beam currents. This will amplify the effects of thermomechanical drift and sample charge drift. This means that operating the SAM in 'spot mode', with the electron beam on the particle, runs the risk of the electron beam spot drifting onto the sample surrounding the particle over time. In order for the electron beam to stay on the particle, a raster pattern using the electron beam is more resistant to drift, but signals from surrounding materials can significantly contaminate the result. In any case, background contamination of Auger analysis results is a serious problem requiring Auger analysis of surrounding material to uniquely identify signals from particles. Background analysis will reduce yield and damage samples.
TEM通常用来分析表面上或其内部的颗粒。有许多方法可隔离要分析的颗粒,包括复制、提起或横切所探测的区域。这些方法都要破坏样品表面,并且要离线进行,因而会增加成本和延长循环周期。TEM is commonly used to analyze particles on or within surfaces. There are many ways to isolate particles for analysis, including duplicating, lifting, or transecting the area being probed. These methods destroy the sample surface and are performed off-line, thereby increasing cost and cycle time.
无论用EDS还是俄歇分析进行元素鉴别,将颗粒从第一样品表面移动到更容易控制的环境进行测试,都可以极大地提高成功的几率和产量。这个过程的关键部分是移动颗粒的方法。本发明公开了一种新方法,用它可以将所要探测的颗粒从样品表面取下,并传送到具有受控制的X射线或俄歇背景的第二样品表面,然后在那儿使用上文提及的各种方法进行电子束诱导的X射线或俄歇电子分析。这将不需要高空间分辨率的分析技术,但是,具有高空间分辨率的技术,例如在SEM和SAM分析中使用的EDS分析通常是优选的。能成功应用于对减少的或无干扰的背景上的颗粒进行分析的具有非高空间分辨率的技术例如包括X射线光电子能谱(XPS)和X射线荧光分析(XRF),这在唯一而明确的情况下非常有益。Whether using EDS or Auger analysis for elemental identification, moving particles from the surface of the first sample to a more easily controlled environment for testing can greatly improve the chances of success and yield. A key part of this process is the method of moving the particles. The present invention discloses a novel method by which the particles to be detected can be removed from the sample surface and transported to a second sample surface with a controlled X-ray or Auger background, where the above mentioned Various methods for electron beam induced X-ray or Auger electron analysis. This would not require high spatial resolution analytical techniques, however, techniques with high spatial resolution such as EDS analysis used in SEM and SAM analysis are usually preferred. Non-high spatial resolution techniques that can be successfully applied to the analysis of particles on a reduced or non-interfering background include, for example, X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence analysis (XRF), which are uniquely defined in situation is very beneficial.
这种用于颗粒处理和EDS X射线分析的方法可在现有的晶片制造设备上在线进行。使用现有的制造和检测设备的在线过程极大地降低了去除污染物的循环时间。SEM是晶片检测的常规方法,在SEM系统中使用电子束的分析方法比离线分析提高了产量。This method for particle processing and EDS X-ray analysis can be performed in-line on existing wafer fabrication equipment. The in-line process using existing manufacturing and testing equipment greatly reduces the cycle time for contaminant removal. SEM is a conventional method for wafer inspection, and analysis methods using electron beams in SEM systems increase throughput compared to off-line analysis.
尽管此项发明主要阐述处理和检测在半导体制造过程中成为污染物的颗粒的新方法的使用,但是读者应该注意到这里的“颗粒”一词也包括在其它环境下不是污染物的物质,如化学淀积物、生物材料或微机械机构。在后一种情况下,本申请所描述的处理的新方法可以用来处理这些物质,通常用于除电子束X射线或俄歇电子分析以外的其他目的。Although this invention primarily describes the use of new methods for handling and detecting particles that become pollutants in semiconductor manufacturing processes, readers should note that the term "particles" here also includes substances that are not pollutants in other contexts, such as Chemical deposits, biological materials or micromechanical mechanisms. In the latter case, the new method of processing described in this application can be used to treat these substances, often for purposes other than electron beam X-ray or Auger electron analysis.
附图说明Description of drawings
图1为将颗粒附着到微操纵器探针上并将颗粒移动到第二表面以进行分析的步骤。Figure 1 shows the steps of attaching a particle to a micromanipulator probe and moving the particle to a second surface for analysis.
