Beamline – a Useful & Must Have (?) Tool

for Industrial Material Science

Development

Ying Shi Sr. Research Scientist Characterization and Materials Processing

April 8, 2014

Characterization and Materials Processing © 2014 Corning Incorporated 2

About Corning

A global company with 160 years of innovation history

Characterization and Materials Processing © 2014 Corning Incorporated 3

My Career Path

1997 Ph.D. in Solid State Physics, Institute of Physics, Chinese

Academy of Science.

1997-1999: 1st post doctor, National Institute for Materials Science, Japan

1999-2001: 2nd post doctor, Kansa State University

2001-2007: 1st industrial job, analytical scientist, Delphi Catalyst, Tulsa, OK

2007-2011: 2nd industrial job, XRD/XRF scientist, Dow Chemical, Midland, MI

2011-current: 3rd industrial job, XRD scientist, Corning Inc., Corning, NY

Characterization and Materials Processing © 2014 Corning Incorporated 4

My 1st National Lab User Experience

ORNL-HTML User program

Best program ever for a

budget tight post doc!

Unfortunately…

Characterization and Materials Processing © 2014 Corning Incorporated 5

My 1st Beamline Experience

APS- 5 DND-CAT

• Free ride provided by the XRD

predecessors of Dow Chemical.

• No worry about budget and

legal issue, just go and do!

• Application on XRD, SAXS,

XAFS.

• Convinced and devoted to

beamline!

Characterization and Materials Processing © 2014 Corning Incorporated 6

My 2nd Beamline Experience

Devoted to synchrotron, the opportunity finally came a year after joining Corning…

• Obtained budget is just the 1st step…

• Headache legal process: NDA,

Proprietary user agreement, WFO…

• Payment process: supplier account set

up, pre-payment…

• Finally it is the fun time: beam time

started!!!

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Application: PDF Analysis of Nanoporous Carbon

Two major attractive:

1. High surface area;

2. Nano sized pores.

Applications:

1. Hydrogen & natural gas storage;

2. Anode for rechargeable battery;

3. Ultracapacitor.

Two step synthesis:

1. Carbonization at N2.

2. Activation: chemical or physical method.

Performance:

1. Capacity: macro properties (surface area & pore size distribution);

2. Lifetime: stability (local structure).

Characterization and Materials Processing © 2014 Corning Incorporated 8

Comparison between in house and Synchrotron

20000

40000

60000

80000

Counts

Position [°2Theta] (Copper (Cu))

10 20 30 40 50 60 70

HS1 HS3 HS2 LS8

(002)

2000

4000

6000Counts

Position [°2Theta] (Copper (Cu))

40 50 60 70

HS1 HS3 HS2 LS8

(100) (004)

(a)In house Cu X-ray 8.04 KeV

0

100000

200000Counts

Position [°2Theta] (Copper (Cu))

10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

HS3 HS2 HS1 LS8

10000

20000

30000

40000

50000

Counts

Position [°2Theta] (Copper (Cu))

30 40 50 60 70 80 90 100 110 120

HS3 HS2 HS1 LS8

(b)NSLS X7B 38.79 KeV (004)

(300)

Characterization and Materials Processing © 2014 Corning Incorporated 9

Data Getting Better After Correction

20000

40000

60000

Counts

Position [°2Theta] (Copper (Cu))

10 20 30 40 50 60 70

HS1

HS3 HS2

LS8

0

2

4

6Counts

Position [°2Theta] (Copper (Cu))

5 10 15

(a) In house Cu x-ray

(b) Raw data of X7B

(c) Corrected and normalized structure factor

(002)

Characterization and Materials Processing © 2014 Corning Incorporated 10

Diffraction Pattern of Represented Samples

0

5

10

Counts

Position [°2Theta] (Copper (Cu))

5 10 15

HS3_140-00325-342Y-SQ HS2_140-00030-44Y-SQ HS1_140-00045-48Y-SQ LS8_140-00024-29Y-SQ

(002)

High small angle

scattering for HS

materials

(100)

Weak or none (004) for HS

(110)

(200) (210) (300)

(004)

(002) shifts, wider peak

indicating disordering.

0

1

2Counts

Position [°2Theta] (Copper (Cu))

8.50 9 9.50

HS3_140-00325-342Y-SQ HS2_140-00030-44Y-SQ HS1_140-00045-48Y-SQ LS8_140-00024-29Y-SQ

Peak width indicating

local disordering

Characterization and Materials Processing © 2014 Corning Incorporated 11

Other Beamlines Approach

CHESS-A2

LNSC, LANL

APS

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Expectation of a Convinced User

• On-time delivery: guaranteed beamtime every cycle with possible

make up time.

• Mail-in service !!!

• Error-proof set up to ensure the quality of measurements: incident

beam monitor, better sample alignment system…

• Support: not only measurement, but also analysis.

• More flexible for payments.

• Better accommodation: room & dinning.

Characterization and Materials Processing © 2014 Corning Incorporated 13

Attract New Users:

• No direct incentive for industrial user to initiate the program under

the current R&D environment.

• Outreach to the potential users – conference, word of mouth, a

referral system…

• Free beamtime offer for the first time user: 1st visit must be

productive for the returning visits.

• Simplified legal process: accept industrial template or

standardized all national labs.