Electron microscopy

Grain Analysis in OIM Analysis

Dr. Sophie Yan, Applications Engineer, EDAX

Recently, we held a webinar on Grain Analysis in OIM Analysis™. After the webinar, many users mentioned that the basic operation overview was very helpful. Since there was a very enthusiastic response, I want to take this opportunity to share these fundamental tips and tricks with the greater electron backscatter diffraction (EBSD) community.

Perhaps the most popular EBSD application is grain analysis, as it’s fundamental to characterizing many materials. Because the results of grain analysis are sometimes consistent or inconsistent with other tests, it’s great to start with a basic understanding of a grain with respect to EBSD and how grain analysis works.

The definition of a grain in OIM Analysis differs from the strict academic definition, which refers to the collection of pixels within a certain orientation range. This orientation range, namely grain tolerance angle, can be changed in OIM Analysis, which is generally set to 5° by default. You can also vary the number of pixels in a grain (the default is 2). These parameters affect the result of grain size, so we should pay attention to them in the analysis. The prerequisite of grain analysis is that the data is statistically valuable. Sometimes this requires a lot of tests to achieve the goal, repetitive studies to diminish errors, or the data should be filtered or processed before the analysis (per relevant standards, accordingly).

Figure 1. A typical grain map.

A standard display for grain size analysis is the Grain Size (diameter) chart. First, the grain is fit to a circle, and then the software calculates the diameter. The data distribution range and average grain size are on the chart’s right side. The most frequent question users ask is, “What is the formula to calculate the average grain size?”. In fact, two results of the average grain size, which are calculated by two different methods, are shown. The ‘number’ method calculates the average area of each grain first (the sum area is divided by grain number values first) before it determines the diameter. In contrast, it considers different weights due to different areas for the ‘area’ method. Since large grains have larger weight percentages, it first calculates the average grain area using different weight percentages, then calculates the average grain size.

In addition to the average grain size, OIM Analysis offers a variety of charts and plots to characterize grain shape. The most popular one is the grain shape aspect ratio, an essential parameter to display the columnar grain property (grains are fit as an ellipse). In addition to the shape aspect ratio, the Grain Shape Orientation in OIM Analysis shows the angle between the long axis and the horizontal direction, which is suitable for grains with a specific growth direction.

OIM Analysis offers numerous functions. Concerning grain analysis, there are six different charts for grain size and eight for grain shapes. Some charts are not common, but they have corresponding application scenarios. If you do not know the meaning of those charts, you can query the OIM Analysis Help file to get relative information.

Grain analysis is a very common function of EBSD applications. As a webinar speaker, I enjoyed digging up some less familiar details so users could gain a deeper understanding of software operations. I look forward to continually introducing webinar topics to meet the EBSD community’s needs and make greater progress in the new year.

关于晶粒那些事儿

Dr. Sophie Yan, Applications Engineer, EDAX

最近我们办了一期OIM Analysis如何进行晶粒分析的直播，效果颇出我意料。大家对于基本操作的热情令我始料未及，在播出之后联系我的人中，也往往会提到这一场直播对他们有所帮助。我本以为，这一类关于基本操作的直播并不太吸引人，充其量也不过是成为大家在日常操作中备查的工具视频而已；但，果然是我灯下黑，事实并不是如此。我也借此机会，给大家分享一些基本的原则或窍门。

可能在EBSD的各种应用场景中，最常碰到的是就是粒度分析。绝大多数的人都会有这个需求。EBSD粒度分析的结果，有些会与其它测试的结果吻合，有些会有出入。这时，我们就必须了解EBSD的晶粒是怎么定义，粒度又是怎么测得的，才可能更好的分析EBSD测试的结果。

OIM中的晶粒不同于学术上严格的定义，是指在一定取向范围内的像素点的集合。这个取向范围，即容差角，是可以设置的，一般默认为5度。像素点的个数，也同样可以设置，默认个数为2; 这些参数的设置，其实都会影响我们统计晶粒粒径的结果，因此需要在粒径分析中予以注意。当然，进行粒径分析的前提是数据具有统计意义，有时需要进行大量的重复性的测试来减少误差，也需要在测试之前对数据进行筛选或处理（可参照相关标准进行操作）。

