Combined EBSD & EDS analysis: Advances in modern materials characterization

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1 Combined EBSD & EDS analysis: Advances in modern materials characterization Gert Nolze, Bruker Nano, Berlin EBSD/EDS Webinar, April 6 th, 2011 Innovation with Integrity

2 Talk outline QUANTAX CrystAlign EBSD System Fast and sensitive EBSD detectors with different resolution SEM images using color-coded orientation contrast Software: simultaneous acquisition and data processing EBSD & EDS integration Offline phase ID & phase discrimination 05/04/2011 2

3 CrystAlign: Experimental setup Electron beam hits sample surface tilted by about 70 The formation of a diffraction pattern (EBSP) takes place in a nm thick layer only. EDX spectra can be acquired simultaneously. A complete interpretation of a single diffraction pattern takes not longer than 1ms. The acquisition time is usually in the range of ms. Numerous interpretations can be used to describe orientation and phase maps. 05/04/2011 3

4 EBSD detector: e - Flash series 05/04/2011 4

5 EBSD detector: e - Flash series e - Flash 1000 : fast detector 640x480 pixels: 160x120 pixels: versatile detector 210 fps 630 fps e - Flash HR : HiRes detector 1600x1200 pixels: 160x120 pixels: 35 fps 130 fps ~3-times more sensitive in-situ positionable detector screen Move the screen to the position of the optimal signal irrespectively of which experimental set-up you are using, or material you are interested in! Completely software controlled Control your detector by only two Ethernet cables: motor, camera, FSE/BSE detectors. Even the tilt angle is available electronically. All electronics inside Whether operation panel, tilt sensor, or signal amplifier all is integrated. 05/04/2011 5

6 Versatility 5kV 10kV 15kV 20kV Experiment (Ni patterns) Pattern simulations (as proof) 05/04/2011 6

7 High resolution with e - Flash 1000 Lattice parameters: d 3.8% simulation Austenite a o =3.660Å experiment simulation Nickel a o =3.524Å 20kV 15kV 05/04/2011 7

8 e - Flash HR 05/04/2011 8

9 Application fields e - Flash 1000 Fast orientation maps, i.e. if speed higher than 130 fps are possible High voltage & high current applications Mainly metals and alloys Phase identification e - Flash HR Weak diffraction patterns, low voltage & low current application, low density phases Small probe size, i.e. Nano or highly deformed materials Non-conductive or sensitive samples Lattice strain investigations Phase identification 05/04/2011 9

10 Specific feature: In-situ screen positioning 10kV Spatial distribution of backscattered electrons is a function of WD=22.6mm 60 - phase density - acceleration voltage - surface tilt - working distance - Spatial distribution of BSE. The straight lines mark the direction of intensity maximum. Automatic system calibration Usually called pattern center calibration but also considers sample-screen distance and detector tilt. 05/04/

11 Specific feature: In-situ screen positioning 10kV Spatial distribution of backscattered electrons is a function of WD=22.6mm 60 - phase density - acceleration voltage - surface tilt - working distance - Spatial distribution of BSE. The straight lines mark the direction of intensity maximum. Automatic system calibration Usually called pattern center calibration but also considers sample-screen distance and detector tilt. 05/04/

12 Specific feature: In-situ screen positioning 10kV Spatial distribution of backscattered electrons is a function of WD=22.6mm 60 - phase density - acceleration voltage - surface tilt - working distance - Spatial distribution of BSE. The straight lines mark the direction of intensity maximum. Automatic system calibration Usually called pattern center calibration but also considers sample-screen distance and detector tilt. 05/04/

13 Specific feature: In-situ screen positioning 10kV Spatial distribution of backscattered electrons is a function of WD=22.6mm 60 - phase density - acceleration voltage - surface tilt - working distance - Spatial distribution of BSE. The straight lines mark the direction of intensity maximum. Automatic system calibration Usually called pattern center calibration but also considers sample-screen distance and detector tilt. 05/04/

