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c) o FINAL TECHNICAL REPORT September 1, 1994 through August 31, 1995 Project Title: DESIGN AND FABRICATION OF ADVANCED MATERIALS FROM ll..LINOIS COAL WASTES DOE Cooperative Agreement Number: DE-FC22-92PC92521 (Year 3) ICCI Project Number: 94-1/3. lA-3M Principal Investigator: Viv8.k M. Malhotra, Professor Southern illinois University at Carbondale Other Investigators: Maurice A. Wright, Director Materials Technology Center, Southern TIlinois University at Carbondale Project Manager: . Dr. Dan Banetjee, Illinois Clean Coal Institute ABSTRACT The main goal of this project is to develop a bench-scale technology which converts coal combustion residues from TIlinois sources into high-value, advanced composite materials. Pulverized coal combustion (PCC) fly ash (Baldwin), fluidized bed combustion (FBC) fly ash (ADM, Unitsl-6), FBC spent bed ash (ADM, Unitsl-6), and scrubber sludge (CWLP) were characterized for their structural, chemical, and thermal suitability for our composite materials by undertaking scanning electron microscopy (SEM), differential scanning calorimetry (DSC) at 30°C < T < 600°C, differential thermal analysis (DTA) at 50°C < T < 1100°C, and Fourier transform infrared (FTIR) measurements. Our spectroscopic and SEM results indicate that the scrubber sludge is mainly composed of a gypsum-like phase whose lattice structure is different from the lattice structure of conventional gypsum. The sludge does not contain hannebachite phase. The thermal signatures of the residues examined suggest that these coal by-products, when properly combined, can act as excellent raw materials. Besides characterization, we evaluated various variables in the formation of our composites, e.g., fibers, type of coal by-products, admixture and combination of coal residues, binders, and fabrication pressure and temperature. Our data suggest that FBC spent bed ash by themselves are not a suitable raw material for our brake pads. However, this is not the case for PCC fly ash particles or for scrubber sludge particles. SEM results on fabricated composites show a lack of cross-linking between carbon fibers and matrix, while this is not the case for slag fibers which showed excellent bonding .. The SEM and Young's modulus analyses of brake composites fabricated at 400 psi < Pressure < 2200 psi imply pressure has a strong influence on the particle packing and the filling of interstices in our materials. On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's (E ) modulus and yield force (F yf) values of our brake shoe pads suggest mechanical behavior better than a high-performance, commercial automotive brake composite.

c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's

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Page 1: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's

c)

o

FINAL TECHNICAL REPORT September 1, 1994 through August 31, 1995

Project Title: DESIGN AND FABRICATION OF ADVANCED MATERIALS FROM ll..LINOIS COAL WASTES

DOE Cooperative Agreement Number: DE-FC22-92PC92521 (Year 3) ICCI Project Number: 94-1/3. lA-3M Principal Investigator: Viv8.k M. Malhotra, Professor

Southern illinois University at Carbondale Other Investigators: Maurice A. Wright, Director

Materials Technology Center, Southern TIlinois University at Carbondale

Project Manager: . Dr. Dan Banetjee, Illinois Clean Coal Institute

ABSTRACT

The main goal of this project is to develop a bench-scale technology which converts coal combustion residues from TIlinois sources into high-value, advanced composite materials. Pulverized coal combustion (PCC) fly ash (Baldwin), fluidized bed combustion (FBC) fly ash (ADM, Unitsl-6), FBC spent bed ash (ADM, Unitsl-6), and scrubber sludge (CWLP) were characterized for their structural, chemical, and thermal suitability for our composite materials by undertaking scanning electron microscopy (SEM), differential scanning calorimetry (DSC) at 30°C < T < 600°C, differential thermal analysis (DTA) at 50°C < T < 1100°C, and Fourier transform infrared (FTIR) measurements. Our spectroscopic and SEM results indicate that the scrubber sludge is mainly composed of a gypsum-like phase whose lattice structure is different from the lattice structure of conventional gypsum. The sludge does not contain hannebachite (CaS03.0.5~O) phase. The thermal signatures of the residues examined suggest that these coal by-products, when properly combined, can act as excellent raw materials. Besides characterization, we evaluated various variables in the formation of our composites, e.g., fibers, type of coal by-products, admixture and combination of coal residues, binders, and fabrication pressure and temperature. Our data suggest that FBC spent bed ash by themselves are not a suitable raw material for our brake ~hoe pads. However, this is not the case for PCC fly ash particles or for scrubber sludge particles. SEM results on fabricated composites show a lack of cross-linking between carbon fibers and matrix, while this is not the case for slag fibers which showed excellent bonding .. The SEM and Young's modulus analyses of brake composites fabricated at 400 psi < Pressure < 2200 psi imply pressure has a strong influence on the particle packing and the filling of interstices in our materials. On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's (E ) modulus and yield force (F yf) values of our brake shoe pads suggest mechanical behavior better than a high-performance, commercial automotive brake composite.

Page 2: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 3: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 4: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 5: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 6: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 7: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 8: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 9: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 10: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 11: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 12: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 13: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 14: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 15: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 16: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 17: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 18: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 19: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 20: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 21: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 22: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 23: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 24: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 25: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 26: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 27: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 28: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 29: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 30: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 31: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 32: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 33: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's
Page 34: c) · On sintering the brake composite, the scrubber sludge derived composite's Young's modulus decreases, while the opposite trend is seen for the PCC derived composite. The Young's