图2为其它三种将颗粒附着到微操纵器探针上的方法。Figure 2 shows three other methods of attaching particles to micromanipulator probes.
图3为用可极化的微粒轰击以改变静电力的过程。Figure 3 shows the process of bombardment with polarizable particles to change the electrostatic force.
图4为同时观察颗粒并改变颗粒电荷状态的方法。Figure 4 is a method for simultaneously observing a particle and changing the charge state of the particle.
图5为将颗粒固定到第二表面以便进行分析的几种方法。Figure 5 shows several methods for immobilizing particles to a second surface for analysis.
图6为在将颗粒固定到微操纵器探针尖端上的同时对颗粒进行分析的过程。Figure 6 is a process of analyzing particles while immobilizing them on the micromanipulator probe tip.
图7为对移动到第二表面以进行分析的颗粒成分进行分析的过程。Fig. 7 is a process of analyzing particle components moved to a second surface for analysis.
发明内容Contents of the invention
本发明公开了一种分析固定在第一样品表面上的微小颗粒成分的方法。通常,颗粒是半导体生产系统中的污染物,而此方法不只限于在该环境下使用。此方法包括将微操纵器探针放到颗粒附近;将颗粒附着到探针上;从第一样品表面将探针和所附着的颗粒移走;将颗粒放置在第二样品表面上;通过能量分散型X射线法、俄歇微探针分析法或其它合适的分析技术来分析第二样品表面上的颗粒的成分。在分析过程中,第二表面相对第一表面的背景信号而言具有减弱的或无干涉的背景信号(在权利要求中申请人将减弱的或无干涉的背景信号称为“受控制”的背景信号)。本申请也公开了调整探针、颗粒和样品表面之间静电力和直流电压的方法,使用此方法可取下颗粒,传送到第二样品表面,并在其上重新定位。包括调整静电力以在探针和颗粒之间产生吸引力。调整静电力包括局部调整入射到样品系统中单个组件上的电子束、离子束或光子束的能量或强度(强度指电子或离子束的束流),以在颗粒和探针尖端之间产生静电吸引力,或在颗粒和第一样品表面之间产生静电排斥力,这些组件包括探针尖端、颗粒和第一样品表面。将颗粒从探针尖端传送到第二样品表面的过程与此相反。The invention discloses a method for analyzing the composition of tiny particles fixed on the surface of a first sample. Typically, particles are a contaminant in semiconductor production systems, and this method is not limited to use in that environment. The method includes placing a micromanipulator probe near a particle; attaching the particle to the probe; removing the probe and attached particle from a first sample surface; placing the particle on a second sample surface; Energy dispersive X-ray methods, Auger microprobe analysis, or other suitable analytical techniques are used to analyze the composition of the particles on the surface of the second sample. During analysis, the second surface has a reduced or non-interfering background signal relative to the background signal of the first surface (the applicant refers to the reduced or non-interfering background signal as a "controlled" background in the claims). Signal). The present application also discloses a method of modulating the electrostatic force and DC voltage between the probe, particle and sample surface, whereby the particle can be removed, transported to a second sample surface, and repositioned thereon. This includes tuning electrostatic forces to create attractive forces between probes and particles. Adjusting the electrostatic force involves locally adjusting the energy or intensity of the electron beam, ion beam, or photon beam (intensity refers to the beam current of the electron or ion beam) incident on individual components in the sample system to generate electrostatic force between the particle and the probe tip Attractive, or electrostatic repulsive forces are created between the particle and the first sample surface, these components include the probe tip, the particle and the first sample surface. This process is reversed for transporting particles from the probe tip to the second sample surface.
第二样品表面也可能是探针尖端本身。在这种情况下,探针尖端由受控制的背景材料组成。由于这些微小的颗粒也可能透射能量束,或将能量束散射到下面的表面,因此有必要将附着有颗粒的探针尖端转换为由受控制的材料组成的表面,或使这种受控制背景材料位于附着有颗粒的探针尖端的下面。在本文中,“下面”指颗粒上与受到能量束入射的一侧相对的一侧(即,透射侧)。The second sample surface may also be the probe tip itself. In this case, the probe tip consists of a controlled background material. Since these tiny particles may also transmit the energy beam, or scatter the energy beam to the underlying surface, it is necessary to convert the particle-attached probe tip to a surface composed of a controlled material, or to make this controlled background The material is located under the probe tip to which the particle is attached. Herein, "lower side" refers to the side of the particle opposite to the side on which the energy beam is incident (ie, the transmission side).