14 Specific feature: In-situ screen positioning 10kV Spatial distribution of backscattered electrons is a function of WD=22.6mm 60 - phase density - acceleration voltage - surface tilt - working distance - Spatial distribution of BSE. The straight lines mark the direction of intensity maximum. Automatic system calibration Usually called pattern center calibration but also considers sample-screen distance and detector tilt. 05/04/

15 Specific feature: ARGUS FSE / BSE detectors ARGUS multiple electron detection system with optimally arranged single detectors. BSE detectors perpendicular aligned to the tilted surface. FSE detectors capture three orientation contrast images simultaneously. Parallel acquisition of the SE image. Brilliant images due to low signal loss (integrated electronics). 05/04/

16 Area of interest FSE/BSE imaging system SE images have very low contrast. It is not easy to find region of interest. 05/04/

17 Area of interest FSE/BSE imaging system SE images have very low contrast. It is not easy to find region of interest. Common FSE detectors already show an enormous improvement. 05/04/

18 Area of interest FSE/BSE imaging system SE images have very low contrast. It is not easy to find region of interest. Common FSE detectors already show an enormous improvement. However, color-coded FSE images can reveal much more detail. 05/04/

19 Iron meteorite (white plessite) 05/04/

20 Iron meteorite (white plessite) 05/04/

21 PM martensitic steel 05/04/

22 PM martensitic steel 05/04/

23 Multiphase steel 05/04/

24 Multiphase steel 05/04/

25 Deformed Tantalum 05/04/

26 Rocks (variable pressure mode) 05/04/

27 Rocks (variable pressure mode) 05/04/

28 ESPRIT EBSD software: Some selected differences Single user interface: separate or combined use of EBSD and EDS for acquisition and post processing Data streaming: nothing is lost, no pattern and no spectrum Data access: at any time Real-time data processing: simultaneous data interpretation Real-time data visualization: synchronously updated pole figures, IPFs, orientation maps, misorientation tools, etc.) Assistants: automatic setup of the EBSD camera; automatic detector calibration Superfast re-indexing: up to points/s (single phase) Intensity simulation: different tools for realistic band intensity prediction 05/04/

29 Phase assignment: EBSD & EDS? Identical chemistry but different crystal structure SiO 2 : TiO 2 : ZrO 2 : CaCO 3 : Fe 2 SiO 4 : Fe x O y : Quartz, Cristobalite, Tridymite Rutil, Anatase Arkelite, Zirconia, Baddeleyite Calcite, Aragonite Ringwoodite, Fayalite Hematite, Magnetite, Wuestite 05/04/

30 Phase assignment: EBSD & EDS? Identical chemistry but different crystal structure SiO 2 : TiO 2 : ZrO 2 : CaCO 3 : Fe 2 SiO 4 : Fe x O y : Quartz, Cristobalite, Tridymite Rutil, Anatase Arkelite, Zirconia, Baddeleyite Calcite, Aragonite Ringwoodite, Fayalite Hematite, Magnetite, Wuestite Identical crystal structure but different composition Periclase (MgO), Galena (PbS), Lime (CaO), Wuestite (FeO) Spinel, Magnetite, Gahnite Calcite (CaCO 3 ), Siderite (FeCO 3 ), Magnesite (MgCO 3 ) Sphalerite (ZnS), Chalcopyrite (CuFeS 2 ), Pyrite (FeS 2 ), Galena (PbS) Baryte (BaSO 4 ), Celestine (SrSO 4 ), Anglesite (PbSO 4 ) 05/04/

31 Differences between EBSD & EDS EBSD is a single-crystalline technique. The crystal must be bigger than the beam diameter. The information depth of EBSD is a few 10nm. The requirements on sample preparation are clearly higher. The information depth is different to EDS (~100 times smaller). EBSD works with unusually highly-tilted samples. Spatial resolution in x and y direction is different. Topography effects are difficult to correct for EDS. EBSD pattern acquisition is usually faster than EDS. Nevertheless, SDD technology fulfills the requirements. 05/04/

