FINAL TECHNICAL REPORT

September 1, 1997, through August 31, 1998

Project Title: EXTRUDED FIBER-REINFORCED CEMENT COMPOSITES CONTAINING FLY ASH

ICCI Project Number: 97-1/3.1D-9

Principal Investigator: Dr. Surendra P. Shah, Notrhwestern University

Other Investigators Dr. Alva Peled, Herman Yost, Notrhwestern University

Project Manager: Dr. Daniel D. Banerjee, ICCI

ABSTRACT

The proposed research is a two years program consisting of two phases: product development and commercialization feasibility. The major goals are to: 1) develop extrudable compositions of fiber-reinforced cement composites that contain substantial quantities of Illinois fly ash, 2) identify the best compositions for targeted products, and 3) to promote the most promising products for commercialization. The first year involved development and testing of different compositions: 1) finding the maximum allowable contents of Illinois fly ash, 2) evaluating different fiber types such as PVA, cellulose, glass and acrylic fibers, and 3) developing curing schedules to achieve the desired mechanical properties. The fly ash was examined as replacement for cement and silica sand.

The addition of the Illinois Class F fly ash significantly improves the rheology of the fresh extruded mixtures. This helps the extrusion process and reduced composite defects. Fly ash used as replacement for cement improves the flexural performance of the composite for all fiber types. This improvement is different for each type of fiber. The highest improvement in both flexural strength and ductility is obtained for composites containing acrylic fibers when as high as 70% by volume of cement replaced by fly ash. For PVA fibers, only a slight improvement in the flexural behavior is observed. In this case the highest flexural strength is obtained when 60% by volume of cement is replaced by fly ash. It is important to note that even when 80vol% of the cement was replaced by the Illinois fly ash the flexural strength is not significantly effected. Fly ash also improves the rheology of the mixture when compared with sand. Therefore it can be used as a good substitute for sand. Comparable improvements in flexural response are obtained in the composites cured for 2 days in a steam environment at 90C when compared with the conventional 28 days moist curing. This result is of great practical significance since shorter curing time is often desirable in a manufacturing plant.

It can be summarized that the Illinois Class F fly ash is particularly suitable for extruded fiber-reinforced cement composites, since mixtures containing substantial quantities of this fly ash are extrudable and provide high flexural properties (flexural strength of about 5000 psi and strain hardening type of response are observed).

EXECUTIVE SUMMARY

The project is being submitted in the category of Process Research. The applicable 1997-1998 Research Program Funding Area is Coal Related Residues/By-Product Management and is within the specific area of Pulverized Coal Combustion Residues (PCCR). The particular PCCR was Class F fly ash from the Illinois Basin Coal Combustion Residues Sample Program (CRSP).

The proposed research is a two years program consisting of two phases: product development and commercializing feasibility. The major goals are to: 1) develop extrudable compositions of fiber-reinforced cement composites that contain substantial quantities of Illinois fly ash, 2) identify the best compositions for targeted products, and 3) to promote the most promising products for commercialization. The first year involved development and testing of different compositions: 1) finding the maximum allowable contents of Illinois fly ash, 2) evaluating different fiber types such as PVA, cellulose, glass and acrylic fibers, 3) optimizing the content of the fibers, and 4) developing curing schedules to obtain the desired mechanical properties.

Fibers are incorporated in the brittle cement matrix to control the cracking, to provide high ductility and impact resistance, and to increase the tensile and flexural strengths. Extrusion is a processing technique that has been shown to impart high performance characteristics to fiber reinforced cementitious materials((1)).

Extrusion is a forming process, which forces a highly viscous plastic-like mixture through a rigid opening (a die) of the desired cross-section. It has been a widely used process in several industries such as, ceramic, clay, and polymer industries. There is a growing interest in the use of the extrusion process for the fiber reinforced cement composites industry. With properly designed dies and properly controlled material proportions, the fibers can be aligned in the load-bearing direction. The matrix and fiber packing can be identified to achieve low porosity and to improve the interface bond between the fiber and matrix. Extrusion also allows more flexibility in the product shape than possible with the standard board manufacturing processes. It is a potential candidate for low cost commercial applications, such as roofing tiles, flooring tiles, building panels, and pressure pipes. During the extrusion processing the viscosity (rheology) of the material is a controlling factor. If the rheology of the material is not close to ideal, defects form in the material during extrusion leading to reduce performance of the composites.

Besides the economical and ecological reasons for using fly ash in cement-based products, the round particle morphology of fly ash can improve the rheology of extrusion systems. Therefore fly ash can be considered as a replacement for sand, silica fume as well as for cement. Partial replacement of cement with fly ash not only makes cement-based products inexpensive, but also reduces the total life cycle energy consumption by lowering the amount of cement needed.

