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Enterprise for Multi - scale Research of Materials Microanalysis and Atomic-Resolution Characterization of Boron-rich Ceramics Martin P. Harmer & Christopher J. Marvel Lehigh University How We Fit Technical Approach Key Accomplishments Key Goals Major Results Impact Transitions to ARL, within CMRG and to other CMRGs UNCLASSIFIED UNCLASSIFIED Sample Characterization ac-STEM (JEOL ARM200-CF) Sample Preparation - Focused Ion Beam (FEI Scios) Aberration-corrected Scanning Transmission Electron Microscopy Interfacial Design of Armor Ceramics to Enhance Mechanical Performance Engineer grain boundary complexions in armor ceramics Develop and implement light element microanalysis via z-factor quantification Study SiB 6 :B 4 C and B:B 4 C diffusion couples to evaluate bulk and grain boundary thermodynamics 1. Design microstructures and interfaces (e.g. grain boundaries) to modify fracture mechanisms 2. Develop and implement quantitative microanalysis of light elements (e.g. B, C, and O) 1. All raw data is supplied to ARL and CMRG collaborators 2. New techniques and z-factor approach/computer code can be shared with CMRG collaborators Final Equations Validation of z-factor Microanalysis using SiB 6 Standard Development of z-factor Microanalysis Diffusion Zone and Region of Interest B 4 C Diffusion Zone SiB 6 B 6 O Diffusion Zone SiB 6 B 6 O 50 mm 15 mm TEM Sample STEM-EDS Map of B 4 C:B 6 O Diffusion Line Bulk Phase Quantification (at.%) Boron Carbon Oxygen Silicon B 4 C 85.7 ± 0.4 11.0 ± 0.4 1.2 ± 0.2 2.2 ± 0.3 B 6 O 86.8 ± 0.7 2.2 ± 1.1 10.4 ± 2.0 0.7 ± 0.3 Boron Carbon Oxygen Silicon B 4 C N/A N/A 0.4 ± 0.4 3.3 ± 0.6 B 6 O N/A 1.1 ± 3.2 N/A 3.7 ± 1.0 1. Interfacial design and new microanalysis techniques can be used to develop other materials relevant to ARL and the CMRG 2. Atomic-resolution capabilities can be applied to study local chemistry differences of amorphization bands or planar defects z-factor microanalysis includes a built-in absorption correction which is necessary to quantify EDS results Elemental mapping and grain boundary excess coverage measurements are possible Grain Boundary Quantification (atoms/nm 2 ) B 4 C Amorphization Band Y-doped B 6 O Grain Boundary Thermodynamic Evaluation of B 4 C:SiB 6 Diffusion Couple
Transcript
Page 1: Microanalysis and Atomic-Resolution Characterization of Boron … · 2018-10-18 · Validation of z-factor Microanalysis using SiB 6 Standard Development of z-factor Microanalysis

Enterprise for Multi-scale Research of Materials

Microanalysis and Atomic-Resolution

Characterization of Boron-rich Ceramics

Martin P. Harmer & Christopher J. Marvel

Lehigh University

How We Fit Technical Approach Key Accomplishments

Key Goals

Major Results

Impact

Transitions to ARL, within

CMRG and to other CMRGs

UNCLASSIFIED

UNCLASSIFIED

Sample Characterization – ac-STEM

(JEOL ARM200-CF)

Sample Preparation - Focused Ion Beam

(FEI Scios)

Aberration-corrected Scanning Transmission Electron Microscopy

Interfacial Design of Armor Ceramics to Enhance Mechanical Performance

• Engineer grain boundary complexions in armor ceramics

• Develop and implement light element microanalysis via z-factor quantification

• Study SiB6:B4C and B:B4C diffusion couples to evaluate bulk and grain boundary

thermodynamics

1. Design microstructures and interfaces (e.g. grain boundaries)

to modify fracture mechanisms

2. Develop and implement quantitative microanalysis of light

elements (e.g. B, C, and O)

1. All raw data is supplied to ARL and CMRG collaborators

2. New techniques and z-factor approach/computer code can be

shared with CMRG collaborators

Final Equations

Validation of z-factor Microanalysis using SiB6 Standard

Development of z-factor Microanalysis

Diffusion Zone and Region of Interest

B4C Diffusion Zone SiB6B6O

Diffusion Zone SiB6B6O

50 mm

15 mm

TEM Sample

STEM-EDS Map of B4C:B6O Diffusion Line

Bulk Phase Quantification

(at.%)

Boron Carbon Oxygen Silicon

B4C 85.7 ± 0.4 11.0 ± 0.4 1.2 ± 0.2 2.2 ± 0.3

B6O 86.8 ± 0.7 2.2 ± 1.1 10.4 ± 2.0 0.7 ± 0.3

Boron Carbon Oxygen Silicon

B4C N/A N/A 0.4 ± 0.4 3.3 ± 0.6

B6O N/A 1.1 ± 3.2 N/A 3.7 ± 1.0

1. Interfacial design and new microanalysis techniques can be used to

develop other materials relevant to ARL and the CMRG

2. Atomic-resolution capabilities can be applied to study local chemistry

differences of amorphization bands or planar defects

• z-factor microanalysis includes a built-in absorption correction which

is necessary to quantify EDS results

• Elemental mapping and grain boundary excess coverage

measurements are possible

Grain Boundary Quantification

(atoms/nm2)

B4C Amorphization Band Y-doped B6O Grain Boundary

Thermodynamic Evaluation of B4C:SiB6 Diffusion Couple

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