IONTOF. Latest Developments in 2D and 3D TOF-SIMS Analysis. Surface Analysis Innovations and Solutions for Industry 2017 Coventry

Transcription

1 Latest Developments in 2D and 3D TOF-SIMS Analysis Surface Analysis Innovations and Solutions for Industry 2017 Coventry Matthias Kleine-Boymann Regional Sales Manager Heisenbergstr Münster Germany IOTOF

2 Outlook > Basic introduction into SIMS > The principle of TOF-SIMS > The different operation modes of TOF-SIMS instruments - Spectroscopy - Imaging - Depth profiling - 3D Analysis > Combination of topography and TOF-SIMS 2

3 Secondary Ion Mass Spectrometry (SIMS) Ion - Solid interaction Excitation > Bombardment with primary ions (Ga, Bi n, O 2, Cs, Ar, Xe, C 60, Ar n, O n...) > Energy kev Collision cascade in solid Results > Desorption of neutrals, secondary ions (/-) and electrons > area 5-10 nm diameter > depth of origin 1-2 monolayers > Implantation of primary ions > Atoms relocation (mixing) > Damaging of organic molecules 3

4 Time-of-Flight Secondary Ion Mass Spectrometry > High sensitivity High transmission Parallel mass detection > High mass resolution 200 u > High mass accuracy 1-10 ppm > High lateral resolution < 50 nm at moderate mass resolution < 500 nm at high mass resolution > High mass range up to 12,000 u > Advantageous for charge compensation due to pulsed ion beam 4

5 Superior Performance for all SIMS Applications 5

6 Modes of Operation Quasi non-destructive surface analysis of the outer monolayers Elemental and molecular information Resolution: 200u Chemical mapping of the surface Lateral distribution of elements and molecules Lateral resolution down to 50 nm Parallel acquisition of all masses / images Mass range: 12,000 u ppm/ppb sensitivity Surface Spectrometry Surface Imaging Depth Profiling 3D Analysis Analysis of the in-depth distribution Elemental and molecular information From a few nm to several µm Depth resolution < 1 nm Combination of imaging and in-depth information Elemental and molecular information 6

7 Modes of Operation Quasi non-destructive surface analysis of the outer monolayers Elemental and molecular information ppm/ppb sensitivity Chemical mapping of the surface Lateral distribution of elements and molecules Lateral resolution down to 50 nm Parallel acquisition of all masses / images Surface Spectrometry Surface Imaging Depth Profiling 3D Analysis Analysis of the in-depth distribution Elemental and molecular information Depth resolution < 1 nm From a few nm to several µm Combination of imaging and in-depth information Elemental and molecular information 7

8 PMMA / PS Polymer Blend 30 x 30 µm² Surface Imaging: 60 kev, Bi 3, FoV: 30 µm 2 C 3 D 5 C 4 D 5 O C 7 D 9 O PMMA m/z C 6 H 5 C 7 H 7 C 9 H 7 PS m/z 8

9 Modes of Operation Quasi non-destructive surface analysis of the outer monolayers Elemental and molecular information ppm/ppb sensitivity Chemical mapping of the surface Lateral distribution of elements and molecules Lateral resolution down to 50 nm Parallel acquisition of all masses / images Surface Spectrometry Surface Imaging Depth Profiling 3D Analysis Analysis of the in-depth distribution Elemental and molecular information Depth resolution < 1 nm From a few nm to several µm Combination of imaging and in-depth information Elemental and molecular information 9

10 Intensity [counts] Diffusion in Polycrystalline Metal Oxides Sample profile from total area Cr Fe Y > Polycrystalline metal oxide La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 2.8 > Layer of Cr, Fe, Y > Diffusion study for Cr, Fe, Y 3 10 Measurement Y > Sputtering: DSC EI gun with 1 kev O2 Fe > Analysis: Ga gun in image mode field of view 60 x 60 µm² 2 10 Cr Depth [nm] 11

11 ormalized to Maximum Diffusion in Polycrystalline Metal Oxides Field of View: 62 x62 µm 2 profiles from selected areas total SI image Result > Different slopes for different areas > Diffusion is more pronounced along the grain boundaries selected raster 10 blue: grain boundary region red: inside the grains Y Fe Cr Y Cr Fe Depth [nm] (Sample provided by Prof. Martin, RWTH Aachen, Germany) 12