典型的晶粒图

最常见的粒度分析的结果是将晶粒拟合成圆，计算其平均直径，即常见的Grain Size(diameter)曲线。曲线（或柱状图）的右边是数据部分，有不同粒度分布的占比，也列出了平均粒径。这是我被客户问得最多的部分，即，我们的平均粒径的结果是怎么计算的：这个平均粒径其实列出了两种结果，由两种方法分别计算。“number”方法是指按数数目的方法，先计算每个颗粒平均的面积(总面积除以晶粒数)，然后再计算直径；”area”则要考虑因面积不同而带来的不同权重，大颗粒占权重较大，按权重计算出颗粒的平均面积，再计算平均粒径。

除平均粒径外，OIM Analysis还提供了多种表征颗粒形状的图表。最常见的是短长比（grain shape aspect ratio）,是描述非等轴晶粒径的重要参数(晶粒被拟合成椭圆)。当然，除了短边长边的比值，有些颗粒有形状还有明显的择优，按特定的方向生长，针对这一点，Grain Shape Orientation表征长边与水平方向的角度，可以描述这一特性。

OIM Analysis提供非常丰富的功能，晶粒粒径有6种不同图表，晶粒形状有8种。有些图表可能不太常用，但都有对应的应用场景。对于这些相对冷门的图表，一般用户，如不了解其功能，可以在OIM Analysis提供的帮助文件中查询，可以得到关于其功能或定义的相关信息。

粒度分析是EBSD应用非常常用的功能。这一次，作为主讲人，在准备过程中我也挖掘出一些平常不注意的细节，对软件操作也有了更深的了解。相信，随着我们随后不定期推出的一系列培训，我们能更加贴合用户的需求，协助大家把软件用得更好，在新的一年里，获得更大的进步。

Reaching Out

Dr. René de Kloe, Applications Scientist, EDAX

2022 was a year of changes. In the beginning, I set up a desk in the scanning electron microscope (SEM) lab where, without truly reaching out, I only needed to turn in my chair to switch from emails and virtual customers on my laptop to the live energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) system and real data on the microscope. As travel restrictions gradually eased worldwide, we were all able to start meeting “real” people again. After almost two years of being grounded, I finally met people face to face again, discussing their analysis needs, and answering questions do not compare to online meetings. We restarted in-person training courses, and I participated in many external courses, exhibitions, and conferences, reaching out to microscopists all over Europe.

And as always, I try to correlate real life with some nice application examples. And what is similar to reaching out to people in the microanalysis world? Reaching out to things! So, what came to mind are remote thermal sensors, which most of us will have at home in the kitchen: a thermostat in an oven and a wired thermometer that you can use to measure food temperatures. And I just happened to have a broken one that was ready to be cut up and analyzed.

Figure 1. a) A food thermometer and b) an oven thermostat sensor.

On the outside, these two sensors looked very similar; both were thin metal tubes connected to a control unit. Because of this similarity, I was also expecting more or less the same measuring method, like using a thermocouple in both thermometers. But to my surprise, that was not quite the case.

The long tube of the food thermometer was mostly empty. Right at the tip, I found this little sensor about 1 mm across connected to copper wires that led to the control unit. After mounting and careful sectioning, I could collect EDS maps showing that the sensor consisted of a central block of Mn-Co-Fe-oxide material sandwiched between silver electrodes soldered to the copper-plated Ni wires.

Note that in the image, you only see one of the wires, the other is still below the surface, and I did not want to polish it any deeper.

Figure 2. The temperature sensor taken out of the tube of the food thermometer.

Figure 3. A forward scatter SEM image of the polished cross-section showing the central MnCoFe-oxide material and one of the connecting wires.

This was no thermocouple.

Figure 4. The element distribution in the sensor.

Figure 5. The EDS spectrum of the central CoMnFe-oxide area.

Instead, the principle of this sensor is based on measuring the changing resistivity with temperature. The EBSD map of the central Co-Mn-De oxide area shows a coarse-grained structure without any preferred orientation to make the resistivity uniform in all directions.

Figure 6. An EBSD IPF on Image Quality map of the sensor in the food thermometer.

Figure 7. (001) pole figure of the MnCoFe oxide phase, showing a random orientation distribution.

And where the tube of the food thermometer was mostly empty, the tube of the oven thermostat sensor was completely empty. There were not even electrical connections. The sensor was simply a thin hollow metal tube that contained a gas that expands when heated. This expansion would move a small disk with a measurement gauge that was then correlated with a temperature readout. Although this sounded very simple, some clever engineering was needed to prevent the tube from pinching shut when bending and moving it during installation.

I cut and polished the tube, and an EBSD map of the entire cross-section is shown below.

Figure 8. a) EBSD IQ and b) IPF maps of a cross-section through the entire tube of the oven thermostat sensor.

