NCER Assistance Agreement Final Center Report Summary

Date of Final Report: September 30, 2007

EPA Agreement Number: R-83042001

Center: Center for Environmental and Energy Research (CEER)

Project Title: Final Center Report

Investigator(s): Terese Vascott

Institution(s) of PI(s): Alfred University

Research Category: Congressionally Mandated Center

Project Period: 07/01/2002 – 06/30/2007

 

 

I. Center Accomplishments and Activities

 

1. Center Overview

 

The Center for Environmental and Energy Research (CEER) at Alfred University is a multidisciplinary research and education program which makes use of Alfred’s expertise in ceramic engineering, materials science/engineering, and related programs to develop new materials, processes, and products that promote environmental sustainability. Center funds are primarily directed towards supporting graduate research. The Center is managed by Alfred University and is supervised by an external science advisory committee (SAC). A strategic planning board (SPB), drawn from the University’s science and engineering faculty, provides direction on policy and long-term strategy.

 

Alfred University is a residential, coeducational institution of approximately 2,300 students located in Alfred, New York. The University is comprised of Colleges of Business, Liberal Arts and Sciences, Engineering and the publicly supported New York State College of Ceramics. Alfred University’s educational and research expertise is well known, with a worldwide reputation in ceramic engineering and materials science. Alfred’s graduate ceramic engineering program is ranked #1 in the U.S. by the Gourman report.

 

The goals of the Center are to become a world leader in developing materials and processes for achieving environmental sustainability, and the world leader in developing ceramic materials for environmental benefits. To better advance the goals and objectives of the Center, new vision and mission statements were drafted in January 2005. These statements formalize the focus and scope of the Center’s research efforts.

 

• Vision Statement: The Center for Environmental and Energy Research (CEER) at Alfred University will be a world leader in developing materials and processes for achieving environmental sustainability. The Center will become the world leader in the development of ceramic materials for environmental applications.

 

• Mission Statement: The Center for Environmental and Energy Research (CEER) at Alfred University utilizes Alfred’s world renowned expertise and facilities in ceramic engineering, materials science/engineering, and related programs to develop materials and processes for environmental sustainability. The Center focuses on research areas of 1) materials and processes for clean, renewable energy, and 2) improvements in materials efficiency, environmental impact and recycling. The Center strives to establish outside funding sources in order to secure long-term sustainability.

 

CEER research projects will help to facilitate ‘green’ energy production and the reduction of hazardous waste material. Here are several examples of successes:

 

·      Photo-enhanced hydrogen diffusion through glass microspheres: Development of microsphere production for hydrogen storage. PIs: J. Shelby, M. Hall

 

This project built on previous research supported by CEER showing photo-enhanced hydrogen diffusion through glasses doped with optical activators.  (US DOE subsequently approved $2.2 million in funding for a continuation of the research.) The study provides the “reduction to practice” needed to patent a hydrogen storage device and to convince potential funding agencies and automobile manufacturers of the viability of this technique. Ultimately, the work should lead to a revolutionary new method for storing, transporting, and delivering hydrogen on demand.  The replacement of gasoline with hydrogen for operating automobiles has the potential to transform the transportation industry into a “clean fleet” by significantly reducing smog as every car that is running on hydrogen produces zero noxious emissions.

 

This work is continuing with current CEER funding, from EPA Grant No. X-83254101-1: “Recovery and purification of hydrogen from mixed gas streams”, J. Shelby, PI.

 

·      Microarray system for contaminated water analysis. PIs: J. Cardinale, R. DeRosa

 

The objective of this study was to develop a miniaturized ELISA (enzyme linked immunosorbent assay) on a glass surface. Results of the investigation established the use of a physicochemical method to develop a reusable glass substrate for an ELISA. ELISA, while a good method of detection, is one-time use and therefore generates tremendous amounts of non-recyclable waste, typically around 450 grams per plate (8.5 x 12 x 1.5 cm). ELISA plates (polystyrene, polyvinyl chloride, polypropylene) and polypropylene tips (96 per plate) are typically decontaminated by autoclaving followed by incineration or disposal in landfills. This project employed slides made from glass (7.5 x 2.5 x 0.1 cm) which can be decontaminated by autoclaving and then reused. The glass plates are smaller and weigh less (4.5 g vs. ~60 g), resulting in less energy use in decontamination, and do not generate plastic waste as the entire glass slide may be treated as a single unit during exposure and treatment.

 

This work was continued with CEER funding from EPA Grant No. X-83254101-1: “Microarray system for contaminated water analysis”, J. Cardinale, R. DeRosa, PIs (work completed September 2007).

