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Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)

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Presentation on theme: "Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)"— Presentation transcript:

1 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM) - construction, components, features and applications

2 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- Electron gun Vacuum tube - Tungsten filament - Lanthanum hexaboride (LaB6) single crystal - field emission gun Focussed e - beam - accelerating voltage 20 – 200 keV SEM construction, components and features Spot size – nm to m range Magnification: 100 – 200,000 x Resolurion: 0,7 nm to 50 nm Electron optics Objective (final lens) JEOL JSM-890 field emission: Magnification: 900,000 x 35 keV, Resolurion: 0,7 nm Microstructure of the specimen surface

3 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Sample (one / several) e-e- Condensing magnetic coils SEM construction, components and features Objective (final lens) Electron optics Au: sputter coater

4 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- Sample Feature: images of morphology or topology - 3-d view Scan coils Scan mode SEM construction, components and features Objective (final lens) Condensing magnetic coils Electron optics

5 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- Scan coils Objective (final lens) Secondary e - 0,1 - 1 eV Topography Sample Amplifier & detector SEM construction, components and features Condensing magnetic coils B/W photo CCD matrix www video PC control

6 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- Secondary X rays (element microanalysis, X-ray mapping) Detector Sample SEM construction, components and features Condensing magnetic coils Objective (final lens) Scan coils WD(crystal)S: B – Am, EDS (Si,Ge,Li, Be): B–U(AM), spot 1 m, 0,1% EPMA

7 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- EBS: crystallography, EBSD: local phase identification and orientation meas., EBS mapping: sp. lattice features, grain boundary misorientation Scan coils Back scattered e - 50-200 keV Atomic Nr, topogr. Sample Amplifier & detector SEM construction, components and features Condensing magnetic coils Objective (final lens)

8 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- Magnification: up to 50,000 x, resolution 10 nm. Sample E (environmental) SEM Environment: T: -200 to +1000 o C Humidity, Atmosphere Real time video VHS recording - Effect of wetting/drying on fibres. - Water reactions with cement to produce bulk properties, -Soil science, catalysis, -Polymers, ceramics, - - Microelectronics.

9 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD PbO 2 crystals morphology vs. electrolyte concentration 6 M, 1.34 s.g.5 M, 1.28 s.g. Source: D. Pavlov, A. Kirchev, M. Stoycheva and B. Monahov, Influence of H2SO4 concentration on the mechanism of the processes and on the electrochemical activity of the Pb/PbO2PbSO4 electrode, accepted for publication in J.Power Sources, 2004

10 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD 2.8 M, 1.17 s.g. 1.56 M, 1.095 s.g. PbO 2 crystals morphology vs. electrolyte concentration Source: D. Pavlov, A. Kirchev, M. Stoycheva and B. Monahov, Influence of H2SO4 concentration on the mechanism of the processes and on the electrochemical activity of the Pb/PbO2PbSO4 electrode, accepted for publication in J.Power Sources, 2004

11 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD 0.18 M, 1.010 s.g. 0.5 M, 1.030 s.g. PbO 2 crystals morphology vs. electrolyte concentration Source: D. Pavlov, A. Kirchev, M. Stoycheva and B. Monahov, Influence of H2SO4 concentration on the mechanism of the processes and on the electrochemical activity of the Pb/PbO2PbSO4 electrode, accepted for publication in J.Power Sources, 2004

12 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Our secret goal: green battery, 100% natural products Nephrolepis (fern) Polypodium (fern)

13 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD PAM, charged, after thermal rise 1 m Source: D. Pavlov, B. Monahov, and A. Kirchev, to be published

14 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD NAM, formed, before thermal rise 1 m3.3 m Source: D. Pavlov, B. Monahov, and A. Kirchev, to be published

15 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD NAM, charged, after thermal rise 1 m Source: D. Pavlov, B. Monahov, and A. Kirchev, to be published

16 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Determinations in PAM/AMCL/CL 1.XRD: - phase composition, - average crystallite size; 2.SEM: - crystal morphology, - structure SGT positive plate structure studies setup Sample collecting points Pb CL AMCLPAM Pb strap grid interface - sample collecting point

17 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Morphology of PbO 2 in the corrosion layer dense aggregates on the metal surface fine, globular, hydrated PbO 2 particles, almost no pores

18 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD dense structure porous structure Morphology of PbO 2 in the AMCL

19 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD e-e- TEM construction, components and features The internal structure of the specimen (2-d imaging) Electron gun U acc - up to 1000 keV Sample: 0,2 m Magnification: 350 - 600,000 x Resolurion: down to 0,2 nm JEOL JEM-4010 - atoms Magnification: 2,000,000x 40-100 keV, Resolurion: 0,15 nm Mesh, goniometer specimen stages Secondary X rays (element microanalysis) TEM microprobe TEM nanoprobe STEM EDS CCD camera Cryogenic facility

20 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Source: D. Pavlov, I. Balkanov, and P. Rachev, J. Electrochem. Soc., 134 (1987) 2390. a: TEM micrograph of an active mass agglomerate after discharge; b: electronogram of the crystals in the defined area with interpretation of its interplanar spacings TEM micrograph and electron diffractogram of a PbO 2 particle

21 Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD 1.Structure of the Pb/PbSO 4 electrode system. Membrane model of PbSO 4. 2.Structure of the Pb/PbO/PbSO 4 electrode system. Semiconductor model of PbO n. 3.Structure of PAM. PbO 2 agglomerates, aggregates and particles. Hydrated structures in PAM and in the corrosion layer. Gel-crystal model of PbO 2. Influence of the electrolyte concentration on the crystal morphology of PbO 2. 4.Structure of NAM. Skeleton and energetic structures. 5.Structure of the CL. CL/AMCL/PAM model. 6.Mapping of PAM and the corrosion layer. Battery knowledge developed using SEM/TEM microscopy

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