The tube is constructed out of three layers of a Fe-Cr-Ni alloy with fine-grained multiphase chromium phosphide layers in between. This microstructure is what provides corrosion protection, and it also adds flexibility to the tube. And this, in turn, is crucial to prevent cracks from forming that would cause the leaking of the contained gas, which is critical in getting a good temperature reading.

The detailed map below shows a section of the phosphide layer. There are two chromium phosphide phases, and in between, there are dendritic Ni grains that link everything together.

Figure 9. EDS maps showing the composition of one of the phosphide layers.

Figure 10. EBSD IPF maps of the different phases. a) All phases on a PRIAS center image, b) CrP, c) Fe matrix, and d) Ni dendrites, Cr3P.

When you look at the microstructure of both sensors in detail, it is possible to determine how they work, and you can appreciate why they have been designed as they are. The two devices are efficient and tailored to their intended use. The oven thermostat is designed to be mounted in a fixed position to be secure so that it can be used for a very long time. The food thermometer is very flexible and can easily be moved around.

In that respect, I feel there is another similarity between these sensors and the different kinds of meetings between people we have experienced over the past year. It does not matter how you do it; you can always reach out and feel some warmth.

I wish everybody a very happy and peaceful 2023.

APEX, now with WDS!

Dr. Shangshang Mu, Applications Engineer, Gatan/EDAX

The new APEX™ 3.0 is the ultimate materials characterization software, integrating Energy Dispersive Spectroscopy (EDS), Electron Backscatter Diffraction (EBSD), and Wavelength Dispersive Spectrometry (WDS) to deliver previously unattainable solutions. This optimized configuration offers the uncompromised performance of each technique and allows users to combine them for the ultimate materials insight. All three techniques seamlessly operate within the APEX, blending powerful elemental and crystallographic analysis routines through an intuitive interface to deliver outstanding data collection, faster analysis, and flexible reporting for users of all levels.

What does APEX WDS look like?

WDS functionalities are implemented seamlessly with the EDS graphical user interface. The user can quickly adapt to the new functionalities and employ WDS when and where EDS reaches the limit. With one-click from start to finish, Auto WDS allows fully automated WDS scan list generation, optimum sample height determination, and spectrum collection. It simultaneously collects EDS and WDS spectra and displays them side-by-side or overlaid for easy data visualization and interpretation (Figure 1), with no overlapping or overloading of windows.

Figure 1. Simultaneous EDS-WDS spectrum acquisition user interface.

APEX allows you to set an intermediate position for the EDS detector to ensure optimal count rates for both techniques.

Figure 2. Simultaneous EDS-WDS mapping user interface.

Sets of combined EDS-WDS spectrum, linescan, and mapping data at different stage positions can be done via automated batch collection routines (Figure 2) to streamline SEM experiments. EDS and WDS data collection settings are managed in one user-friendly batch scan list (Figure 3).

Figure 3. Combined EDS-WDS batch list.

The quantitative elemental analysis supports individual technique or combined EDS-WDS standards. You can easily switch between EDS and WDS standards for each element by clicking on the icon in front of the element (Figure 4).

Figure 4. Quantitative results with combined EDS-WDS standards.

With the addition of WDS capabilities, APEX 3.0 now includes EDS, EBSD, and WDS. Each characterization tool can operate independently to utilize EDAX’s technological advancements or integrates data to provide solutions that were once unachievable.

Simulate them!

Dr. Chang Lu, Application Specialist, Gatan & EDAX

In early 2022, Gatan and EDAX completed the integration, and our new division was named Electron Microscope Technology (EMT). As an EMT application scientist on the China applications team, I am responsible for almost all the Gatan and EDAX products for Northern China, on both Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) platforms. Therefore, I work with diversified products and diversified user groups that focus on different subject matters. In the first half of this year, I found that the data analysis software from EMT Gatan’s DigitalMicrograph® (DM) and EDAX’s OIM Analysis™ are not completely isolated, but in many cases, they can cooperate with each other to help our customers.

For instance, DM can do a series of electron microscopy-related data processing. For some energy dispersive spectroscopy (EDS) mapping data from the minor content, there are various methods to achieve smoothing and enhance the contrast. While in the MSA panel, the principal component analysis (PCA) function can be helpful in terms of high-resolution EDS mapping. However, in today’s EDAX blog, I will talk a little bit more about one feature in OIM Analysis that could potentially benefit a lot of Gatan camera users.