具体实施方式Detailed ways
半导体制造业通常使用扫描电子显微镜(SEM)、聚焦离子束(FIB)仪器或扫描俄歇微探针(SAM)来分析微小颗粒。FIB仪器有单光束或双光束(SEM和离子束)两种模式。常用的FIB仪器由Hillsboro,Oregon的FEI公司制造,有200、235、820、830和835几种型号。下文提及的探针120是连接到具有真空馈通的FIB仪器的微操纵器的一个组件。一种常规的此类微操纵器是由Dallas,Texas的Omniprobe公司制造的100型微操纵器。典型的SAM仪器包括Peabody,Massachusetts的JEOL USA公司制造的JAMP-7810和JAMP-7830F。Semiconductor manufacturing typically uses scanning electron microscopes (SEM), focused ion beam (FIB) instruments, or scanning Auger microprobes (SAM) to analyze tiny particles. FIB instruments are available in single-beam or dual-beam (SEM and ion beam) modes. Commonly used FIB instruments are manufactured by FEI Corporation of Hillsboro, Oregon, and there are several models of 200, 235, 820, 830 and 835. The
图1描述处理和分析颗粒的常见装置。图1A为停留在第一样品表面110上的所要探测的颗粒100。微操纵器探针120位于颗粒100附近。探针尖端可以相对颗粒和第一样品表面带有静电荷。或者,一个电压源130可连接在探针120和第一样品表面110之间。用带电粒子束照射粒子可以改变粒子上的局部静电荷。图1B到1D分别示出了用光子或带电粒子束140照射颗粒100和第一样品表面110以使颗粒100附着到探针120上,将探针120和附着到其上的颗粒100从第一样品表面110上移开,以及,将颗粒100淀积到第二样品表面150以供分析。这些图不是按照比例绘制的。Figure 1 depicts a common setup for handling and analyzing particles. FIG. 1A shows a
将颗粒附着到探针上Attach particles to probes
真空中的颗粒具有强大的静电力。由于颗粒100和探针120上静电荷的存在,导致在相对的表面产生像电荷。这些像电荷产生的力与暴露的面积成正比,与物体间的距离成反比。减小或增大暴露面积将使作用在颗粒100上的力减小或增大,最终影响探针120和颗粒100间的附着力。使用这种方法,通过导电或绝缘的探针120可直接将所要探测的颗粒从样品上取下。导电的探针有更多的功能,它可以将静止或随时间变化的电压或静电荷从电压源或静电荷源130引入到探针120,如图1A所示。Particles in a vacuum have strong electrostatic forces. Due to the presence of electrostatic charges on the
探针120尖端的形状也会影响到尖端的电场。在比较钝的尖端上的静电荷对与该尖端对齐的颗粒的影响力比在尖锐的尖端要大。相反,在导电尖端上具有直流电压的情况下,尖锐的尖端会在该尖端处产生最强大的电场。例如,在使用FIB仪器的电子束140成像时,探针120能够移动到非常接近颗粒100的地方,如图1B所示。电子束也能影响表面-颗粒-探针系统中的电荷分布,因而能有助于将颗粒100附着到探针120上。下面将讨论这种作用的应用。在图1B和其它图中示出的电子束140应该被理解为也可以是带电粒子束或光子束,也可能包含离子束。本文中,这些束以及从激光发出的光子束在权利要求部分都被称为“能量”束。The shape of the tip of the
一般情况下,调整系统中的静电力包括调整入射在颗粒100、探针120和第一表面110上的电子束140的能量,以在颗粒100和探针120之间建立相对的静电吸力,以及在颗粒100和第一样品表面110之间形成相对的静电排斥力。此过程可在连接于第一样品表面110和探针120之间的电压源130的协助下完成。显然,碰撞束140也可以是光子束,具有足够的能量释放光电子,能改变系统中的电荷分布和静电力。In general, adjusting the electrostatic forces in the system includes adjusting the energy of the
该优选实施例也可在探针120上使用粘合剂160来进行,如图2A所示。合适的粘合剂160可以是任何具有较低的蒸气压的物质,如真空油脂、低熔点蜡或其它低蒸气压的胶水。在这种情况下,尽管有静电力存在,粘合力只捕获颗粒100。This preferred embodiment can also be implemented using an adhesive 160 on the
如图2B所示,在另一实施例中,与探针120相连的镊子170抓住颗粒100,并把它从第一样品表面110移开。Berkeley,CA的MEMS Precision Instruments就生产带有镊子170和类似夹子的合适装置。As shown in FIG. 2B , in another embodiment, tweezers 170 attached to probe 120