 

• Robust, Spectrally Selective Ceramic Coatings for Recycled Solar Power Tubes. PIs: D. Edwards, W. Carty

 

The results of this study have the potential to reduce the cost of solar-derived electricity and remove failed solar collector tubes from the waste stream. Robust, spectrally selective ceramic coatings were developed for refurbishing (recycling) failed solar collector tubes. The effects of composition and processing variables on the optical performance of the oxide coatings was investigated, and large-scale deposition methods were evaluated so that the developed coatings could be applied to actual tubes that will ultimately be field tested. This technology has the potential to greatly expand the ability to harvest solar energy, and it could substantially reduce the long-term operating costs of the facilities currently in use, making solar-derived electricity a more attractive alternative to other, more polluting electricity-generating technologies.

 

• Interaction of sealing glasses with metallic interconnects in solid oxide and polymer fuel cells. PI: S. Misture

 

In-situ high temperature X-ray diffraction was successfully employed as the primary tool to study the interactions of three compositions of sealing glasses for solid oxide fuel cell (SOFC) seals with six candidate interconnect alloys. The study was focused on fundamental phase equilibria, reaction mechanisms, and reaction kinetics under oxidizing and reducing atmospheres, to provide the basic science to aid in fuel cell design and future materials compositional design work.

 

·      Environmental Impact of Fuel Cell Power Generation Systems. PI: X. Wang

 

The purpose of this study was to compare three unique fuel processor designs under the paradigm of industrial ecology. Three designs were compared utilizing two different methods, and an evaluation was made regarding each design in three specific impact areas: Environmental impact, economic impact, and methane retail resale cost. This comparison technique allowed determination of which design would minimize negative impact on the environment during its production; which design would be the most economical to produce; and which design would be the greatest producer of methane for retail resale were this to be a commercial product.

 

2. Contact Information

 

·      List of key contacts at Alfred University

Name	Function	Email	Telephone
Terese Vascott	Center Director	vascott@alfred.edu	607-871-2983
Alastair Cormack	Dean, School of Engineering	cormack@alfred.edu	607-871-2980
Garth Gregor	Director, Office of Sponsored Research	gregorg@alfred.edu	607-871-2128
Ken Lotter	Quality Assurance Manager	lotterk@verizon.net
Tammara Raub	Controller/AU Business Office		607-871-2128

 

 

·      Science Advisory Committee

 

Chad Nelson, Ph.D., SAC Chair                  
National Environmental Technology Institute (NETI), University of Massachusetts

chnelson@alumni.caltech.edu

Louis Pilato, Ph.D., SAC Vice Chair                       

Pilato Consulting                                                        

Pilato-consulting@worldnet.att.net                            

                                                                                   

Eldred Chimowitz, Ph. D., Dept. of Chemical Engineering, University of Rochester

chim@che.rochester.edu

 

Joseph H. Koo, Sc.D. , KAI, Inc., University of Texas, Austin                                      

jkoo@austin.rr.com                                                    

 

William Reinhardt, Sr. Project Manager,

NY State Energy Research & Development Authority (NYSERDA), R&D Dept.

wwr@nyserda.org

 

Gunnar Walmet, Director, Industry and Buildings

NY State Energy Research & Development Authority (NYSERDA)

gew@nyserda.org

·      Strategic Planning Board

 

Michele Hluchy

Professor and Chair, Environmental Studies

fhluchy@alfred.edu

 

James E. Shelby

John F. McMahon Professor of Glass Science, Ceramic Engineering, Materials Science

shelbyje@alfred.edu

 

Harrie J. Stevens

Director, Center for Glass Research

stevenshj@alfred.edu

 

Alastair Cormack (ex-officio)

Dean, Kazuo Inamori School of Engineering, Van Derck Frechette Professor of Ceramic Science

cormack@alfred.edu

 

3. Research

 

Grant no. R-83042001-4

Principal Investigator	Project Title	Start/End Date	Budget Amount ($US)
Carty	Preparation of ceramic glaze waste for recycling using froth flotation.	2006/2007	80,883
Carty	Elimination of lead from ceramic glazes by refractive index tailoring.	2006/2007	80,883

 

 

Grant no. R-83042001-2

Principal Investigator	Project Title	Start/End Date	Budget Amount ($US)
Shelby and Hall	Photo-enhanced hydrogen diffusion through glass microspheres.	2004/2005	79,495
Jones, Shelby, and Cormack	Nanostructured C6B: a novel boron rich carbon for H2 storage.	2004/2005	79,943
Misture	Interaction of sealing glasses with metallic interconnects in solid oxide and polymer fuel cells.	2004/2005	80,000

 

 