A small-scale extrusion rheometer was used to extrude the specimens for this work. Specimens containing different ratio of fly ash as replacement for cement, silica sand and silica fume were prepared. Different fiber types were added to the mixtures: PVA, glass, acrylic and cellulose fibers. Four combinations with different ratios of cement:fly ash were tested: 20:80, 30:70, 40:60, and 50:50. All the sand in the mixtures was replaced with fly ash (resulting in a 12% replacement by volume). The fiber volume fraction was 3% for PVA and glass fibers, and 7% - 8% for cellulose and acrylic fibers.

The influence of fiber content on flexural properties was also tested for PVA fibers. Different volumes of fibers were used: 1%, 2%, 3%, and 4%. The cement:fly ash ratio was kept constant at 40:60. In most of the cases two different cross sections of specimens were extruded and tested: 4mm sheet and 12.7mm diameter cylinders.

After the extrusion the specimens were covered with a plastic sheet. After 24 hours the specimens were placed in 100% RH at 90C for 2 days. Some specimens were subjected to conventional curing at 100% RH at room temperature for 28 days. Thereafter all the specimens were dried at 105 C for 2 days and kept for another 24 hours at 50% RH at room temperature, before final testing.

Three-point flexural tests were performed at a rate of 0.0114 mm/sec. The span was 101.6mm for the sheet specimens and 203.2mm for the cylinder specimens.

It was clear during the extrusion process that the addition of fly ash significantly improved the rheology of the fresh extruded mixtures. This lead to the reduction in composite defects and resulted in improved mechanical performance of the composite. This was observed for all fibers. The improvement in the flexural behavior on using fly ash varied with the fiber type. For example, for composites made with acrylic fibers, when 70% of cement was replaced with fly ash, a four-fold increase in ductility (as measured by deflection at peak load) was observed. For PVA fibers, only a slight improvement of the flexural strength was observed with fly ash replacement. In this case the highest flexural strength was obtained when 60% by volume of cement was replaced with fly ash. In the cases of cellulose, glass and PVA fibers cement replacement with fly ash resulted in a two-fold increase in ductility. It is important to note that even when 80% by volume of the cement was replaced with the Illinois fly ash the flexural behavior of the composites was not influenced significantly (only a 20% reduction was observed when compared with the 60-70% replacement).

Microstructural examination of fractured surfaces using Scanning Electron Microscope (SEM) indicated a different mechanism of fracture for composites containing fly ash compared with those without fly ash. Large composite defects (large pores) were observed in composites that did not contain fly ash. This can be attributed to the poor rheological properties of mixture used to extrude these composites, resulting in low flexural properties of composites without fly ash.

It was also found that the fly ash improved the rheology of the mixture over sand and achieved similar flexural behavior. Therefore fly ash can be used as a good substitute for sand.

The flexural strength obtained with fly ash was comparable to that with silica fume, but the corresponding toughness was lower. This was true even when half of the silica fume was replaced by fly ash. Therefore, silica fume can not be replaced when toughness is necessary.

Curing the specimens in a moist environment at 90C for 2 days gave similar flexural results compared to moist curing at room temperature for 28 days, for PVA and cellulose fibers. Shorter curing time can be an advantage from an economical point of view, when considering manufacturing of these composites.

One of the main advantages of extrusion technology is that it allows more flexibility in product shape than possible with the standard board manufacturing processes. Complicated solid cross-sections and open or cellular cross-sections can be extruded, usually with only minor modifications in batch composition. Where reduction in total weight or increase in structural rigidity is necessary, cellular cross sections can be extruded. In the second phase of this project specimen with different cross sections including two scales of cellular dies will be designed and extruded for use in lightweight construction for commercial applications.

Summary and Conclusions: It can be summarized that the Illinois Class F fly ash is particularly suitable for extruded fiber-reinforced cement composites, since mixtures containing substantial quantities of this fly ash are extrudable and provide high flexural properties (flexural strength of about 5000 psi and strain hardening type of response). The Illinois Class F fly ash significantly improves the rheology of the fresh extruded mixtures, which leads to a reduction in composite defects and results in improved mechanical performance. Fly ash can also be used to replace cement and sand, but can not replace silica fume when toughness is necessary (since silica fume greatly improved toughness over fly ash). Similar flexural response is obtained for composites cured for 2 days in a steam environment at 90C when compared with the conventional 28 days moist curing. This result is of great practical significance since shorter curing time is often desirable in a manufacturing plant.