探针120可以接触到颗粒100,但在多数情况下这不是必须的,因为颗粒100由于静电吸引力的作用会跳到探针120上。静电场受表面面积控制,并且探针120上钝的尖端或颗粒100或探针120的钝边能够增强它的作用,而集中了电场线的尖锐尖端能够增强直流电势的作用。图2C和2D示出了通过控制暴露在操纵器下的颗粒100的表面面积,通过将探针120的尖端125和探针120的边135作用到颗粒100上以获取需要的颗粒100的运动,来附着并传送颗粒100的方法。The
还有另外一种调整颗粒-探针-表面系统中静电场的方法,以附着并移动颗粒100,它包括将导电材料淀积到第一样品表面110或第二样品表面150上,在这种情况下,分布并调整颗粒所在的表面上的静电荷,以产生所需的作用在颗粒上的吸引力或排斥力。图3A示出了可极化微粒250(如水)在样品表面11上的淀积。图3B示出了通过源的蒸发作用产生的导电薄膜255的淀积。图3C示出了气体245的直接射流240喷到附着有颗粒100的表面110。气体245被能量束140分解,这个能量束可能是电子束、离子束或从激光发出的光子束。Yet another method of adjusting the electrostatic field in the particle-probe-surface system to attach and move the
图4为在真空系统中同时观察颗粒100并调整颗粒电荷状态的方法。在典型的FIB仪器中,SEM束和离子束以光栅图260扫描所要探测的物体。在扫描的同时发出二次电子,产生电信号,该信号以图像的形式显示给设备的操作者。由于扫描束不可避免地包含带电粒子,并导致样品发出带电粒子,如二次电子,因此,它本身就可以用来改变颗粒100的电荷状态。FIB仪器通常使用数字扫描发生器,其通过光栅图数字化地增加束斑的位置,每次一行,通常在行间反向,以消除传统模拟扫描仪具有的每行后回扫的特点。所以操作者或控制扫描的计算机程序能够确定在每个像素上的停留时间。例如,程序可以将颗粒上的遮盖物(或精确的颗粒轮廓)设定为零停留时间,扫描时直接空过。任一停留时间可被设置为由行频决定的最大时间,以避免在单一扫描中图像扭曲。也可以在遮盖物周围交替扫描,然后以不同的参数扫描遮盖物内部,这个动作很快,人眼看不出中断。FIG. 4 is a method for simultaneously observing
图4示出了在包括颗粒100的视电场上光栅扫描一次电子束270的步骤,产生并探测与一次电子束270同步的二次电子280,改变光栅扫描图260,以指定在与要组合和添加到标准光栅图中的颗粒100相关的光栅260场中具体像素的停留时间和位置。在停放有光栅260时,颗粒100相对于样品表面150经受一个过大的或减少的负电荷作用。这样,就可以调整颗粒100、探针120和样品表面150之间的静电场,以获得需要的吸引力或排斥力。光栅必须由离子束或扫描激光以相同方式产生。FIG. 4 shows the steps of raster scanning a
传送颗粒Teleportation Particles
一旦以上述方法将颗粒100附着到探针120上,就可以手动或用自动的探针120部件在真空环境中移动探针120。也可以用另一种方法轻轻地升起或收回探针120,并可以移动样品台以将受控制的背景材料带到探针120下面。Once the
也可以用探针120将颗粒100传送到由具有低背景或无干涉背景信号的受控制背景材料组成的第二样品表面150。用EDS进行分析时,低原子序数的材料,如碳和铍,将产生低能量的X射线,不会干涉大多数无机颗粒的分析过程。最好是原子序数小于或等于12。有机颗粒显然需要无机背景材料。作为第二样品表面150的低背景材料的例子包括光致抗蚀剂、碳平板、铍箔、导电的碳基浆料(胶状石墨悬浮液)、聚合体膜或碳管针。X射线背景不会在制作过程中与典型材料发生干涉的任何材料都可以用来做第二样品表面150。在某些情况下,第二样品表面150可以是第一样品表面110的不同部分。在其它情况下,如果知道或能猜测到颗粒100的部分成分,则第二样品表面150的材料应该具有与预料的从颗粒100发出的信号不同的背景信号。必须小心操作,防止第二样品表面150掩盖从制作设备外部的污染物可能发出的信号,如吸入的气体或化学物品中的杂质。对第二表面上的颗粒进行俄歇分析时,第二表面应该由低俄歇电子背景或无干涉俄歇电子背景组成。第二表面的组成应该具有一致的深度,该深度大于任何要在颗粒上进行的纵深分布检测的深度。第二表面的材料应该具有导热导电的能力,以最小化由于高电子束电流引起的带电或热机漂移问题,但不是必须的。在传送颗粒之前先对第二表面进行预溅射将消除原有的表面涂层(主要是碳和氧)并简化分析工作。可以用俄歇中的纵深分布离子源或FIB中的离子束进行这种预溅射。众所周知,第二表面的组成免去了背景分析,提高了产量。The
图5为将附着的颗粒100从探针120传送到第二样品表面150以供分析的几种方法。图5A示出了悬浮在下部框架190上的颗粒,比分析束140的穿透深度要薄。框架190通常是TEM栅格,可能有聚合体膜195如FORMVAR穿过栅格的开口处。Figure 5 illustrates several methods of transporting attached