32 Challenges Sample preparation (sophisticated, especially for multiphase materials) Local charging (inhomogeneous coating, variation of acquisition conditions) Inconsistent EBSD and EDS data ( matrix effect : particle too small or layers too thin) Intensity prediction of EBSD patterns (instead of band intensities reflector intensities are still in use) Stable data transfer at high speed (especially if EBSD and EDS are collected simultaneously) 05/04/

33 Common application fields Phase identification using single patterns (acquisition time in the scale of several 10 s), EDS spectra captured on certain positions where an indexing was impossible Phase assignment by superposition of predefined element maps 1. Successive measurement of EDS and EBSD maps using the EDS information for phase recognition. 2. Simultaneously measured but subsequently analyzed EBSD and element distribution maps. Reassignment of phases by manually defined EDS thresholds. Disadvantages: 1. One needs to know all required elements. 2. It is comparatively slow. 05/04/

34 EBSD & EDS integration: The difference! In comparison to predefined element distribution maps acquisition and interpretation of complete EDS spectra & EBSD patterns at any point of a map are standard. This permits a subsequent selection of any element distribution, element quantification at any point, processing and post-processing of EDS and EBSD data at any time. The sophisticated combination of EBSD and EDS does not slow down the measurement speed significantly. 05/04/

35 Examples 1. Discrimination of phases forming similar patterns 2. Offline phase identification

36 Friction welded Al-Cu bar Al & Cu have the same crystal structure and similar lattice parameters. Using EBSD they are hard to distinguish. So also orientation analyses are useless Thus, the phase assignment fails and displays mostly Cu which is on first position in the phase list. The orientations however are correctly determined. EBSD phase map Cu Al EDS: element map (Qmap) Nevertheless, the simultaneously acquired EDS data would permit a clear separation of both materials. Use EBSD & EDS together! ZEISS Supra 55 VP, 15kV, 15nA 05/04/

37 Real-time interpretation ZEISS Supra 55 VP, 15kV, 15nA 1. Simultaneous acquisition of EBSD patterns and EDX spectra 2. Parallel orientation determination and EDS interpretation to assign the correct phase. Cu Al Maximum speed * for EBSD/EDS acquisition & real-time interpretation: 730 indexed points/sec ( * a suitable detector & sufficient patterns assumed) 05/04/

38 New phase? Re-interpretation! ZEISS Supra 55 VP, 15kV, 15nA Friction welded sample of Al with Cu. 05/04/

39 New phase? Re-interpretation! ZEISS Supra 55 VP, 15kV, 15nA Friction welded sample of Al with Cu. 05/04/

40 New phase? Re-interpretation! ZEISS Supra 55 VP, 15kV, 15nA Friction welded sample of Al with Cu. Mechanical alloying discovered: Al 4 Cu 9 (green) 05/04/

41 New phase? Re-interpretation! ZEISS Supra 55 VP, 15kV, 15nA Friction welded sample of Al with Cu. Mechanical alloying discovered: Al 4 Cu 9 (green) Reanalysis speed: 1440 points/s Duration: 5:43 min 05/04/

42 Example 2 Aim: Sample: Hardware: EBSP resolution: Acquisition speed: Phase recognition and distribution known: Ferrite; unknown: oxides and sulfides Power plant heat exchanger steel pipe EBSD: e - Flash HR EDS: XFlash x120 pixels (10x10 binning) Simultaneous EBSD/EDS fps Experimental: Pipe from new generation of coal power plant CO 2, CO and SO 2 atmosphere High pressure water vapor Temperature ~575ºC 05/04/

43 Pattern quality map Steel pipe ~2.5Cr 0.3Si Corrosion layer Temperature: ~575ºC Atmosphere: CO 2, CO and SO 2 05/04/

44 Phase distribution map using Ferrite Steel pipe Raw phase map Ferrite No data cleaning! Map size: 800x600 Pixel size: 0.25 μm 05/04/