In northern China, there are a group of Gatan users who are focused on nanoscale phases and grains in the TEM. In most scenarios, they heavily employ electron diffraction or bright field imaging to make judgments. However, it is really difficult to determine the unknown (unidentified but has a known x-ray diffraction (XRD) pattern and chemical composition, so there is a potential for it) phase by simply relying on the minor changes of grayscale bright field images. You may say diffraction could help. Yes, a clean, beautiful diffractogram of a particular crystal direction can be helpful. But, no, you need to find the zone axis carefully. If this unknown phase has a crystal structure of low symmetry, most of the time, the effort will be in vain. Generally speaking, the Difpack tool in the DM software could help in determining d-spacing and angles, however, it is not intuitive enough to know the sample at first sight.

The solution is pattern simulation with OIM Matrix™. At first, I noticed this feature because it helped an EDAX user who was studying strains. It can easily export a theoretical Kikuchi pattern for a specific sample orientation with zero stress. Then one day, I had a sudden thought during my morning shower. Maybe I can change the acceleration voltage to 200 kV (typical for TEM), and the sample tilt angle to 0° (make it flat). After entering a specific orientation, we can get a Kikuchi pattern under TEM conditions! For example, take the simulated pattern from NdCeB. With Kinematic Color Overlay, we can also find out what crystal plane corresponds to a specific Kikuchi line. Now, when we start changing the zone axis in an unidentified sample, we can first simulate several orientations and compare them with what we see under TEM. In this way, the process of finding the Kikuchi pole turns out to be very convenient.

Figure 1. A simulated pattern from NdCeB using OIM Matrix.

Now, when some Gatan users bring in some “weird” unidentified samples and say they want to find various zone axis for doing diffractions. I don’t worry about it. I think from a problem-solving point of view, the powerful software from both Gatan and EDAX, like the integration of two companies, can also be combined to solve complex and difficult problems for our customers in the future.

模拟他们！

Dr. Chang Lu, Application Scientist, Gatan & EDAX

2022年初，Gatan和EDAX这两家公司完成了整合，我们的部门更名为Electron Microscope Technology (EMT)。作为EMT中国团队的应用技术支持，我负责中国北方区扫描电镜（SEM）还有透射电镜（TEM）上Gatan还有EDAX的几乎全部产品。产品多样，服务的用户群体也多样。慢慢地在工作过程中，我就发现两边的数据分析软件（Gatan的Digital Micrograph以及EDAX的Orientation Imaging Microscopy）其实并不是完全分开的，很多时候它们可以在不同程度上相互支持，互通互联。

比如说，Gatan公司在TEM平台上知名的DigitalMicrograph（DM）软件。DM可以处理一系列的电镜相关的表征数据。对于部分信号较弱的EDAX能谱结果，我们也可以把数据载入，通过DM内置的图像平滑，互相关算法以及主成分分析（PCA）进行数据的优化处理。但是我今天更想要分享的是EDAX Orientation Imaging Microscopy（OIM）软件在TEM平台上的一些应用。

在我服务的客户群体中，有一些用户尤其关注一些纳米级的物相和晶粒。这时候在TEM平台，我们往往需要使用到电子衍射的手段来对样品进行判断。然而，很多时候单单依靠透射电镜下灰度值衬度的变化，一些微弱的物相的改变很难被发觉。同时，一张干净，漂亮的来自特定晶向的电子衍射，往往需要我们对样品旋转晶带轴。虽然我们可以沿着特定的菊池线去找菊池极，但是这条菊池线对应什么晶面？菊池极对应哪个晶带轴？我们往往需要在Difpack工具里面标定晶格间距和角度，再比对样品材料不同晶面和夹角才有可能清楚，这很麻烦。

我第一次注意到OIM中的Pattern Simulation功能是因为帮助某个研究应力应变的老师输出无应力的特定取向的标准菊池花样图。然后我注意到，其实我是可以对应更改电镜的加速电压，样品倾斜角度还有取向来得到一系列的菊池花样，比如下图这个200 kV加速电压下得到的NdCeB 样品的模拟花样。我们可以对左下角的orientation参数进行修改，得到一系列模拟出来的菊池花样。通过Kinematic Color Overlay，我们还可以知道对应的菊池线对应的是什么晶面。现在，当我们处于未知状态开始转晶带轴的时候我都会首先模拟几个相似的取向，进行对比。这样一来，我沿着那个晶面（菊池线）在找哪个晶带轴（菊池极）都变得异常清楚，这非常方便。

图 1. NdCeB 使用 OIM Matrix。

现在，当Gatan的用户再拿来一个“奇奇怪怪”的样品说要找到特定晶带轴做衍射，我也不像以前担心怎么搞了。需要什么，我们就在EDAX OIM中先模拟出来一个，对着这个模拟的图，旋转，调整晶面，然后在TEM电子衍射过程中去找。我想从解决问题的角度来讲，Gatan和EDAX丰富的软件资源，就像我们这两家公司的合并一样，未来也可以合并解决客户复杂和困难的问题。

Is lack of invention a side effect of COVID?

