High Performance Silicon Carbide Fiber Hi-Nicalon for Ceramic Matrix Composites

Takeda, Michio; Sakamoto, Junichi; Saeki, Akinori; Imai, Yoshikazu; Ichikawa, Hiroshi

doi:10.1002/9780470314715.ch3

Cited by 63 publications

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“…The NLM, Hi and Hi-S grades of Nicalon fibers withstand annealing up to 1200-1300°C [18] , 1500°C [72] and ≥1600°C [32] , respectively. The low stability of the NLM fiber is attributed to the internal oxidation of its "free" carbon by the oxygen of the oxycarbide phase [18,73] .…”

Section: Raman Spectroscopy and Sic Fibers Micro/nano-structurementioning

confidence: 99%

“…Only in the very last generation of SiC fibers can SiC spectrum be recorded (Hi-S, SA and Sylramic fibers all have a C/Si ratio below 1.1) and it mainly consists of peaks around 796 and 972 cm -1 . These peaks correspond respectively to the transversal optic (TO 1 and TO 2 ; degenerate) and the longitudinal optic (LO) modes of β-SiC (cubic structure, 3C-SiC in Ramsdell notation), which was identified by x-rays diffraction as the SiC phase present in Nicalon (NLM, Hi & Hi-S) [32] , SA [22] and Sylramic [33] fibers. Yet, satellite Raman lines like the prominent contribution around 765 cm -1 , are detected.…”

Section: Correlation Between Raman Spectra and Microstructurementioning

confidence: 99%

“…±700 [3] 2970 [33] 1.4 [22,72] 1.2 ±0.09 [3] Hi 1.39 [21] 1.41 [5] 1.55 [81] 1.35 [82] 0.5 [21,33,72] e-5 [5] 5.4 [32] 4.5 [21] 2-15 [5,7] 5-20 $ [4] 3-5 [82] 1-30…”

Section: Fig 6 (A)mentioning

confidence: 99%

“…±600 [3] 1 [72] 0.95 [4] 0.9 ±0.03 [3] Hi-S [32] 1.05 0.2 e-10.9 / / 3.1 420 ≥2500 0.6 SA * 1.08 [22] ≈ 0.3 Ox 38 [22] 200 [21] 100-300 [22] # 3.02 [21,22] 420 [22] 2800-3000 [22] 0.7 [22] Sylramic [33] < cited references give a size range based on electronic microscopy observations ; ♦ 0.2 wt% H [72] ; ∅ 2-3 layers of 10 "C 6 -rings" [7] ; $ mostly 5-7.5 nm ; & from Selected-Area Diffraction Pattern ; layers ; * ≤1wt% Al ; #At triple points [21] ; ♠ B = sintering aid ⇒ 3wt% TiB 2 (0.5 µm)+1wt% B 4 C(0.1 µm)…”

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Non-destructive mechanical characterization of SiC fibers by Raman spectroscopy