Grant no. R-83042001-1

Principal Investigator	Project Title	Start/End Date	Budget Amount ($US)
Carty and Sinton	The development of passive humidity-control materials.	2003/2004	52,000
Earl and Sinton	Utilization of paper mill waste in ceramic products.	2003/2005	152,644
Earl and Carty	Material and environmental sustainability in ceramic processing.	2003/2005	148,542
Cardinale and DeRosa	Microarray system for contaminated water analysis.	2003/2005	147,940

 

 

Grant no. R-83042001-0

Principal Investigator	Project Title	Start/End Date	Budget Amount ($US)
Shelby	Accelerated hydrogen diffusion through glass microspheres.	2003/2004	106,536

 

 

Undergraduate Summer Research Projects

 

In March 2005, CEER solicited proposals for undergraduate summer projects with focus on the areas of 1) materials and processes for clean, renewable energy, and 2) improvements in materials efficiency, environmental impact, and recycling. The following eight projects were funded from June through August 2005:

• Characterization and removal of AlN laser slag. (K. Goetschius/A. Meier)
• Development of glass phosphors for white light emitting diodes. (S. Morris/A. Clare)
• Evaluation of microbial community structures and coliform persistence in the Alfred waste water treatment plant reed bed sludge treatment system. (D. Roe/J. Cardinale)
• Low temperature Gd doped CeO₂ nano-layer electrolytes for solid oxide fuel cells.

(P. Willson/V. Amarakoon)

• Recycling of amber glass. (J. Peek/J. Shelby)
• Reduction of hazardous waste at AVX Olean, New York. (H. Schulze/S. Pilgrim)
• Solar absorbing ceramics increasing the efficiency of environmentally friendly energy production. (M. Naylor/D. Edwards)
• Synthesis and characterization of doped iron oxide electrodes for photo assisted electrolysis of water. (S. Sanford/V. Amarakoon)

CEER awarded summer research funding to eight Alfred University students for summer 2004.

• Initiating use of the environmental scanning electron microscope for CEER. (C. Clark/C. Boehlert)
• Construction of a hybrid-renewable energy-efficient home water heating unit. (W. Fabrizio/J. Baghdadchi)
• Electrostatic air filters modifications. (M. Klingensmith/X. Wang)
• Removal of laser slag on AlN via chemical cleaning. (D. Mandich/A. Meier)
• Boron volatilization from borosilicate melts. (M. Snyder/J. Shelby)
• A new disc design containing a charge storage layer for the application of electrical energy generation via wind power. (D. Streib/T. Seward)
• Mechanical properties of lightweight alloys. (I. Szabo/C. Boehlert)
• Development of a microarray system for analysis of contaminated water. (J. Villone/R. DeRosa)

 

Summer 2003

• Recycling of amber glass. (M. Ashton-Patton/J. Shelby)
• Production of hollow glass microspheres from amber glass frit. (K. Carlson/A. Clare)
• Surface preparation of aluminum nitride for metallization: effect of temperature on surface reactivity. (A. Crawford/A. Meier)
• Recycling of fiberglasses. (A. Hedlund/J. Shelby)
• Alternative energy solutions: coated submersible heating elements and wind energy. (A. Hydrick/J. Baghdadchi)
• Improving the reliability of active metal brazed Cu/AlN: interfacial reaction kinetics and microstructural development between Ag-Cu-Zr braze alloys and AlN. (J. Villone/A. Meier)

 

Summer 2002

• Fuel processor control. (J. Byrnes/X. Wang)
• Evaluating possible wind turbine sites in Allegany County using GIS and satellite imagery. (C. DeMay/D. Sinton)
• Microstructural analysis of recycled thermoset composites. (G. Gaustad/R. DeRosa)
• Replacement of BeO by AlN and development of an AlN surface preparation method utilizing “green” solvents. (D. Mandich/A. Meier)
• Investigation of the operating characteristics of a manure-fueled engine. (N. Wodka/C. Pian)

 

Many of these projects were continued as senior or graduate thesis research.

 

4. Quality Assurance

 

All Requests for Proposals (RFP) issued from CEER require that research proposals are submitted with a Quality Assurance Project Plan (QAPP) which is part of the evaluation/acceptance criteria. CEER’s Quality Assurance Manager reviews/approves the QAPPs prior to the consideration of proposals by CEER’s Science Advisory Committee (SAC). Proposals are not eligible for consideration unless they include a completed and approved QAPP.

Audits/surveillances of project facilities and procedures are conducted at the beginning and end of the research project (and at one year from the start date if the project period is greater than one year) to ensure compliance with the QAPP. CEER’s Quality Assurance Manager conducts an annual Quality System Management Review, usually in late summer, to insure that the Quality System remains effective. The Dean of the School of Engineering, the Center Director, and representatives of the Principal Investigators participate in the meeting.