Dr. David Stowe, Senior Product Manager – EDS and SEM Products, EDAX/Gatan

My friends and family have always thought that, as a microscopist, I spend my working days in a darkened room staring at dimly lit screens or developing negatives. Yet, the reality of working for a commercial company in the electron microscopy business could hardly be more different—scientific meetings, workshops, and spending time with users have allowed me to travel the world and make friends with some of the most interesting people. It’s always been a source of wonder and amazement for my family that the microscopic world could provide so many opportunities to see our world at large!

Sadly, over the last two years, our daily routines have been aligned much more closely to those visions of darkened rooms and computer screens than we care to remember. However, for many of us, there does appear to be (sun)light at the end of the tunnel. In recent weeks, I attended my first in-person workshop in almost two years. Together with colleagues and more than 60 researchers, I traveled to Munich to attend the Gatan-EDAX Leading Edge Workshop held at the Allianz Arena (home to Fußball-Club Bayern München e. V.—known to many as Bayern Munich). As lovely as it was to visit such a famous sporting stadium, the enjoyment of attending scientific talks and engaging in exciting technical discussions with leading researchers far outweighed the attraction of the venue. The feedback from everyone who participated in the day was incredibly positive. Many of us walked away from the event with new ideas inspired by discussions that day.

One of my fears regarding the impact of COVID-19 on the scientific community is the impact that the lack of these in-person interactions has had on innovation, both in terms of new scientific ideas and technological advancements. While working from home, many of us have missed those stimulating ‘coffee break conversations’ with colleagues outside of our teams. To add, there has been a noticeable drop in interactions on virtual platforms at scientific conferences and commercial webinars, with many preferring to review material offline at a time of their choosing.

Fortunately for EDAX, the opportunity for engagement with others during the pandemic had rarely been as high. Since 2019, we have been joined in the Materials Analysis Division of AMETEK by Gatan; the exchange of ideas between the R&D and Applications teams of the two companies has been significant. Within the last year, we have already seen the first innovations arising from the interactions between the two companies with the announcement of EDAX EDS Powered by Gatan for elemental analysis in the transmission electron microscope, simultaneous EDS and cathodoluminescence spectroscopy, and the development of a workflow solution for lithium analysis in the scanning electron microscope.

Within the last month, our applications teams were able to quantify the lithium content in lithium-ion battery cathode materials for the first time using the lithium-composition by difference method (Li-CDM).

Figure 1. First quantitative analysis of lithium content in cathode materials using the Li-CDM technique.

Their analysis used a range of tools from EDAX and Gatan to prepare, transfer, and analyze the specimen in the scanning electron microscope, highlighting the potential for innovation by Gatan and EDAX working together.

Figure 2. The tools from EDAX and Gatan used for the quantitative analysis of lithium in metal oxide cathode materials.

With the imminent arrival of the latest Microscopy and Microanalysis conference in Portland, OR, I am sure we will learn far more about how the changes to working practices have impacted innovation in our world. I am excited to leave my darkened room and discover your latest works in electron microscopy. I am sure that all participants will enjoy and value the personal interactions that are so important for innovation.

EDAX and Gatan Bring You Lithium

Dave Durham, Sales Manager – U.S. Western, EDAX

It has been interesting to recently witness EDAX and Gatan working together to combine the technologies in our portfolios. Although technically, Gatan was acquired by AMETEK back in late 2019, it seems like 2021 has been a year where the integration of our two companies has really begun to hit its stride.

For example, I’ve seen how Gatan’s ion polishing instruments can dramatically improve indexing success for EDAX’s Electron Backscatter Diffraction (EBSD) users compared to the conventional methods for sample preparation. And I’ve seen EDAX’s Elite T Energy Dispersive Spectroscopy (EDS) System undergo a tremendous workflow improvement and ease-of-use overhaul with the implementation of Gatan’s Microscopy Suite user interface. It has been great stuff!

However, the most recent integration between our two companies is truly groundbreaking, and I’m thrilled to see what it will do to enhance the research being done in its field.

