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Material: "Battery Material" The aim of the measurement: particle size distribution etc

Results:
Reduction of particle size by grinding is clearly detectable
. The pore size is reduced by about a factor changing from by SEM evaluation. The morphology changes from
. The crystalline structure , and the crystal size
. From a suspension of 10 g/l solids in water (10,000 ppm) ,

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### EPA-HQ-OPPT-2009-0922

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22/09/2011 Size: 1): SEM The samples were imaged using SEM on representative areas. In the milled sample,

, and , thus,

. SEM Sample 1:

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22/09/2011

SEM Sample 2:

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22/09/2011 2) Size characterization by HG-Porosimetry: Hg-Porosimetry Sample 1:

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22/09/2011

Hg-Porosimetry Sample 2:

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22/09/2011 3) Size distribution from Malvern-Mastersizer:

Presentation of Results

System Parameters Focal Length: Beam Length: Module: Obscuration : Presentation : Analytical Model: Residual : Modifications : Suppress Result Channels: Sample Name: Nr. Measured: 6 Sept 2011 10:05 File: Measurement Nr: Analyzed : 6 Sept 2011 10:05 Path : Comment:

Result Statistics Distribution Type: Concentration: Density: Specific Surface Area

. = Mean Diameter: D (v, 0.5) = D (v, 0.9) = Span : Uni formity:

Size (um) Volume

Under (%) Size

(um) Volume

Under (%) Size

(um) Volume

Under (%) Size

(um) Volume

Under (%)

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22/09/2011 Crystallinity: 4) XRD -Xray Powder Defractometry: Due to the grinding of the sample the peak width in the measured diffraction patterns appears to change slightly

. While the sample has an average crystal size of the ground sample

has only an average crystal size of This result is derived from an exemplary FWHM evaluation only of the strongest diffraction line at about determined. The sample

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22/09/2011 Solubility: 5) X-ray fluorescence: Pretreatment: Sample was dispersed in H 2 O and then fractionated by preparative ultracentrifugation. The supernatant was used to assess the solubility by X-ray fluorescence analysis. In addition, was used t o assess by elemental analysis any possible contaminations by the grinding process. Overview analysis by X-ray fluorescence The X-ray fluorescence is a method for qualitative and quantitative determination of all elements with atomic numbers from 11 (Na), where the detection sensitivity depends both on the matrix and the specific element.