 

The Quality Management Plan (March 2006) is included as Appendix I in the Final Center Report.

 

 

II. Summary Discussion of Research

 

Technical Effectiveness / Economic Feasibility / Environmental Benefits

 

Hollow glass microspheres (HGMS), developed by Dr. James Shelby, are viable candidate materials for storage of hydrogen and fuel cell applications. Results of the study indicated that hydrogen can be stored and released, with repeatable cycles of saturation-outgassing, in HGMS doped with appropriate absorbing species. Further investigation was focused on the preparation of microspheres from sol-gel derived glass for application in photo-induced diffusion of gases. This work is continuing, through funding from EPA grant no. X-83254101-1 administered by CEER, to demonstrate that HGMS can be used in the recovery and separation of hydrogen from mixed gas streams produced by both renewable and non-renewable sources.

 

In a study of sealing glasses for use in solid oxide fuel cells (SOFC), by Dr. Scott Misture, in-situ high-temperature X-ray diffraction (HT XRD) was employed to characterize the interactions of three sealing glass compositions with six candidate interconnect alloys. The research demonstrated successful use of HT XRD to reveal fundamental phase equilibria, reaction mechanisms, and reaction kinetics, thereby providing basic science to assist in fuel cell and materials compositional design in future research and development work.

 

Several projects funded by this grant were focused on processing techniques for reusing waste materials, eliminating hazardous materials from the process, or developing reusable products for existing processes. Benefits lie in reducing raw materials requirements, manufacturing waste, and contaminants in the waste stream.

 

“Material and environmental sustainability in ceramic processing” (PIs: W. Carty, D. Earl), explored techniques to separate glaze components for reuse in whitewares manufacturing. Large amounts of waste water and raw materials are generated in industrial production of colored glazes. The initial investigation, employing hydrocyclone (separation by particle size) technology, while only moderately successful in retrieving usable material, led to continuing research exploiting surface chemistry effects for selective agglomeration and a ‘froth flotation’ separation technique. The research project, “Preparation of ceramic glaze waste for recycling using froth flotation” (PI: W. Carty), achieved 68-69% frit recovery from a frit-pigment-water system by manipulating the pH of the system and the surface charge of the particles. By using a cationic ‘collector’ in conjunction with a non-polar ‘depressant’, the frit was selectively floated to the surface entrained on bubbles, the pigment sank to the bottom of the vessel, and the water appeared particle-free. Repeated flotation, with chemistry adjustments, has the potential to sequentially segregate assorted glaze components after the frit has been removed from the glaze waste.

 

“Utilization of paper mill waste in ceramic products” (PIs: D. Earl, C. Sinton), identified compositional similarities between paper mill waste and ceramic tile raw materials. The performance of porcelain tile body formulations with variable amounts of paper mill ash waste substituted for traditional raw materials was evaluated in comparison with traditional compositions. The tile bodies developed and tested in this study were not successful, primarily due to compositional variations in the ash waste which contributed to inconsistent properties and poor sintering behavior.

 

The objective of “Elimination of lead from ceramic glazes by refractive index tailoring” (PI: W. Carty), was to develop a lead-free glaze with the visual appearance of a leaded glaze, thereby reducing the amount of hazardous material in the manufacturing process and in the waste stream. The glossy appearance of a lead-free glaze is generally accepted as inferior to a leaded glaze, even in the absence of measurable quantitative differences. The approach employed in this project was to locally tailor chemical compositions of the barium-containing glaze to develop a refractive-index gradient and surface smoothness that in combination produce the superior optical quality of a leaded glaze. An interfacial glaze layer with no barium was applied to facilitate body-to-glaze interaction, then over-glazed with a barium-containing top layer. The higher melting temperature of the top layer limited diffusion of BaO from the top layer to the interfacial layer, introducing a refractive index gradient from the surface through the glaze. Although the optical effect observed in leaded glazes was not achieved, the study successfully demonstrated that the effect is achievable without lead by tailoring the concentration gradients in the glaze.