Hopefully, you’ve already seen the news mentioned on our website. For the first time, we’ve been able to perform quantitative mapping of lithium in the Scanning Electron Microscope (SEM) by combining the power of EDAX and Gatan detectors and software! These breakthrough results will enable a new level of lithium research that was previously never possible with the SEM.

Figure 1. EDAX and Gatan bring you lithium.

So who cares about lithium? Everyone should. Lithium compounds and alloys are very important materials with significant commercial value. The compounds are being implemented into lightweight structural alloys in the aerospace and automotive industries. They’re also utilized in lithium-ion batteries for small electronic devices and vehicles. Many governments worldwide have proposed plans to reduce dependence on legacy energy sources, which makes further development of lithium-based technologies critical to the adoption of these plans. This means significant investments are currently being made in R&D, failure analysis, and quality control of these materials.

Figure 2. (left) Lithium-ion battery cross-section prepared by Ilion II broad beam argon milling system. (right) EBSD IQ + orientation map revealing the microstructure of the heat-affected zone in a lightweight structural alloy.

So what are the issues with lithium? While electron microscopy and EDS are already essential characterization tools in this industry, there is a distinct inability to map lithium distribution in the SEM. This has presented a significant obstacle, holding back research on these tools. EDS is typically a valuable technique for material characterization, with high sensitivity and spatial resolution to allow for quantitative analysis on a wide range of sample types. But it is not possible to identify lithium in commercially important materials by EDS because:

  1. There is no guarantee that lithium X-rays will be produced from the sample. The X-ray energy and the number of photons produced from the specimen depend on the lithium bonding state. So, even if you have lithium in your sample, it does not mean that lithium X-rays will be generated.
  2. Even if a sample does generate lithium X-rays, they are easily absorbed back into the sample itself, contamination or oxidation, or by the EDS detector window before they can even reach the EDS detector.

Indeed, specialized windowless EDS detectors can detect lithium, but these have drawbacks that impede their practicality and largescale adoption. Even on samples that have a high lithium fluorescence, these special detectors have a limit of detection of about 20 wt %. This is equivalent to about half of the atoms in the sample being lithium, which restricts analysis to only metallic lithium or simple lithium compounds that may not be relevant to advanced lithium research or applications.

And having a specialized windowless EDS system potentially introduces a slew of operational issues/limitations with the detector that aren’t present with a “standard” windowed EDS system. It also restricts the detector’s utility on non- lithium -research-based applications in the lab.

So what have EDAX and Gatan done? We have solved these issues by using a patent-pending technique called the Composition by Difference Method. In this method, we quantify the backscattered electron signal to determine the mean atomic mass for all elements in a particular area of a sample. And from the same region, we collect the EDS signal to quantify the non-lithium elements. From that information, we have two data points that tell us the actual mean atomic mass from the region and a calculated value based on the EDS results — when they don’t agree with one another, it tells us we are missing something in the EDS data. That something we’re missing is lithium.

Figure 3. Data from the OnPoint and the Octane Elite Super are combined and analyzed to quantify lithium.

By using this method, and specifically by combining the EDAX Octane Elite Super EDS Detector and the Gatan OnPoint Backscattered Electron Detector to collect these two signals, we can now generate lithium maps quantitatively with single-digit mass percentages of lithium with sub-micron spatial resolution. This accuracy has been verified to ~1 wt. % lithium by an external accredited laboratory using Glow-discharge Optical Emission Spectroscopy (GDOES).

Figure 4. Secondary electron image and elemental metal fraction maps (by wt. %) of the same region of the MgLiAl alloy; white pixels are regions excluded from the analysis due to the influence of topography (identified by arrows in the secondary electron image) shown here for clarity.

This is a cutting-edge capability in the SEM, and it is a huge opportunity for anyone wanting to discover where lithium exists in their specimens. Just to reiterate, this method does not use a specially designed EDS system for lithium detection! It uses EDAX’s standard (windowed) Octane Elite Super and Gatan’s OnPoint BSE detector, along with EDAX and Gatan software. Simply amazing!

Now that EDAX and Gatan have introduced the ability to provide quantitative lithium analysis, that is:

  • A substantial improvement in limits of lithium detection
  • Insensitive to the lithium bonding state
  • More tolerant to contamination and oxidation
  • Not limited to metallic materials or simple lithium compounds
  • Free from windowless detector-related limitations on the SEM

It seems that we have helped open an avenue for our customers to expand their lithium research beyond anything previously possible. We are truly beginning a very exciting new stage in lithium analysis, and I can’t wait to see how this new capability is used and what comes next!

You can find more information on this new development in our experiment brief.

