Award Abstract # 1626164
MRI: Acquisition of an In-Situ/Operando Raman Spectrometer

NSF Org: DMR
Division Of Materials Research
Recipient: ALFRED UNIVERSITY
Initial Amendment Date: August 20, 2016
Latest Amendment Date: August 20, 2016
Award Number: 1626164
Award Instrument: Standard Grant
Program Manager: Leonard Spinu
lspinu@nsf.gov
 (703)292-2665
DMR
 Division Of Materials Research
MPS
 Directorate for Mathematical and Physical Sciences
Start Date: September 1, 2016
End Date: August 31, 2018 (Estimated)
Total Intended Award Amount: $370,000.00
Total Awarded Amount to Date: $370,000.00
Funds Obligated to Date: FY 2016 = $370,000.00
History of Investigator:
  • Scott Misture (Principal Investigator)
    misture@alfred.edu
  • Shan Sundaram (Co-Principal Investigator)
Recipient Sponsored Research Office: Alfred University
1 SAXON DR
ALFRED
NY  US  14802-1232
(607)871-2026
Sponsor Congressional District: 23
Primary Place of Performance: Alfred University
NY  US  14802-1205
Primary Place of Performance
Congressional District:
23
Unique Entity Identifier (UEI): J1B5PBG573T1
Parent UEI:
NSF Program(s): Major Research Instrumentation
Primary Program Source: 01001617DB NSF RESEARCH & RELATED ACTIVIT
Program Reference Code(s):
Program Element Code(s): 118900
Award Agency Code: 4900
Fund Agency Code: 4900
Assistance Listing Number(s): 47.049

ABSTRACT

Raman spectroscopy is a critical tool used to study bonding between atoms, which allows direct interrogation of both ordered and disordered systems. Such studies often provide new understanding of the atomic-scale origins of the function and properties of materials for next-generation applications. The proposed research, largely within a materials science department, will focus on ceramics and glasses used in energy storage and renewable energy, transportation, energy conversion, health care and defense. Unique to the proposed research is the ability to perform studies at the highest temperatures currently attainable - and with positional resolution using 3-D mapping. By direct examination of materials in-situ or under operating conditions, the research teams aim to uncover new atomic scale processes that can in turn be used to make transformational progress in materials discovery and design. In addition to the research applications, the instrument will be used in graduate and undergraduate laboratory courses, providing a range of baccalaureate and graduate students with training and experience in state-of-the-art materials characterization. With integration into the High Temperature Materials Testing Laboratory (HTMT) and the new Advanced Manufacturing Laboratory (AML) at Alfred University, the Raman spectrometer will be professionally marketed for use by industry and is expected to draw additional corporate users. Alfred University's strong history of industrially-funded research includes collaborations with 50 companies, and these links are expected to draw a continuous stream of corporate Raman users, with new users attracted to campus for Raman studies

Raman spectroscopy is a critical tool for uncovering the structural origins of materials properties and processing dynamics, especially when performed under conditions of controlled temperature or gaseous environment (in-situ) or under operating conditions (operando). In the atmosphere of a materials science department, high temperature Raman spectroscopy can be enabling in building comprehensive models of cation or anion disorder, defects in 2-D oxide nanosheets and related nanomaterials, glass devitrification, materials degradation mechanisms, residual stress, and similar problems. The Raman microprobe will be equipped with 3-D mapping and temperature-controlled chambers to enable discovery of new mechanisms that may lead to transformational progress in the fields of energy, environment and health care.

PROJECT OUTCOMES REPORT

Disclaimer

This Project Outcomes Report for the General Public is displayed verbatim as submitted by the Principal Investigator (PI) for this award. Any opinions, findings, and conclusions or recommendations expressed in this Report are those of the PI and do not necessarily reflect the views of the National Science Foundation; NSF has not approved or endorsed its content.

Raman spectroscopy is a critical tool used to measure vibrations of atoms and molecules and solids, which enables understanding materials properties and behaviors.  Bulk materials can be studied as well as the surfaces of solids and their interactions with their environments, to understand and subsequently optimize the properties and/or performance of materials in various devices. Indeed, this level of understanding often leads to invention of new materials for challenging applications, such as for making surface-strengthened glasses for cell phones and displays.  Important industrial processes such as chemical sensing, charge storage in batteries, and catalysis are easily studied using Raman spectroscopy as are problems like corrosion of surfaces and degradation of building materials.

The instrument provides new insight into materials processing and materials properties, to enable new breakthroughs in many areas of material science and engineering. With a focus on ceramic materials, we have used the instrument extensively since its installation in July 2018 to study electrochemical supercapacitors, batteries, and catalysts, at both high and low temperatures.

The spectrometer purchased during this project was optimized to enable measurements at high and low temperatures and high and low pressures, as well as under operational conditions such as when a component is attached to an electrical circuit (like a battery) or is placed under magnetic field. Our focus on the study of ceramics means that we need to make measurements at very high temperatures, approaching 1600?C, which is very uncommon but feasible. Although Raman spectroscopy traditionally uses visible light lasers to probe the sample, studies at temperatures above about 1000?C require a special approach using ultraviolet light, and hence the instrument was optimized by including red light, blue light, and ultraviolet light lasers and two separate spectrometers. The instrument complements existing instruments in our high temperature characterization facility, where x-ray diffraction and electrical, thermal, and optical properties measurements can be made up to similar temperature ranges.

The instrument has broadly impacted activities on campus, with the first cohort of undergraduate students using the instrument in a required undergraduate laboratory course. At this point, all 52 of those students were introduced to the instrument and its capabilities, and five graduate students and two laboratory technicians have been trained as expert users.

Our approach using this new state-of-the-art instrument under in-situ or operando conditions has attracted the attention of not only academic researchers at Alfred University, but has led to collaborations with faculty at the University of Wisconsin at Madison and Case Western University, and several industrial partners. Our on-campus Center for Advanced Ceramic Technology, funded by the state of New York, has integrated the instrument into our analytical services program in order to assist companies with scientific research and analytical measurements needs. The University has also assigned one laboratory technician with primary responsibility for maintenance and operation of the instrument, and training of students and other users. We use this approach in our other analytical laboratories with good success, and expect that the extremely broad capability of the new spectrometer will lead to new and expanded interactions with companies and other universities.


Last Modified: 11/30/2018
Modified by: Scott Misture

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