Seeing inside lead-acid batteries using neutron imaging. J. M. Campillo-Robles, D. Goonetilleke, N. Sharma, D. Soler, U. Garbe, P.
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1 Seeing inside lead-acid batteries using neutron imaging J. M. Campillo-Robles, D. Goonetilleke, N. Sharma, D. Soler, U. Garbe, P. Türkyilmaz 1
2 2
3 Causes of aging - Electrode degradation: sulfating, corrosion, non-cohesion of active mass (shedding/degradation). - Electrolyte degradation: stratification, water loss. - Faulty manufacturing of cell: paste production, pasting, grid manufacturing, formation of the cell. 3
4 Limitations of lead acid battery 35 Wh/kg 4
5 What is happening inside? We will try to see inside using neutrons First time 5
6 1.- In operando monitoring. 2.- Neutron imaging techniques. 3.- Cell design. 4.- Results 5.- Conclusions Gaston Planté ( ) 6
7 1.- In operando monitoring Monitoring of inner processes to optimize and improve the cell. A lot of sensors developed to check the SOC of the cell (using electrolyte concentration). Unfriendly environment: acid, electrical, small place. 7
8 1.- In operando monitoring Intrusive techniques: - Optic techniques: point measurement. - Equilibrium potential: point measurement. Non-intrusive techniques: - Electric potential of the cell. - Ultrasounds: line measurement. - Holographic Laser Interferometry (HLI): plane measurement. - Neutron Imaging 8
9 2.- Neutron imaging techniques Non-destructive testing for industrial/engineering applications. Advantages over other imaging techniques: - Neutron interaction only with the nucleus. - Neutron pictures are related to the elemental composition of the object. - Greater penetration than gamma rays. Pb Opaque to X rays. Transparent to neutrons. 9
10 2.- Neutron imaging techniques Different elements/compounds have different attenuation coefficients. Two mean attenuation processes: absorption and scattering. scattering Neutron source collimator Target transmission Detector Nuclear reactor Spallation source absorption 10
11 2.- Neutron imaging techniques Two techniques: - Radiography (2D) Shadow image of the investigated sample. - Tomography (3D) Full three-dimensional image of the object is reconstructed from 2D pictures. Already applied in energy storage: Fuel cells, Lithium-Ion Batteries (LIBs), hydrogen storage, nuclear fuel, etc. First time neutron imaging has been used for monitoring lead acid batteries! 11
12 2.- Neutron imaging techniques: Dingo instrument Open Pool Australian Lightwater (OPAL) Reactor Fuel: 30 kg low enriched uranium T = 60 C 20 MW 13 neutron beam instruments Opened in
13 2.- Neutron imaging techniques: Dingo instrument Neutron radiography/tomography - Thermal neutrons ( 25 mev). - Detector: CCD camera + scintillator. Measured area cm. - Spatial resolution: 27 µm. - Average flux at sample (n cm -2 s -1 ): 10 7 (centre of image) (corner of image) Opened in
14 3.- Cell design Only one cell: 1.2 Ah. Neutron friendly case Teflon (PTFE) 14
15 3.- Cell design: electrodes Dry charged commercial plates. 3 negative electrodes 2 positive electrodes 15
16 3.- Cell design: separators Commercial separators in positive plates (not in all cells). Polyethylene hydrogen high attenuation of the beam. 16
17 3.- Cell design: electrical connections 17
18 3.- Cell design: electrolyte Deuterated electrolyte: D 2 SO 4 (Sigma-Aldrich) wt. % in D 2 O, 99.5 atom % D. D 2 O (Cambridge Isotope Laboratories) 99.9 atom % D. Initial concentration (previous activation): 5 M. 18
19 4.- Results 19
20 4.- Results: electrical behaviour C/3 C/3 C/4 Charge-discharge processes: C/5 (0.182 A) C/2 (0.38 A) Problems at higher intensities! 20
21 4.- Results: attenuation Beer-Lambert law of attenuation of radiation valid for neutrons: II = II 0 ee μμμμ. µ - linear attenuation coefficient of the target: µ = µ absorption + µ scattering. d - thickness of the sample. Intensity reduction for different attenuation coefficients 21
22 4.- Results: attenuation Neutron linear attenuation coefficient, µ, for λ = 1.54 Å: ρ (g/cm 3 ) µ (cm -1 ) Pb (porous) PbO 2 (porous) Pb (metal) PbSO D 2 SO 4 (liquid) D 2 O (liquid) Less attenuation in concentrated electrolyte!!! Data obtained from: NIST, Center for neutron research, 22
23 4.- Results: open beam / as measured picture Open beam profile not homogeneous not centred Cell without separators as measured 23
24 4.- Results: as measured pictures Intensity profile as measured in air Electrodes Separators More attenuation at electrodes and separators Cell with separators 24
25 4.- Results: as measured pictures Intensity profile as measured Electrodes Separators Separators cause measurement problems Cell with separators 25
26 4.- Results: as measured pictures Intensity profile as measured Electrodes More attenuation at electrolyte than at electrodes Cell without separators 26
27 4.- Results: corrections Corrections to be performed: - Subtraction of noise (gamma rays). - Correction of open beam profile: 30 % reduction from maximum to minimum. - Correction of battery case. - Fluctuations of reactor beam. 27
28 4.- Results: empty cell More than 70% of the neutrons pass through the cell 28
29 4.- Results: cell with electrodes The electrodes reduce the transmittance from 70% to 40% 29
30 4.- Results: electrolyte Final state after slow charging Final state after fast charging 30
31 4.- Results: neutron tomography Same principle as in X-R tomography. Only one difference: rotating sample. We can decide the cutting plane to analyse. Detailed inner structure. Full image of the cell. 31
32 4.- Results: neutron tomography What can we see? - Inner structure of the electrodes (also through separators). - Active material behaviour. - Inner structural problems. - Sulfation of the electrodes. - Corrosion. Separator Active material Grid Electrode. 32
33 5.- Conclusions - Neutron imaging is complementary to other monitoring techniques. - Only technique with capability to see inside electrodes. - We can see changes in the electrolyte concentration. - Need to improve the experiment. 33
34 We are working on - Optimization of cell design. - Quantification of electrolyte concentration. - Electrolyte stratification analysis. - Active material degradation analysis. - Transport properties of deuterated acid in heavy water. 34
35 Thanks to Cell design: I. Urrutibeaskoa (MU), B. Turhan (YIGITAKU). Cell manufacturing: G. Arrizabalaga (MU), A. Arrillaga (MU), Parra Mekanizatuak. CAD drawing: E. Ruiz de Samaniego (MU), F. Zugasti (MU), I. Perez (MU). FEM simulations: X. Artetxe (MU), L. Oca (MU). Help at ANSTO: J. Pramudita (UNSW), N. Booth (ANSTO). Data processing: F. Rossi (ANSTO), A. Velasco (ANSTO), J. Coslovich (ANSTO). 35
36 Any question? Thank you! Eskerrik asko! Aramaio valley (Basque Country) 36
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