Research Must Go On

Rudolf Krentik, Sales Manager – Central and Eastern Europe, EDAX

It has been some time since I started working at EDAX as an Area Sales Manager for Central and Eastern Europe. When I think about it, Russia is by far the largest region compared to all the others. If sales grew linearly with the size of the area, I would probably be a millionaire. Unfortunately, it is not the case. The primary purpose of my work is to take care of our distributors and business partners in individual countries. I give them support in business cases, provide up-to-date information about our products, and sometimes I am also an intermediary for the serious requirements of our end customers. The work is very interesting, especially because I meet interesting people. EDAX’s customers are primarily scientists and engineers studying materials, solving complex problems, and dealing with development and innovation. Such meetings are often very fun, inspiring, and rewarding.

Figure 1. My new office.

The market situation has changed dramatically since 2015, when I started. COVID-19 has completely changed the way we work. Instead of meeting customers at scientific conferences, we all locked ourselves in our homes for a long time. After three months, I couldn’t stand it and rented a small office so that I wouldn’t go crazy at my home office with my wife and two small children, who were also schooling and working from home. So I was moving from my home office to an actual office, doing just the opposite of what others were doing during the pandemic.

Moving from real life to the online world was probably frustrating for many of us. Still, we had to adapt and start selling and communicating over the phone and especially over the internet. Online presentations and meetings are still the order of the day. This way of communication will be maintained in the future, that is quite certain. Unfortunately, this does not replace personal contact, which is essential for creating a relationship with customers. It can already be seen that interest in virtual conferences is declining. People are inherently interactive and need to share their needs and feelings with each other. This is not possible in the world of the internet. Therefore, we all hope that everything will return to normal soon. Our service technicians have been traveling to places where it is safe for quite a long time, and we salespeople are also starting to plan our first trips abroad. I’m actually partly writing this blog in Turkey on my first trip in 18 months.

Although it does not seem so, COVID has not yet caused significant losses or loss of orders in terms of business results. Our business is still in good condition. One of the factors that affects this is the life cycle of a business case. This can take months or even years. If we do not soon return to the life we are used to; it will have very negative consequences for our field. I mention this because we are currently at the stage where we want to launch several exciting products. You probably know that Gatan also belongs to our AMETEK family. The company is known for its leading technology in detection systems in TEM and SEM and other devices, e.g., for sample preparation. The acquisition of Gatan is a great benefit not only for AMETEK but also for EDAX. The combination of know-how, development, and experience in the electron microscopy field creates space for innovation and synergies that would not be possible.

Several novelties were introduced three weeks ago at M&M 2021. It is worth mentioning the EDAX EDS Powered by Gatan, in which EDAX hardware is now integrated into the software from Gatan. This brings many benefits, such as a unified GUI for all the TEM techniques available from Gatan. EDS analysis with Elite T can now be performed seamlessly with Gatan EELS, 4D STEM (STEMx), or other techniques. This makes it all much easier and faster. And as we know, time is money, and this is doubly true for time spent at the TEM.

Another interesting novelty is the cooperation of EDS and CL detectors. Thanks to an EDS-compatible cathodoluminescence (CL) mirror that enables line of sight from the sample to the EDS detector while still collecting the CL signal, we can obtain information about the material’s structure that was previously difficult to achieve.

When it comes to EBSD, EDAX has been the leading provider of this technique since the 90s. But for reliable analysis, one needs a high-quality sample preparation tool. Again, with the Gatan PECS II, we can offer a complete workflow from getting the sample ready to post-processing of acquired data. The latest news is also the hottest news. With the help of the highly sensitive OnPoint BSE and Octane Elite EDS Detectors, it is possible to detect lithium for the first time and quantify it. Unique technology, the accuracy of which is verified by another method, is now available and we are very anxious to introduce this product to our customers.

That is why we need to get the COVID-19 pandemic under control. Without the opportunity to travel and meet our customers, our work will be inefficient and not as much fun. However, the newly introduced devices and the ongoing development of the EDAX-Gatan collaboration gives us a strong hope that everything is on track and that our efforts are worthwhile.

Want a Free Set of Microanalysis Standards?

Dr. Shangshang Mu, Applications Engineer, EDAX

Modern EDS systems are capable of quantitative analysis with or without standards. Unlike standard-less analysis, the k-ratio is either calculated in the software or based on internal standards. For analysis with standards, it is measured from a reference sample with known composition under the same conditions as the unknown sample. As an applications engineer, sometimes users ask me where to order these standards. Usually, I point them to the vendors that manufacture and distribute reference standards where you can order either off-the-shelf or customized standard blocks. In addition to these commercial mounts, I always tell them that they can request a set of mineral, glass, and rare earth element phosphate standards from the National Museum of Natural History free of charge! These are very useful standards that I’ve seen widely used in not only the geoscience world but also in various manufacturing industries. These free standards are also great for those graduate students with limited budgets and ideal for practicing sample preparation (yes, I was one of them).

