SEM中的轴上传输Kikuchi衍射

Brief History

OPTIMUS TKD detector head

First proposed in 2012(1), Transmission Kikuchi Diffraction (TKD) in SEM, also known as t-EBSD, has quickly become an established technique due to its spatial resolution being at least one order of magnitude better than that of standardEBSD. The technique requires an electron transparent sample placed horizontally or slightly tilted; for example normal or close to normal to the electron beam, and a standard EBSD detector positioned so that it captures a Kikuchi pattern from below the sample plane.

Recognizing the potential of this technique, Bruker started a collaboration with a team of researchers from Lorraine University in Metz, France, to address the limitations related to the non-ideal sample-detector geometry. This collaboration proved the principle for a new sample-detector geometry known as “on-axis TKD”(2)which later resulted in the launch ofOPTIMUSTMTKDdetector head. The new detector head features a horizontal screen that can be inserted directly beneath the electron transparent sample with the optical axis of the SEM intersecting the screen center, thus the name “on-axis” TKD. This configuration has the advantage of capturing the Kikuchi patterns where signal yield is strongest and with minimized gnomonic projection induced distortions(3).

The OPTIMUS TKD Detector Head

自2015年推出以来OPTIMUSTKD是唯一在SEM中实现轴心TKD的商业解决方案,并且由于其功能而将其定位为领先的TKD解决方案。

Unmatched performance

Low probe current requirements - OPTIMUSTKD enables orientation and phase mapping with nanometer scale spatial resolution at hundreds of points per second using not more than 2 nA probe current and with excellent data integrity or indexing quality.

Spatial resolution - With a spatial resolution of at least 2 nm (when using a high-end FE-SEM), OPTIMUSTKD reveals in high detail features smaller than 10 nm and sometimes features even smaller than 5 nm (see application examples below).

Patented TKD sample holder

便于使用

来自20 nm au膜(左)的原始/未加工方向图和包含退火双胞胎约4 nm的放大区域。重要参数:30 kV EHT,2 Na探针电流,1.5 nm步骤,11.5%零溶液,320 fps速度,6:31分钟测量时间。样本由丹麦哥本哈根DTU Nanolab的Alice Da Silva Fanta提供。

OPTIMUSTKD detector head can be used interchangeably with the standard detector head on all BrukerEflashEBSD探测器,giving easy access to both EBSD and TKD using the same detector. Depending on the measurement requirements; for example spatial resolution, trained users can switch between TKD and EBSD analysis in 10-15 minutes. OPTIMUSTKD works perfectly in combination with our patented TKD sample holder (EP 2824448 A1).

Integrated ARGUS for DF & BF like Imaging

To maximize performance and analysis success, OPTIMUSTKD设计了内置Argus™imaging system. Its high quality and high sensitivity solid state detectors give the user the option to acquire brilliant Dark and Bright Field like images with nanometer resolution at speeds of up to 125k points/sec. While being just qualitative information, these images reveal importantmicrostructure details like: orientation and phase contrast, dislocations and stacking faults or, in certain cases, even residual strain.

假色明亮的场(如(左)和黑暗场,如(右)图像从20 nm au膜中获取,分别由聚合物配体持有的PTNI纳米颗粒。

同时跆拳道/ EDS测量

TKD phase map after offline phase identification and EDS assisted reanalysis (left), patented TKD sample holder retrofitted with X-ray mask (top-right) and XFlash FlatQUAD EDS detector (bottom-right). Important parameters: 30 kV EHT, 6.7 nA probe current, 10 nm steps, 272 pps speed, 1.5 Mcps ICR, 1 Mcps OCR, <3000 counts per spectrum/pixel.

One of Bruker’s QUANTAXEDS/EBSDsystem most appreciated features is its advanced integration of the two techniques. The excellent integration is of course available also for electron transparent samples and is especially powerful when combining theEflashFSand the uniqueXFlash®FlatQUADEDS detector. The two detectors provide unrivaled data quality, spatial resolutionand throughput and work flawlessly with our patented TKD sample holder and the newly released X-ray mask.

Major Specifications

  • Spatial resolution for orientation mapping: 2 nm or better
  • Spatial resolution for DF/BF imaging: 1.5 nm or better
  • Smallest resolved features in maps: ~4 nm annealing twins in Au
  • Measurement speed: up to 630 fps (frames/sec)
  • EHT范围:5-30 kV
  • Probe current: at least 95% of applications require no more than 2 nA

相关出版物

(1)Transmission EBSD from 10 nm domains in a scanning electron microscope, R. Keller and R. Geiss, Journal of Microscopy, Vol. 245, Pt 3 2012, pp. 245–251

(2)Orientation mapping by transmission-SEM with an on-axis detector, J.-J Fundenberger et all., Ultramicroscopy, 161, 17–22, 2016

(3)轴心和离轴传输的系统比较kikuchi衍射,F。Niessen等人,超镜检查,186,158-170,2018