12 Modes of Operation Quasi non-destructive surface analysis of the outer monolayers Elemental and molecular information ppm/ppb sensitivity Chemical mapping of the surface Lateral distribution of elements and molecules Lateral resolution down to 50 nm Parallel acquisition of all masses / images Surface Spectrometry Surface Imaging Depth Profiling 3D Analysis Analysis of the in-depth distribution Elemental and molecular information Depth resolution < 1 nm From a few nm to several µm Combination of imaging and in-depth information Elemental and molecular information 13

13 Fully Integrated Gas Cluster Source for organic depth profiling 3D Analysis 90 pulsing system gas inlet skimmer ioniser lens source DC mass filter pre-chopper Faraday cup deflection crossover skimmer ioniser lens crossover buncher gas inlet chopper deflection target lens target 14

14 Organic Depth Profiling of OLED s Test Structure layer construction layer composition characteristic SI signal (MH) C 44 H nm Bphen ETL / HTL (electron transport- / hole blocking layer O O Al O 585 u (2M-R) C 45 H 30 Al 2 5 O u 10 nm Alq3 30 nm Ir(ppy) 3 / TCTA 10 nm a-pd Flourescent Host Green Dopant / Phosphorescent Host HTL Ir Ir(ppy) 3 : (M) : C 33 H 24 Ir 3 : 655 u TCTA: (MH) : C 54 H 37 4 : 741 u (MH) C 44 H nm BPAPF HTL (hole transport layer) 589 u (M) C 73 H u ITO Substrate In 2 O 3 / SnO In 113 u 15

15 Intensity (counts) Alq3 A-PD Organic Depth Profiling of OLED s test structure 3D Analysis Bphen Ir(ppy) 3 TCTA BPAPF ITO C 44 H 29 2 (585 u) - C 45 H 30 5 O 3 Al 2 (774 u) C 33 H 24 3 Ir (655 u) - C 54 H 37 4 (741 u) - C 44 H 34 2 (589 u) C 73 H 52 2 (956 u) In (113 u) Depth (nm) 16

16 3D Analysis of a Real OLED Device 3D Analysis 17

17 Outlook > > > > Combination of topography and TOF-SIMS 18

18 Influence of Topography and Sputter Rates Model Sample TOF-SIMS 3D Data initial TOF-SIMS does not provide any information about Topography Changes of the topography due to different sputter rates final 19

19 Concept of the Combined Instrument Model Sample SPM Surface Topography TOF-SIMS 3D Data = True 3D Data initial final 20

20 View into the TOF.SIMS 5 chamber Space for SPM..? 21

21 Combined TOF.SIMS 5 SPM Instrument anoscan UHV SPM module Flexure stage scanner with 80 x 80 x 10 µm³ 4-axes high precision piezo stage (XYZR) Various static and dynamic SPM modes Fast cantilever exchange (storage of 4) High precision piezo stage (XYZR) speed: 10 mm/s encoder resolution: 10 nm positioning accuracy: < 1 µm 22

22 TOF-SIMS SPM Setup 3D Chemical Analysis of Inorganic and Organic anostructures nm Overlay 6.0µm 0.00 nm TOF-SIMS module SPM module PS PMMA on SPM Topography Z axis X axis Y axis high precision sample transfer (accuracy < 1 µm) 23

23 3D Overlay - Volume Plot Al Si Ca Mo In Ba TOF-SIMS data only 24

24 3D Volume Plot vs. 3D Image Al Si Ca Mo In Ba Combination of TOF-SIMS SPM data 25

25 Cross Section through 3D Image Al Si Ca Mo In Ba Combination of TOF-SIMS SPM data 26

26 Depth / nm Depth Scale Calibration in SIMS 100 SPM Surface Profile Distance / µm SPM Profiler Mode Depth profiles and 3D data sets need depth calibration (t z) Crater depth needs to be measured relative to the initial surface Typical SIMS crater dimensions: µm Limited SPM scan range: 80 µm 27

27 Topography difference* / nm Topography* / nm Curved Glass Surface with Polymer Coating initial surface initial surface * arbitrary levelling sputtered surface Scan length / µm sputtered surface difference profile scan length / µm 28

28 Summary TOF-SIMS covers a wide range of applications Inorganic and organic surface analysis Microanalysis with high lateral resolution (<60 nm) Inorganic and organic in-depth information Large area mapping Thin layer depth profiling (from a few nm down to 10 µm) Interface analysis Combination of topography and chemistry 29

29 Thank you for I your O V A T I V E attention! S U R F A C E A A L Y S I S Matthias Kleine-Boymann Regional Sales Manager matthias.kleine-boymann@iontof.com Heisenbergstr Münster Germany IOTOF