This set of standards is officially called the Smithsonian Microbeam Standards and includes 29 minerals, 12 types of glass, and 16 REE phosphates. You can find out more information about these standards and submit a request form by clicking on the link below:
https://naturalhistory.si.edu/research/mineral-sciences/collections-overview/reference-materials/smithsonian-microbeam-standards

I mentioned sample preparation earlier. Yes, you read that right. These standards come in pill capsules containing from many tiny grains to a few larger ones and you need to mount them on your own (Figure 1).

Figure 1. Grains in a pill capsule.

Since you can get the information such as the composition, locality, and references for each standard from the website, what I want to discuss in this blog post is how to prepare them properly for X-ray analysis. The first tricky thing is to get them out of the capsules. The grains in Figure 1 are almost the largest in this set and you won’t get too many of this size. Some of the grains are even too tiny to be seen at first glance. For the majority that are really tiny, you need to tap the capsule a couple of times to release the grains that get stick to the capsule wall, then you can open the capsule very carefully and let the grains slide out with a little tapping.

For mounting, the easiest way is to mount the standards in epoxy using a mounting cup and let it cure. I did this in a fancy way to make it look like a commercial mount (Figure 2). I ordered a 30 mm diameter circular retainer with 37 holes used by commercial mount manufacturers (Figure 3) and filled the holes with standards on my own. I must admit that the retainer is not cheap, but you can machine the mount by yourself or have a machine shop do it for you. In addition to looking pretty, the retainer ensures a good layout so you can quickly locate the standards you need during microanalysis, and you can mount the same type of standards on one block and get rid of the hassle of frequently venting and pumping the SEM chamber to switch standard blocks.

Figure 2. Examples of commercial mounts.

 

Figure 3. 30 mm diameter circular retainer with 37 holes.

To prevent the tiny grains from moving and floating up when pouring the epoxy mix, I placed the retainer upside down and pressed it onto a piece of sticky tape (Figure 4a) and positioned the grains on the sticky surface of the tape within the holes. When tapping the capsule to let the grains slide out and fall into the hole, the other holes were covered to prevent contamination (Figure 4b). These holes are small in diameter and pouring the epoxy mix directly will trap air bubbles in the hole to separate the grains from the epoxy mix. To overcome this problem, I filled up the hole by letting the epoxy mix drip down very slowly along the inner surface of the hole.

Figure 4. Positioning grains within the holes of the retainer.

For general grinding, I start with wet 240 grit SiC sandpaper with subsequent use of 320, 400, 600, 800, and 1,200 grit wet SiC sandpapers. But coarser grits can grind off tiny grains in this case, so I would recommend starting with a relatively fine grit based on the sizes of the grains you receive and always use a light microscope or magnifier to check the grinding. For polishing abrasive, I used 1 micron and 0.3 micron alumina suspensions on a polishing cloth. For the grains used as standards or quantification in general, the surface needs to be perfectly flat. However, the napped polishing cloth tends to abrade epoxy and the grains at different rates, creating surface relief and edge rounding, especially on tiny grains. To mitigate this effect, the polishing should be checked under a light microscope constantly and stopped as soon as the scratches are removed. A vibratory final polishing with colloidal silica is optional. Followed by ultrasonic cleaning and carbon coating, the standard mount is ready to use.

Note that commercial mount manufacturers may prepare standards individually (especially for metal standards) and insert them into the holes from the back of the retainer and fasten them with retaining rings (Figure 5a). A benefit of this approach is that the standards on the mount are changeable, so you can load all the standards you need on one mount before microanalysis. I used to make several individual mounted standards that can fit into the retainer (Figure 5b) but this process is very time consuming and much trickier to keep the small surface flat during grinding and polishing.

Figure 5. a) The back of a commercial metal standard mount. b) A tiny cylindrical mount that can fit into the retainer holes.

This is definitely a good set of standards to keep in your lab. With EDAX EDS software, in addition to quantification with these standards, you can also use them to create a library and explore the Spectrum Matching feature. The next time you want to quickly determine the specific type of a mineral, you can simply collect a quick spectrum and click the “Match” button, and the software will compare the unknowns to the library you just created.