Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties
Two types of wood-based biomorphous SiC composites with different microstructure are obtained by infiltration of carbon template with liquid or vapour silicon. The oak, pine, lilac, walnut, acacia woods available in Ukraine are used as the biological template in this work. The SEM, optical and EP...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
2009
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| Cite this: | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties / V.S. Kiselov, E.N. Kalabukhova, A.A. Sitnikov, P.M. Litvin, V.I. Poludin, V.A. Yukhymchyk, A.E. Belyaev // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2009. — Т. 7, № 1. — С. 237-243. — Бібліогр.: 16 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859762020553850880 |
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| author | Kiselov, V.S. Kalabukhova, E.N. Sitnikov, A.A. Litvin, P.M. Poludin, V.I. Yukhymchyk, V.A. Belyaev, A.E. |
| author_facet | Kiselov, V.S. Kalabukhova, E.N. Sitnikov, A.A. Litvin, P.M. Poludin, V.I. Yukhymchyk, V.A. Belyaev, A.E. |
| citation_txt | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties / V.S. Kiselov, E.N. Kalabukhova, A.A. Sitnikov, P.M. Litvin, V.I. Poludin, V.A. Yukhymchyk, A.E. Belyaev // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2009. — Т. 7, № 1. — С. 237-243. — Бібліогр.: 16 назв. — англ. |
| collection | DSpace DC |
| container_title | Наносистеми, наноматеріали, нанотехнології |
| description | Two types of wood-based biomorphous SiC composites with different microstructure
are obtained by infiltration of carbon template with liquid or vapour
silicon. The oak, pine, lilac, walnut, acacia woods available in Ukraine
are used as the biological template in this work. The SEM, optical and EPR
data indicate that biomorphous SiC obtained by melt infiltration consists of
crystalline 3C-SiC phase while that obtained by vapour infiltration consists
of both crystalline and amorphous 3C-SiC phase.
Були одержані два типи деревного біоморфного SiC-композиту з різною
мікроструктурою просочення вуглецевого шаблону газоподібним або рідким кремнієм. Деревина дуба, сосни, бузку, волоського горіха, акації,
які поширені в Україні, використовувалися як біологічний шаблон у цій
роботі. Дані оптичні, СЕМ і ЕПР показали, що одержані просоченням
розтопом біоморфні композити SiC складаються із кристалічної й аморфної фаз 3C-SiC.
Были получены два типа древесного биоморфного SiC-композита с различной микроструктурой пропитки углеродистого шаблона газообразным или жидким кремнием. Древесина дуба, сосны, сирени, грецкого
ореха, акации, распространенные в Украине, использовались как биологический шаблон в этой работе. Данные оптические, СЭМ и ЭПР показали, что полученные пропиткой расплавом биоморфные композиты SiC
состоят из кристаллической и аморфной фаз 3C-SiC.
|
| first_indexed | 2025-12-02T04:02:15Z |
| format | Article |
| fulltext |
237
PACS numbers: 62.23.Pq, 68.37.Hk, 68.37.Ps, 81.16.Fg, 83.80.Mc, 87.64.-t, 87.85.jf
Effect of Si Infiltration Method on the Biomorphous SiC
Microstructure Properties
V. S. Kiselov, E. N. Kalabukhova, A. A. Sitnikov*, P. M. Litvin,
V. I. Poludin, V. A. Yukhymchyk, and A. E. Belyaev
V. E. Lashkaryov Institute of Semiconductor Physics,
National Academy Science of Ukraine,
Prosp. Nauky, 45,
03028 Kyyiv, Ukraine
*National Technical University of Ukraine ‘Kyyiv Polytechnic Institute’,
Prosp. Peremogy, 37,
03056 Kyyiv, Ukraine
Two types of wood-based biomorphous SiC composites with different micro-
structure are obtained by infiltration of carbon template with liquid or va-
pour silicon. The oak, pine, lilac, walnut, acacia woods available in Ukraine
are used as the biological template in this work. The SEM, optical and EPR
data indicate that biomorphous SiC obtained by melt infiltration consists of
crystalline 3C-SiC phase while that obtained by vapour infiltration consists
of both crystalline and amorphous 3C-SiC phase.
Були одержані два типи деревного біоморфного SiC-композиту з різною
мікроструктурою просочення вуглецевого шаблону газоподібним або рід-
ким кремнієм. Деревина дуба, сосни, бузку, волоського горіха, акації,
які поширені в Україні, використовувалися як біологічний шаблон у цій
роботі. Дані оптичні, СЕМ і ЕПР показали, що одержані просоченням
розтопом біоморфні композити SiC складаються із кристалічної й аморф-
ної фаз 3C-SiC.
