sem/eds-coseva advanced trs cm000015583 – nanoshell

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covalentmetrology.com CM000015583 – Nanoshell SEM/EDS-COSEVA Advanced TRS 30 September, 2020

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covalentmetrology.com

CM000015583 – Nanoshell SEM/EDS-COSEVA Advanced TRS

30 September, 2020

Contents

Job Description 3Summary 4Sample Description 5System Used 6Results and Analysis 7 – 21

2

Job Description3

• Determine the elemental composition of particles in liquid suspension– Make special note of similarity or dissimilarity to zeolite, especially clinoptilolite– If clinoptilolite is found, the sample is to be compared to a reference

Clinoptilolite4

Clinoptilolite:(Na,K,Ca)2-3Al3(Al,Si)2Si13O36·12H2O

Range of Possible Stoichiometries for Clinoptilolite:

(Na,K,Ca)2-3Al3Si15O36·12H2O

(Na,K,Ca)2-3Al4Si14O36·12H2O

(Na,K,Ca)2-3Al5Si13O36·12H2O

Element Clinoptilolite

Typical reference compositional % for Clinoptilolite:

*Na, K, Ca, Al, and Si can (slightly) vary.

Summary5

• 3 sites are analyzed via EDS for composition with 5 kV incident beam• After corrections, all display a reasonable match to clinoptilolite• All particles show trace levels of Mg (used in processing buffer)• Particles are clumped together due to drying on the Cu/C specimen plate.• Particles range in size from 20 to 100 nm

Element Part. 1 Part. 2 Part. 3 Average

Composition*, Atomic %

Approximate Stoichiometry for Product:(Na,K,Ca)2-3Al3Si13O31·17H2O

Clinoptilolite

Sample Description6

• Liquid sample is drop-cast on Cu tape – Chosen for its dissimilarity to target Zeolite and Clinoptilolite

• Dried under vacuum at room temperature• Sample is not coated prior to measurement

Sample in-situ

Liquid Sample in Original Packaging

Drop-cast sampleon Cu and C tape

System Used7

SEM images and EDS maps were obtained on a FEI Scios Dualbeam with an Oxford 150mm2 detector.

Results and Analysis

SEM Images9

SEM Images10

Site 1 – Results 11

Site 1 – EDS Maps12

Site 1 – EDS Maps13

Site 1 – Spectrum14

Site 2 – Results 15

Site 2 – EDS Maps16

Site 2 – EDS Maps17

Site 2 – Spectrum18

Site 3 – Results 19

Site 3 – EDS Maps20

Site 3 – EDS Maps21

Site 3 – Spectrum22

covalentmetrology.com