图5B示出了在第二样品表面上150用粘合剂200附在其上的颗粒。图5C示出了由低弹性模量的背景材料210如真空油脂、低熔点蜡或低聚合物构成的第二样品表面150。在这种情况下,颗粒100就可以被推入低模量材料210中并粘在那里。FIG. 5B shows particles attached thereto with adhesive 200 on the
图5D为绝缘的第二样品表面150上的褶皱表面220。褶皱表面220能够增加颗粒100与第二样品表面150的接触面积,因而能改变它们之间的静电力。FIG. 5D is a corrugated surface 220 on the insulating
图5E为通过带电粒子束140写在第二样品表面150上的充电图案230。该图案的静电场有助于将颗粒从探针120传送到第二样品表面150上。FIG. 5E is a charge pattern 230 written on the
图5F为具有多个孔或小孔的第二样品表面150。这样的表面可能是微孔过滤器,如St.Paul,Minnesota的3M Corporation制造的MICROPORE系列过滤器,也可能是玻璃纤维过滤器,如St.Paul,Minnesota的3M Corporation制造的FILTRETE或EMPORE系列过滤器,或者“多孔碳”薄膜,如QUANTIFOIL系列,是由West Chester,PA的Structure Probe,Inc制造的。这些表面的优点在于,颗粒100在这些表面的孔或小孔里可以静止或被静电捕获并保持不动以供分析。Figure 5F is a
在某些情况下,可能需要寻找局部的高静电场区域,足以把颗粒100从探针120上取下而不发生接触(如果需要)。In some cases, it may be desirable to find localized areas of high electrostatic field sufficient to remove the
当然,上文描述的在颗粒-探针-样品表面系统中调整静电力以将颗粒100附着到探针120上的方法也可以用来将颗粒100从探针120上取下并附着到第二样品表面150上。特别是,如通过探针120迅速转换来自电容器中储存的负电荷,或通过从电荷源130作用到探针120上的随时间变化的电压,如方波或脉冲,使电压或电荷源130能产生快速转变或谐振现象。Of course, the above-described method of adjusting the electrostatic force to attach the
分析颗粒Analyzing particles
X射线分析或俄歇分析能够在探针尖端125上直接分析颗粒100,如图6所示。当然,这样就会从探针尖端120本身产生X射线或俄歇电子。可以使用低背景或无干涉背景材料作为探针尖端的材料,如上文所述,在分析时将低背景或无干涉背景材料放在探针120下面,或将平台和探针120附近的所有其它部件全部放低,以降低其它干涉信号。对颗粒100的分析已经完成,所以本步骤以后可以破坏性地取下颗粒100。有许多破坏性的方法,如将探针120插入某些类型的等离子清洁器中,在V型槽这样的机械结构中摩擦掉颗粒100,在真空中或在大气中暴露以后光学照射探针,或融化颗粒100。X-ray analysis or Auger analysis can analyze the
但是,通常要在第二样品表面150分析颗粒100,如图7所示,其中,颗粒100在带电粒子分析束140的照射下,发出特征俄歇电子或X射线180,可以使用本申请背景部分描述的任何方法进行成分分析。在权利要求部分,术语“发射”指俄歇电子或X射线。However, the
在探针尖端分析颗粒Particle Analysis at the Probe Tip
第二样品150表面也可以是探针尖端135本身。在这种情况下,探针尖端135由受控制的背景材料组成。在使用其中可进行表面离子束研磨的SAM或FIB等分析仪器时,在将颗粒100附着到尖端135前,先对探针尖端135的表面进行离子束研磨,可减少原有表面涂层和探针尖端135表面上的残余物发出的信号。由于微小的颗粒也能透过能量束140,或将能量束140散射到下面的表面上,因此有必要将附着有颗粒100的探针尖端135转换到由受控制的背景材料构成的表面上,或使这种受控制背景表面转移到附着有颗粒100的探针尖端135的下面。在本文中,“下面”指颗粒100上与受到能量束140入射的一侧相对的一侧(即,透射侧)。The
由于本领域技术人员能够改进上述的具体实施例,因此我们的权利要求包含这些改进及其等同物。Since modifications of the specific embodiments described above will occur to those skilled in the art, our claims cover such modifications and their equivalents.
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| CN104236978A (en) * | 2014-09-30 | 2014-12-24 | 中国原子能科学研究院 | Method for measuring isotope ratio of uranium in single particle |