45 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

46 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

47 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

48 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

49 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

50 Raw EDS data Steel pipe EDS HyperMap Average counts/spectrum ~1100 Main elements: Fe, Cr, O, S, Si Map size: 800x600 Pixel size: 0.25 μm 05/04/

51 Phase ID by EDS quantification How it works 1. (Manual) Selection of candidates from databases using the EDS spectrum and the EBSD pattern. 2. Quantification of the locally acquired spectrum. 3. Comparison with the chemistry of possible candidates. 4. Assignment of the phase by EDS. 5. Indexing by EBSD. 05/04/

52 Offline phase ID: Sulfide 05/04/

53 Offline phase ID: Sulfide 05/04/

54 Offline phase ID: Sulfide Troilite (FeS) 05/04/

55 Offline phase ID: Silicate 05/04/

56 Offline phase ID: Silicate Fayalite (Fe 2 SiO 4 ) 05/04/

57 Offline phase ID: Oxides 05/04/

58 Offline phase ID: Spinel Magnetite (Fe 3 O 4 ) 05/04/

59 Offline phase ID: Spinel Magnetite (Fe 3 O 4 ) Chromite (FeCr 2 O 4 ) 05/04/

60 Offline phase ID: Spinel Magnetite (Fe 3 O 4 ) Chromite (FeCr 2 O 4 ) 05/04/

61 Reanalysis with EDS quantification Phase map after reanalysis Ferrite (cub) Troilite (hex) Fayalite (ort) Magnetite (cub) Chromite (cub) No data cleaning! Map size: 800x600 Pixel size: 0.25 μm 05/04/

62 There is something missing Phase map after reanalysis Ferrite (cub) Troilite (hex) Fayalite (ort) Magnetite (cub) Chromite (cub) No data cleaning! Map size: 800x600 Pixel size: 0.25 μm 05/04/

63 Iron oxides 05/04/

64 Iron oxides Magnetite (Fe 3 O 4 ) Wuestite (FeO) 05/04/

65 Iron oxides Magnetite (Fe 3 O 4 ) Wuestite (FeO) 05/04/

66 Still another oxide? 05/04/

67 Still another oxide? Hematite (Fe 2 O 3 ) 05/04/

68 Final phase distribution map Phases map Ferrite (cub) Troilite (hex) Fayalite (ort) Chromite (cub) Magnetite (cub) Wuestite (cub) Hematite (tri) No data cleaning! Reindexing + quantification speed: ~620 pps total reanalysis time: 12min 51sec 05/04/

69 Final orientation map Orientation map No data cleaning! Map size: 800x600 Pixel size: 0.25 μm 05/04/

70 Summary Example 1 Real-time discrimination of known phases: Al Cu Post-processing considering also additional phases: Al 4 Cu 9 Example 2 Offline (still manual) phase ID Offline phase discrimination based on EDS quantification Seven phases: Fe, FeO, Fe 2 O 3, Fe 3 O 4, FeCr 2 O 4, FeS, Fe 2 SiO 4 Total SEM occupation: 15 min SEM preparation, 80 min measurement time, 5 min sample withdrawal 05/04/

71 Take home message CrystAlign consists of a powerful combination of hard- and software which attracts attention by totally new approaches. Combined with an easy-to-use interface and special assistants, parallel acquisition, interpretation and visualization of data makes EBSD interesting for everyone. The applied data streaming combined with the superfast reindexing enables multiple and rapid data post-processing. The developed combination of EBSD and EDS points a new level in microanalysis. CrystAlign is presently the only existing analytical system which can simultaneously acquire and quantify EDS spectra and EBSD patterns in a breathtaking speed. 05/04/

72 Copyright 2011 Bruker Corporation. All rights reserved. Innovation with Integrity

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