Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries...
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Transcript of Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries...
![Page 1: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/1.jpg)
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
![Page 2: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/2.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
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 xResolurion: 0,7 nm to 50 nm
Electron optics
Objective (final lens)JEOL JSM-890 field emission:
Magnification: 900,000 x35 keV, Resolurion: 0,7 nm
Microstructure of the specimen surface
![Page 3: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/3.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
Sample (one / several)
e-
Condensing magnetic coils
SEM construction, components and features
Objective (final lens)
Electron optics
Au: sputter coater
![Page 4: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/4.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
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
![Page 5: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/5.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
e-
Scan coils
Objective (final lens)
Secondary e-
0,1 - 1 eVTopography
Sample Amplifier & detector
SEM construction, components and features
Condensing magnetic coils
B/W photoCCD matrix
wwwvideo
PC control
![Page 6: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/6.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
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
![Page 7: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/7.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
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 keVAtomic Nr, topogr. Sample Amplifier &
detector
SEM construction, components and features
Condensing magnetic coils
Objective (final lens)
![Page 8: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/8.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
e-
Magnification: up to 50,000 x, resolution 10 nm.
Sample
E (environmental) SEM
Environment:T: -200 to +1000oC
Humidity, Atmosphere
Real time videoVHS recording
- Effect of wetting/drying on fibres. - Water reactions with cement to produce bulk properties, -Soil science, catalysis, -Polymers, ceramics, -- Microelectronics.
![Page 9: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/9.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
PbO2 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
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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.
PbO2 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
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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.
PbO2 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
![Page 12: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/12.jpg)
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)
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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
1 m
1 m
1 m
Source: D. Pavlov, B. Monahov, and A. Kirchev, to be published
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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
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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 1 m
Source: D. Pavlov, B. Monahov, and A. Kirchev, to be published
![Page 16: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/16.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
Determinations in PAM/AMCL/CL1. XRD: - phase composition,
- average crystallite size;2. SEM: - crystal morphology,
- structure
SGT positive plate structure studies setupSample collecting points
Pb CL AMCL PAM
PAM
Pb strap gridinterface
- sample collecting point
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Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
Morphology of PbO2 in the corrosion layer
dense aggregates on the metal surface fine, globular, hydrated PbO2 particles, almost no pores
![Page 18: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/18.jpg)
Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
dense structure
porous structure
Morphology of PbO2 in the AMCL
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Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
e-
TEM construction, components and features
The internal structure of the specimen (2-d imaging)
Electron gunUacc - up to 1000 keV
Sample: 0,2 m
Magnification: 350 - 600,000 xResolurion: down to 0,2 nm
JEOL JEM-4010 - atomsMagnification: 2,000,000x
40-100 keV, Resolurion: 0,15 nm
Mesh, goniometer specimen stages
Secondary X rays (element microanalysis)
TEM microprobe
TEM nanoprobe
STEMEDS
CCD camera Cryogenic facility
![Page 20: Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES WP 2. Lead-acid batteries for POEMES, LABD Scanning Electron Microscopy (SEM)](https://reader035.fdocuments.net/reader035/viewer/2022070306/55165a19550346c6758b5d30/html5/thumbnails/20.jpg)
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 PbO2 particle
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Centre of Excellence POEMES, IEES (CLEPS), BULGARIAN ACADEMY OF SCIENCES
WP 2. Lead-acid batteries for POEMES, LABD
1. Structure of the Pb/PbSO4 electrode system. Membrane model of PbSO4.
2. Structure of the Pb/PbO/PbSO4 electrode system. Semiconductor model of PbOn.
3. Structure of PAM. PbO2 agglomerates, aggregates and particles. Hydrated structures in PAM and in the corrosion layer. Gel-crystal model of PbO2. Influence of the electrolyte concentration on the crystal morphology of PbO2.
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