Month: January 2023

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.