 

Dr. Jean Cardinale and Dr. Rebecca DeRosa directed a study to create a reusable glass miniaturized multianalyte device (microarray) for detection of multiple water microbial contaminants. This device, a physicochemically-tailored flat glass substrate, could replace the traditional enzyme linked immunosorbent assay (ELISA) which employs a non-reusable polystyrene wellplate, generating large amounts of polymer and biologically-contaminated waste, and requires a large volume of expensive high-purity antibodies and consumable reagents. This study identified and characterized candidate glass substrates, developed physicochemical surface treatment protocol to prepare the microarray, and tested for direct binding of antigens. Direct binding assays indicated that the capture antibody was improperly immobilized on the glass surface such that antigen binding did not occur. Further study is underway to fully characterize the glass surface in order to correlate the dependence of antibody binding efficiency with a functionalized surface. This work is continuing, with current CEER funding from EPA Grant No. X-83254101-1: “Microarray system for contaminated water analysis”, J. Cardinale, R. DeRosa, PIs.

 

 

 

 

III. Final Report Executive Summaries

 

Project summaries for the investigations listed below are included in Section III of the Final Center Report. The Report Summaries are also posted on EPA’s NCER web site and can be accessed via the link,

http://cfpub.epa.gov/ncer_abstracts/index.cfm/fuseaction/outlinks.centers/center/145.

 

1. Accelerated hydrogen diffusion through glass microspheres. (J. Shelby, M. Hall)
2. Microarray system for contaminated water analysis. (J. Cardinale, R. DeRosa)
3. Material and environmental sustainability in ceramic processing. (W. Carty, D. Earl)
4. Utilization of paper mill waste in ceramic products. (D. Earl, C. Sinton)
5. Development of passive humidity-control materials. (W. Carty, C. Sinton)
6. Interaction of sealing glasses with metallic interconnects in solid oxide and polymer fuel cells. (S. Misture)
7. Nanostructured C₆B: A novel boron-rich carbon for H₂ storage. (L. Jones, A. Cormack, J. Shelby)
8. Preparation of glass microspheres from sol-gel derived glass for application in photo-induced diffusion of gases. (J. Shelby, M. Hall)
9. Elimination of lead from ceramic glazes by refractive index tailoring. (W. Carty)

10. Preparation of ceramic glaze waste for recycling using froth flotation. (W. Carty)

 

 

IV. Publications and Presentations

 

1. Assistance Agreement R-83042001

 

Graduate Theses:

D. B. Rapp, Photo-induced Hydrogen Outgassing of Glass. Ph. D. thesis, 2004.

Advisor: J. Shelby.

G. I. Schwerzler, Recycling of Glaze Waste Through Hydrocyclone Separation.

M. S. thesis, 2005. Advisors: B. Carty & D. Earl.

A. Cooper, Microarray System for Contaminated Water Analysis.

M. S. thesis, 2005. Advisors: R. DeRosa & J. Cardinale.

B. Sechrist, Surface Chemistry of Glaze Constituents in Preparation for Froth Flotation

Separation, M. S. thesis, 2007 (in progress). Advisor: W. Carty.

 

Publications:

D. B. Rapp & J. E. Shelby, “Photo-Enhanced Hydrogen Outgassing of Glass,”

J. Non-Cryst. Solids 349, 254-59 (2004).

R. L. DeRosa, E. Telfeyan, and J. S. Mayes, “Expanding the Use of Recycled SMC in BMC’s”,

Proceedings of GPEC 2004, Society of Plastics Engineers Environmental Division, February 18-19, Detroit, MI.

E. Telfeyan, R. L. DeRosa, and J. S. Mayes, “Current State of Recycling SMC and Similar

Materials”, accepted by Journal of Thermoplastic Composites, February 2004.

 

 

A. Cooper, J. Cardinale, R. DeRosa, “Functionalized Glass Surface for Bioapplications”,  for

publication in the Proceedings of the 107^th Annual Meeting & Exposition of The American Ceramic Society, accepted for publication 07/31/05. 

A. Cooper, J. Cardinale, R. DeRosa, “Functionalized Glass Substrate for Microarray Analysis”,

submitted to Thin Solid Films, 09/21/05.

G. I. Schwerzler, “Recycling of Glaze Waste through Hydroclone Separation”, accepted

09/07/05 for publication in Powder Technology.

 

Patents:

Xingwu Wang, Huihui Duan, and Bigang Min, “Fuel Processor”, U.S. Patent # 6,800,386, Oct.

5, 2004.

Xingwu Wang, Huihui Duan, and Bigang Min, “Fuel Processor”, U.S. Patent # 6,811,907, Nov.

2, 2004.

 

Presentations:

J. E. Shelby, 16^th University Conference. on Glass Science: Glasses for High Technology,

Rensselaer Polytechnic Institute, Troy, NY, Aug. 13-15, 2003.

 

 

Supplemental Key Words: environmental research, energy research, US EPA NCER, environmental sustainability, ceramic engineering, materials science, ceramic materials for environmental applications, Alfred University

 

Relevant Web Sites: http://ceer.alfred.edu