Были получены два типа древесного биоморфного SiC-композита с раз-
личной микроструктурой пропитки углеродистого шаблона газообраз-
ным или жидким кремнием. Древесина дуба, сосны, сирени, грецкого
ореха, акации, распространенные в Украине, использовались как биоло-
гический шаблон в этой работе. Данные оптические, СЭМ и ЭПР показа-
ли, что полученные пропиткой расплавом биоморфные композиты SiC
состоят из кристаллической и аморфной фаз 3C-SiC.
Key words: biomorphous SiC/Si composites, SEM, Raman spectroscopy, EPR.
Наносистеми, наноматеріали, нанотехнології
Nanosystems, Nanomaterials, Nanotechnologies
2009, т. 7, № 1, сс. 237—243
© 2009 ІМФ (Інститут металофізики
ім. Г. В. Курдюмова НАН України)
Надруковано в Україні.
Фотокопіювання дозволено
тільки відповідно до ліцензії
238 V. S. KISELOV, E. N. KALABUKHOVA, A. A. SITNIKOV et al.
(Received November 23, 2007)
1. INTRODUCTION
Biomorphous composites SiC/Si are known in the literature as ecoceram-
ics–environment conscious ceramics [1—3]. Among the biomorphous
composites, the porous SiC ceramics has been considered to be one of the
best candidate materials for orthopaedic and dental implants due to their
high level of biocompatibility, chemical inertness and mechanical
strength [4—6]. Porous SiC has also a great potential for many industrial
applications such as light ultra strong material in aerospace and motor-
car industry, and as well as a heat insulation material due to its low ther-
mal expansion coefficient, small value of the relative density, mechanical
strength, high chemical inertness, oxidation and corrosion resistance.
The objective of the present work is to examine the effect of infiltra-
tion method on the parameters of wood-based biomorphous SiC com-
posite. For this purpose, the biomorphous SiC was fabricated by infil-
tration of the carbon template with liquid or vapour silicon (Si).
2. PREPARATION TECHNOLOGY
The technology process of biomorphous SiC preparation is well known
[1—3]. The developed processing scheme for manufacturing of wood-
based biomorphous SiC composite by infiltration method used in this
work is shown in Fig. 1.
Oak, pine, lilac, walnut, acacia woods available in Ukraine with av-
erage dimensions of 20—40 mm in diameter and height of 12 mm were
used as the biological templates in this study. At initial stage, wood
samples were pyrolized at 900°C in argon atmosphere. After pyrolysis,
the carbon templates were reacted with liquid Si produced by melting
Si powder at 1500°C in graphite crucible in inert (Ar) atmosphere. For
this purpose, the resistive furnace (REDMET 30) with graphite cruci-
ble was used. The carbon templates were placed into the graphite cru-
cible together with well-milled Si. The C/Si ratio was of 1/2. Design of
the graphite crucible allows fixing the position of the carbon templates
so that only half of the carbon template was immersed into the Si melt
providing the infiltration of that with both liquid and vapour Si.
The spontaneous Si infiltration of the carbon templates was performed
at 1500—1600°C during 60—120 min in inert atmosphere (Ar or He). Af-
ter that, the temperature was raised up to 1800—1900°C and held for 30—
60 min. During this synthesis and unreacted Si evaporation occurred.
The final material of the reaction was a Si/C composite with a wood-
like microstructure. An excess carbon was burn out in furnace in oxy-
gen atmosphere at 900°C for 2 hours.
EFFECT OF Si INFILTRATION METHOD ON THE BIOMORPHOUS SiC PROPERTIES 239
3. EXPERIMENTAL RESULTS AND DISCUSSION
Optical and scanning electron microscopy (SEM), atomic force micros-
copy, Raman scattering spectroscopy and electron paramagnetic reso-
nance (EPR) were used for compositional and structural analysis of
biomorphous SiC.
Surface and transverse cross section of the template were studied by
SEM after infiltration and carbonizations. Figure 2 shows images of
the transverse cross section of biomorphous SiC grown of walnut.
It was established that the mechanical properties, structure and col-
our of biomorphous SiC depend on the carbon template infiltration
method. The melt infiltration resulted in final material with high me-
Fig. 1. Processing scheme for fabrication of biomorphous SiC.
a
b c
Fig. 2. Photo (a) and SEM images (b, c) of the transverse section of bio-
morphous SiC grown from walnut.