Gouadec

Colomban

2001

Journal of the European Ceramic Society

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The paper provides a comprehensive study on Raman spectroscopy versatility as a fast and non destructive tool for the prediction of the mechanical properties of SiC fibers derived from a polymeric precursor (NLM™, Hi™, Hi-S™, SA™ and Sylramic™ grades) or produced by CVD (SCS-6™ fiber), including in situ analysis in CMCs or MMCs. We show how the results of very simple spectra fitting are correlated with Young's modulus, tensile strength and microhardness. The reason why such a correlation exists, the common dependency of Raman signal and mechanical behavior to the micro/nanostructure of ceramics, is discussed. Keywords :SiC-fibers / Raman spectroscopy / Mechanical properties / Microstructure / Carbon ∂ Author to whom correspondence should be addressed Fax : 33 (0) 1 49 78 13 18 e-mail : colomban@glvt-cnrs.fr IntroductionThe reinforcement of ceramic materials by long ceramic fibers leads to low density and refractory materials, of high damage tolerance, that should be appropriate for metal alloys substitution in advanced engines (turbines) and waste treatment energy plants [1] . Ceramic fibers can also be incorporated directly in metal matrices to increase their high temperature mechanical properties [1] .SiC fibers, which are among the most stable fibers, have always been produced by the 3D reticulation of a polymeric precursor. This synthesis route leads to a high matter homogeneity and very smooth surfaces, the lack of defects explaining tensile strengths σ r as high as 3 GPa. SiC fibers have been widely studied, especially their aging [2][3][4][5][6][7] which evidenced that densification is linked to compositional changes (for instance the loss of some residual hydrogen [8] ). A peculiarity of ceramics issued from polymeric precursors is no impurities are concentrated at the grains boundaries. Abnormal grain growth is very common in the lack of such usual diffusion regulators [9] and the know-how of SiC fibers manufacturers consists in postponing the onset of SiC crystallization and grain growth, since a high correlation is anticipated with mechanical degradation. A close relationship has been evidenced, for instance, between the micro-hardness and short-range ordering in sol-gel prepared nanocrystalline oxides [10] and some authors have already pointed out fibers overall mechanical ability is governed by their microstructure [5,7,11] .The purpose of this paper is to try correlating, to the best extent possible, the tensile strength (σ r ), the Young's modulus (E) and the micro-hardness (μH) of different SiC fibers, either to Raman spectra or to "Raman Extensometry" S coefficient (measuring the straininduced shifts of Raman bands). Unlike most experimental methods intended to measure directly σ r and E, Raman analysis does not require extracting fibers from the matrix, either by mechanical grinding/crushing [12] or by chemical attack [13] . Only the most resistant fibers are extracted in the former case while fibers surface might be altered in the latter. Besides, it will always be difficult to extract...

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Section: Raman Spectroscopy and Sic Fibers Micro/nano-structurementioning

confidence: 99%

Section: Correlation Between Raman Spectra and Microstructurementioning

confidence: 99%

“…±700 [3] 2970 [33] 1.4 [22,72] 1.2 ±0.09 [3] Hi 1.39 [21] 1.41 [5] 1.55 [81] 1.35 [82] 0.5 [21,33,72] e-5 [5] 5.4 [32] 4.5 [21] 2-15 [5,7] 5-20 $ [4] 3-5 [82] 1-30…”

Section: Fig 6 (A)mentioning

confidence: 99%

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Non-destructive mechanical characterization of SiC fibers by Raman spectroscopy

Gouadec

Colomban

2001

Journal of the European Ceramic Society

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“…18,19 A duplex surface layer of boron nitride (BN) over coated with silicon carbide was applied on the fibers by a commercial vendor using a continuous chemical vapor deposition (CVD) reactor. The BN coating was deposited at ∼1000 • C utilizing a proprietary precursor and was amorphous to partly turbostratic in nature.…”

Section: Materials and Experimental Methodsmentioning

confidence: 99%

Mechanical properties of Hi-Nicalon fiber-reinforced celsian composites after high-temperature exposures in air

Bansal¹

2009

Journal of the European Ceramic Society

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Raman analysis of materials corrosion: the example of SiC fibers

Colomban

Gouadec

Mazérolles

2002

Materials and Corrosion

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Advanced materials (ceramics, fibers, composites...) exhibit unique high temperature properties but long term durability assessment is mandatory on account of high processing costs. We used Raman micro‐spectroscopy to analyze the corrosion resistance of commercially available SiC fibers versus Na+ ions, with or without fiber thermal treatment (in air or in a reducing atmosphere) prior to sodium attack. The lateral resolution of the technique approaches the submicron scale and the analysis of colored materials can be limited to a few tens of nanometers in‐depth, which makes Raman micro‐spectrometry well suited for the analysis of corrosion films. Although corrosion starts with localized defects in pristine NicalonTM fibers attacked with Na+ (in oxidizing conditions), a protective effect of a silica film is clear for oxidized fibers. The corrosion of SiC crystals seems to be related to stacking faults.

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High Performance Silicon Carbide Fiber Hi-Nicalon for Ceramic Matrix Composites

Cited by 63 publications

References 0 publications

Non-destructive mechanical characterization of SiC fibers by Raman spectroscopy

Non-destructive mechanical characterization of SiC fibers by Raman spectroscopy

Mechanical properties of Hi-Nicalon fiber-reinforced celsian composites after high-temperature exposures in air

Raman analysis of materials corrosion: the example of SiC fibers

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