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Title: Investigation of forced and isothermal chemical vapor infiltrated SiC/SiC ceramic matrix composites. Final report

Abstract

Mechanical properties of two different layups for each of the forced CVI (41 specimens) and isothermal CVI (36 specimens) materials were investigated in air at room temperature (RT), 1000C, and at room temperature after thermal shock (RT/TS) and exposure to oxidation (RT/OX). The FCVI specimens had a nominal interfacial coating thickness of 0.3 {mu}m of pyrolytic carbon, while CVI specimens had a coating thickness of 0.1 {mu}m. Effect of reinforcement and interfacial bond on mechanical properties of composite were investigated. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed to analyze the fiber-matrix interface and the toughening mechanisms in this ceramic composite system.

Authors:
; ;  [1]
  1. North Carolina Agricultural and Technical State Univ., Greensboro, NC (United States). Dept. of Mechanical Engineering
Publication Date:
Research Org.:
North Carolina Agricultural and Technical State Univ., Greensboro, NC (United States). Dept. of Mechanical Engineering; Oak Ridge National Lab., TN (United States)
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
10110665
Report Number(s):
ORNL/SUB-88-SC423/01
ON: DE94004544
DOE Contract Number:
AC05-84OR21400
Resource Type:
Technical Report
Resource Relation:
Other Information: PBD: Sep 1993
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; COMPOSITE MATERIALS; MECHANICAL PROPERTIES; PROGRESS REPORT; REINFORCED MATERIALS; SILICON CARBIDES; FIBERS; 360603

Citation Formats

Sankar, J., Kelkar, A.D., and Vaidyanathan, R. Investigation of forced and isothermal chemical vapor infiltrated SiC/SiC ceramic matrix composites. Final report. United States: N. p., 1993. Web. doi:10.2172/10110665.
Sankar, J., Kelkar, A.D., & Vaidyanathan, R. Investigation of forced and isothermal chemical vapor infiltrated SiC/SiC ceramic matrix composites. Final report. United States. doi:10.2172/10110665.
Sankar, J., Kelkar, A.D., and Vaidyanathan, R. Wed . "Investigation of forced and isothermal chemical vapor infiltrated SiC/SiC ceramic matrix composites. Final report". United States. doi:10.2172/10110665. https://www.osti.gov/servlets/purl/10110665.
@article{osti_10110665,
title = {Investigation of forced and isothermal chemical vapor infiltrated SiC/SiC ceramic matrix composites. Final report},
author = {Sankar, J. and Kelkar, A.D. and Vaidyanathan, R.},
abstractNote = {Mechanical properties of two different layups for each of the forced CVI (41 specimens) and isothermal CVI (36 specimens) materials were investigated in air at room temperature (RT), 1000C, and at room temperature after thermal shock (RT/TS) and exposure to oxidation (RT/OX). The FCVI specimens had a nominal interfacial coating thickness of 0.3 {mu}m of pyrolytic carbon, while CVI specimens had a coating thickness of 0.1 {mu}m. Effect of reinforcement and interfacial bond on mechanical properties of composite were investigated. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed to analyze the fiber-matrix interface and the toughening mechanisms in this ceramic composite system.},
doi = {10.2172/10110665},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Wed Sep 01 00:00:00 EDT 1993},
month = {Wed Sep 01 00:00:00 EDT 1993}
}

Technical Report:

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  • The objective of this program was to investigate the fiber/matrix interfacial chemistry in CVI SiC matrix composites utilizing Nicalon SiC and Nextel 440 mullite fibers and to determine how this interface influences composite properties such as strength, toughness, and environmental stability. The SiC matrix was deposited using three different reactants; methyldichlorosilane (MDS), methyltrichlorosilane (MTS), and dimethyldichlorosilane (DMDS). The fiber/matrix interface was tailored by means of introducing a carbon, BN, or carbon rich SiC interfacial layer. It was found that applying a carbon interfacial layer to either NICALON or Nextel 440 fibers prior to deposition of SiC resulted in a weaklymore » bonded interface that imparted toughness to CVI matrix composite through its ability to deflect matrix cracks. This carbon layer can be applied either deliberately by the decomposition of methane or by utilizing an argon flushing gas in the reactor that apparently interrupted the normal deposition of SiC from silane precursors and instead allowed carbon to deposit. It was found that this carbon interfacial layer, no matter how it was deposited, was not oxidatively stable at elevated temperatures, leading to severe degradation of composite properties.« less
  • The objective of this program is to investigate the fiber/matrix interfacial chemistry in Chemical Vapor Infiltrated Silicon Carbide matrix composites utilizing Nicalon SiC and Nextel 440 mullite fibers and how this interface influences composite properties such as strength, toughness, and environmental stability. The SiC matrix was deposited using three different reactants; methyldichlorosilane (MDS), methyltrichlorosilane (MTS), and dimethyldichlorosilane (DMDS). It was found that by varying the reactant gas flow rates, the ratio of carrier gas to reactant gas, the type of carrier gas (hydrogen or argon), the flushing gas used in the reactor prior to deposition (hydrogen or argon), or themore » type of silane reactant gas used, the composition of the deposited SiC could be varied from very silicon rich (75 at %) to carbon rich (60%) to almost pure carbon. Stoichiometric SiC was found to bond very strongly to both Nicalon and Nextel fibers, resulting in a weak and brittle composite. A thin carbon interfacial layer deposited either deliberately by the decomposition of methane or inadvertently by the introduction of argon into the reactor prior to silane flow, resulted in a weakly bonded fiber/matrix interface and strong and tough composites. However, composites with this type of interface were not oxidatively stable. Preliminary results point to the use of a carbon-rich SiC interfacial zone to achieve a relatively weak, crack-deflecting fiber/matrix bond but also exhibiting oxidative stability.« less
  • Conventional Chemical Vapor Deposition (CVD) and Organometallic Chemical Vapor Deposition (MOCVD) were employed to deposit a series of interfacial coatings on SiC and carbon yarn. Molybdenum, tungsten and chromium hexacarbonyls were utilized as precursors in a low temperature (350[degrees]C) MOCVD process to coat SiC yarn with Mo, W and Cr oxycarbides. Annealing studies performed on the MoOC and WOC coated SiC yarns in N[sub 2] to 1,000[degrees]C establish that further decomposition of the oxycarbides occurred, culminating in the formation of the metals. These metals were then found to react with Si to form Mo and W disilicide coatings. In themore » Cr system, heating in N[sub 2] above 800[degrees]C resulted in the formation of a mixture of carbides and oxides. Convention CVD was also employed to coat SiC and carbon yarn with C, Bn and a new interface designated BC (a carbon-boron alloy). The coated tows were then infiltrated with SiC, TiO[sub 2], SiO[sub 2] and B[sub 4]C by a chemical vapor infiltration process. The B-C coatings were found to provide advantageous interfacial properties over carbon and BN coatings in several different composite systems. The effectiveness of these different coatings to act as a chemically inert barrier layer and their relationship to the degree of interfacial debonding on the mechanical properties of the composites were examined. The effects of thermal stability and strength of the coated fibers and composites were also determined for several difference atmospheres. In addition, a new method for determining the tensile strength of the as-received and coated yarns was also developed. The coated fibers and composites were further characterized by AES, SEM, XPS, IR and X-ray diffraction analysis.« less
  • Development of a new, faster process for the fabrication of ceramic-fiber-reinforced-ceramic-matrix composites by chemical vapor infiltration has continued. Composites of SiC fibers infiltrated with a matrix of either SiC or Si/sub 3/N/sub 4/ have been produced. Process and equipment improvements led to the fabrication of preforms with a higher fiber content, and infiltration improvements reduced infiltration times and increased infiltrated densities. These improvements have produced composites with higher flexural strengths (up to 475 MPa) and high strain values (up to 1%). The high strength and high strain values along with the gradual loss of strength (in contrast to the suddenmore » loss typical of ceramics) were major goals of this work.« less
  • This report covers work performed under the Advanced Materials for Advanced Industrial Gas Turbines (AMAIGT) program by GE Global Research and its collaborators from 2000 through 2010. A first stage shroud for a 7FA-class gas turbine engine utilizing HiPerComp{reg_sign}* ceramic matrix composite (CMC) material was developed. The design, fabrication, rig testing and engine testing of this shroud system are described. Through two field engine tests, the latter of which is still in progress at a Jacksonville Electric Authority generating station, the robustness of the CMC material and the shroud system in general were demonstrated, with shrouds having accumulated nearly 7,000more » hours of field engine testing at the conclusion of the program. During the latter test the engine performance benefits from utilizing CMC shrouds were verified. Similar development of a CMC combustor liner design for a 7FA-class engine is also described. The feasibility of using the HiPerComp{reg_sign} CMC material for combustor liner applications was demonstrated in a Solar Turbines Ceramic Stationary Gas Turbine (CSGT) engine test where the liner performed without incident for 12,822 hours. The deposition processes for applying environmental barrier coatings to the CMC components were also developed, and the performance of the coatings in the rig and engine tests is described.« less