| CN105797867A (en) * | 2016-05-09 | 2016-07-27 | 长安大学 | Electrostatic mineral particle selector |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN111521623A (en) * | 2020-04-28 | 2020-08-11 | 广西大学 | Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip |
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| WO2022178903A1 (en) * | 2021-02-28 | 2022-09-01 | 浙江大学 | Method and device for manufacturing microdevice |
| CN116329193A (en) * | 2021-12-23 | 2023-06-27 | 三星电子株式会社 | Protective film cleaning device and protective film cleaning method using the same |
| CN116477566A (en) * | 2023-03-23 | 2023-07-25 | 清华大学 | Fabrication Method of Single Particle Microelectrode Based on Microcapillary Injection |
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| DE102006045620B4 (en) | 2006-09-25 | 2009-10-29 | Roland Dr. Kilper | Device and method for receiving, transporting and storing microscopic samples |
| EP1953789A1 (en) * | 2007-02-05 | 2008-08-06 | FEI Company | Method for thinning a sample and sample carrier for performing said method |
| JP5849331B2 (en) * | 2011-08-31 | 2016-01-27 | 国立大学法人静岡大学 | Micro-adhesion peeling system and micro-adhesion peeling method |
| CN112180124A (en) * | 2020-08-31 | 2021-01-05 | 上海交通大学 | A kind of preparation method of submicron probe for atomic force microscope |
| WO2022178901A1 (en) * | 2021-02-28 | 2022-09-01 | 浙江大学 | Electronic tweezers |
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| US4590792A (en) * | 1984-11-05 | 1986-05-27 | Chiang William W | Microanalysis particle sampler |
| US6188068B1 (en) * | 1997-06-16 | 2001-02-13 | Frederick F. Shaapur | Methods of examining a specimen and of preparing a specimen for transmission microscopic examination |
| US6777674B2 (en) * | 2002-09-23 | 2004-08-17 | Omniprobe, Inc. | Method for manipulating microscopic particles and analyzing |
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2004
- 2004-06-08 CN CNA2004800379489A patent/CN1977159A/en active Pending
- 2004-06-08 CA CA002543396A patent/CA2543396A1/en not_active Abandoned
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Also Published As
| Publication number | Publication date |
|---|---|
| CA2543396A1 (en) | 2005-12-29 |
| EP1754049A2 (en) | 2007-02-21 |
| WO2005123227A2 (en) | 2005-12-29 |
| WO2005123227A3 (en) | 2006-12-14 |
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