240 V. S. KISELOV, E. N. KALABUKHOVA, A. A. SITNIKOV et al.
chanical strength and green-brown colour which was labelled as SiC-1
(see Fig. 2, b), while the infiltration with Si vapour resulted in final
material of white colour with fibrous structure and was labelled as SiC-
2 (see Fig. 2, c). It was found also that type of infiltration (with liquid
or vapour Si) depends on wood species. The template prepared from
pine and lilac wood were infiltrated only by vapour Si while the tem-
plates prepared from walnut, oak, ash tree, and pear were mainly infil-
trated with liquid Si. This was possibly caused by the different poros-
ity and molecular properties of the carbon template surface prepared
from the wood of various species. The fibrous structure of SiC-2 was
clearly demonstrated when excess carbon was burn out. The fibre di-
ameter is determined by tubular pore sizes in carbon template and var-
ies from 1 to 30 micron. The fibres have a low mechanical strength and
could be easy separated from the carbon template walls.
As it is seen from Figs. 3 and 4, the fibres have flaked structure and
ultrasonic treatment easy separates the flakes.
Fig. 3. Optical microscopy image of tubular fibre packages of the biomor-
phous SiC grown from lilac.
a b
Fig. 4. Photomicrography (a) and AFM image (b) of SiC fibres grown from
pine with scan size of 4×4 μm and Z-range of 0.1 μm.
EFFECT OF Si INFILTRATION METHOD ON THE BIOMORPHOUS SiC PROPERTIES 241
Raman spectra (RS) were taken by double grating spectrometer
DFS-24 at room temperature. The 514.5 nm line of an Ar+
laser was
used for the excitation. The signal was registered with cooled photo-
tube working in photon counting mode in back scattering geometry.
Figure 5 shows RS observed in two types biomorphous SiC grown
from lilac. Analysis of RS peak frequencies observed in biomorphous
SiC shows that biomorphous SiC-1 should be attributed to the 3C
polytype. Slightly higher values of LO and TO phonon bands (TO–796
cm−1
and LO–972 cm
−1) with respect to those in crystalline 3C SiC in-
dicate that the biomorphous SiC is affected by compression. The LO
and TO phonon bands in RS of SiC-2 have lower intensities than in SiC-
1. In addition, a broad band centred at 765 cm
−1
was observed in RS of
SiC-2 and could be attributed to the amorphous phase of SiC [7, 8].
Thus, SiC-2 consists of crystalline and amorphous phase of 3C SiC. It
should be noted that depending on the SiC technology treatment the
disordered (D) and graphitic (G) bands were observed in RS of SiC-1
(see Fig. 5, b) due to clusters of carbon spots [9] which disappeared
when excess carbon was burn out.
EPR spectrum taken on biomorphous SiC-2 at 77 K and 9 GHz is
shown in Fig. 6. The biomorphous SiC-2 under EPR investigation was
preliminary annealed in oxygen atmosphere at 900°C to remove the ex-
cess carbon.
EPR spectrum consists of single intense line with isotropic g-factor
g = 2.0023 and width of 0.3 mT, which could be assigned to the carbon
dangling bonds in 3C SiC [10]. The EPR signal from carbon clusters
was not observed.
Figure 2 shows that 3C SiC grains of 5—10 μm size were formed in the
case of melt infiltration. This conclusion is confirmed by results ob-
tained in [11]. Therefore, it could be suggested that formation of the SiC
and SiC precipitates are caused by process of carbon dissolution in liquid
Si (model via solution-precipitation) [12, 13]. The infiltration with va-
pour Si resulted in smooth-faced, unstructured fibres consisting of
amorphous SiC possibly due to diffusion-controlled process [14—16].
4. SUMMARY
The growth technology and parameters of wood-based biomorphous
SiC ceramics obtained by infiltration with liquid or vapour silicon were
examined. The relationship between infiltration method and micro-
structure of biomorphous SiC was established. It was found that struc-
ture and phase composition of the material depend on the carbon tem-
plate infiltration method. Optical and SEM data indicate that the melt
infiltration results in biomorphous SiC with crystalline phase of 3C
SiC with the faceted morphology while the infiltration with Si vapour
results in SiC with fibrous structure consists of both crystalline and
242 V. S. KISELOV, E. N. KALABUKHOVA, A. A. SITNIKOV et al.
amorphous phases of 3C SiC. Thus, it was suggested that SiC mecha-
nism formation is governed by infiltration method.
REFERENCES
1. P. Greil, T. Lifka, and A. Kaindl, J. Europ. Cer. Soc., 18: 1975 (1998).
2. F. M. Varela-Feria, J. Martinez-Fernandez, A. R. de Arellano-Lopez, and M.
Singh, J. European Ceramic Society, 22: 2719 (2002).
3. M. Presas, J. Y. Pastor, J. Llorca, A. R. Arellano Lopez, J. Martinez Fernandez,
and R. Sepulveda, Int. J. Refractory Metals & Hard Materials, 24: 49 (2006).
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Konttinen, Arch Orthop. Trauma Surg., 118: No. 1—2: 89 (1998).
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Fig. 5. RS of SiC-1 and SiC-2: a–RS of SiC observed in the C—C oscillation
range, 1–SiC-1, 2–SiC-2; b–RS of SiC-1 observed in the 1300—1700 cm
−1
range, 3–as synthesized SiC-1, 4–carbon excess was burn out from SiC-1.
Fig. 6. EPR spectrum recorded at 9 GHz and 77 K in biomorphous SiC-2.
EFFECT OF Si INFILTRATION METHOD ON THE BIOMORPHOUS SiC PROPERTIES 243
Mater. Med., 17: 523 (2006).
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8. S. Klein, L. Houben, R. Carius, F. Finger, and W. Fischer, J. Non-Crystalline
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10. V. S. Kiselov, E. N. Kalabukhova, S. N. Lukin, A. A. Sitnikov, V. A. Yukhym-
chyk, and R. Yakimova, Mat. Sci. Forum, 556—557: 399 (2007).
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12. M. Pyzalski, J. Bialoskorski, and E. Walasek, J. Therm. Anal., 31: 1193 (1986).
13. R. Pampuch, E. Walasek, and J. Bialoskorski, Ceram. Int., 13, No. 1: 63 (1987).
14. P. Greil, T. Lifkaand, and A. Kaindl, J. Eur. Ceram. Soc., 18, No. 14: 1961
(1998).
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|
| id | nasplib_isofts_kiev_ua-123456789-76400 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1816-5230 |
| language | English |
| last_indexed | 2025-12-02T04:02:15Z |
| publishDate | 2009 |
| publisher | Інститут металофізики ім. Г.В. Курдюмова НАН України |
| record_format | dspace |
| spelling | Kiselov, V.S. Kalabukhova, E.N. Sitnikov, A.A. Litvin, P.M. Poludin, V.I. Yukhymchyk, V.A. Belyaev, A.E. 2015-02-10T11:03:56Z 2015-02-10T11:03:56Z 2009 Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties / V.S. Kiselov, E.N. Kalabukhova, A.A. Sitnikov, P.M. Litvin, V.I. Poludin, V.A. Yukhymchyk, A.E. Belyaev // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2009. — Т. 7, № 1. — С. 237-243. — Бібліогр.: 16 назв. — англ. 1816-5230 PACS numbers: 62.23.Pq,68.37.Hk,68.37.Ps,81.16.Fg,83.80.Mc,87.64.-t,87.85.jf https://nasplib.isofts.kiev.ua/handle/123456789/76400 Two types of wood-based biomorphous SiC composites with different microstructure are obtained by infiltration of carbon template with liquid or vapour silicon. The oak, pine, lilac, walnut, acacia woods available in Ukraine are used as the biological template in this work. The SEM, optical and EPR data indicate that biomorphous SiC obtained by melt infiltration consists of crystalline 3C-SiC phase while that obtained by vapour infiltration consists of both crystalline and amorphous 3C-SiC phase. Були одержані два типи деревного біоморфного SiC-композиту з різною мікроструктурою просочення вуглецевого шаблону газоподібним або рідким кремнієм. Деревина дуба, сосни, бузку, волоського горіха, акації, які поширені в Україні, використовувалися як біологічний шаблон у цій роботі. Дані оптичні, СЕМ і ЕПР показали, що одержані просоченням розтопом біоморфні композити SiC складаються із кристалічної й аморфної фаз 3C-SiC. Были получены два типа древесного биоморфного SiC-композита с различной микроструктурой пропитки углеродистого шаблона газообразным или жидким кремнием. Древесина дуба, сосны, сирени, грецкого ореха, акации, распространенные в Украине, использовались как биологический шаблон в этой работе. Данные оптические, СЭМ и ЭПР показали, что полученные пропиткой расплавом биоморфные композиты SiC состоят из кристаллической и аморфной фаз 3C-SiC. en Інститут металофізики ім. Г.В. Курдюмова НАН України Наносистеми, наноматеріали, нанотехнології Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties Article published earlier |
| spellingShingle | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties Kiselov, V.S. Kalabukhova, E.N. Sitnikov, A.A. Litvin, P.M. Poludin, V.I. Yukhymchyk, V.A. Belyaev, A.E. |
| title | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties |
| title_full | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties |
| title_fullStr | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties |
| title_full_unstemmed | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties |
| title_short | Effect of Si Infiltration Method on the Biomorphous SiC Microstructure Properties |
| title_sort | effect of si infiltration method on the biomorphous sic microstructure properties |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/76400 |
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