Preparation of High Specific Surface Area Micro/Meso-porous SiOC Ceramics by the Low Temperature Phase Separation Method

doi:10.15541/jim20180375

Abstract

Abstract:

Micro/meso-porous SiOC ceramics with high surface area and narrow pore size distribution were prepared by the low temperature phase separation method (namely water vapor assisted pyrolysis) followed by etching in hydrofluoric acid (HF) solution. The cross-linked body was made from hydrogen-containing polysiloxane (PHMS), tetramethyl-tetravinylcycletetrasiloxane (D₄^vi) and Pt-complex by thermal cross-linking. Phase compositions, chemical bonds, microstructures, and specific surface area of the prepared SiOC ceramic were investigated by XRD, FT-IR, SEM, and BET, etc. Water vapor can promote the precursor to produce Si-O-Si bonds, SiO₂-rich clusters, and SiO₂ nanocrystals in SiOC ceramics. All of these species act as pore-forming substrate and can be etched away by HF. Water vapor injection and pyrolysis temperature have important effects on phase compositions, microstructures and specific surface area of SiOC porous ceramics, which have a maximum specific surface area of 1845.5 m²/g and pore size distribution of 2.0-10 nm at pyrolysis temperature of 1300℃.

Key words: micro/meso-porous SiOC, low temperature phase separation, phase composition, microstructure, etching

CLC Number:

TQ174

LI Jia-Ke, HAN Xiao-Qi, LIU Xin, WANG Yan-Xiang, GUO Ping-Chun, YANG Zhi-Sheng. Preparation of High Specific Surface Area Micro/Meso-porous SiOC Ceramics by the Low Temperature Phase Separation Method[J]. Journal of Inorganic Materials, 2018, 33(12): 1360-1364.

Figures/Tables 7

Fig. 1 XRD patterns of SiOC ceramics pyrolyzed in Ar +H2O at different temperatures(a) Before etching; (b) After etching

Fig. 2 XRD patterns of SiOC ceramics pyrolyzed in Ar at different temperatures(a) Before etching; (b) After etching

Fig. 3 FT-IR spectra of SiOC ceramics pyrolyzed in Ar+ H2O and Ar at 1300℃ before and after etching

Fig. 4 SEM cross section images of SiOC pyrolyzed at 1300℃ in Ar+H2O before (a) and after (b) etching, in Ar before (c) and after (d) etching

Fig. 5 N2 adsorption (solid symbols) and desorption (open symbols) isotherms for the samples obtained from SiOC ceramics pyrolyzed in (a) Ar +H2O and (b) Ar at 1300℃ after etching

Fig. 6 Cumulative specific surface area (S), interval specific surface area (dS) and pore size distribution (PSD) for SiOC ceramics pyrolyzed in Ar +H2O (a) and in Ar (b) at 1300℃ after etching

Table 1 BET results of SiOC ceramics after etching with different pyrolysis temperatures in Ar and Ar+H2O

Temperature/℃	Specific surface area/ (m²·g^-1)		Average pore size/nm		Pore volume/(cm³·g^-1))
Temperature/℃	Ar	Ar +H₂O	Ar	Ar +H₂O	Ar	Ar +H₂O
900	-	58.6	-	2.05	-	0.105
1100	-	435.23	-	2.16	-	0.142
1200	53.65	654.16	1.43	2.23	0.015	0.202
1300	635.13	1845.50	2.25	2.83	0.282	0.788
1400	632.24	1817.20	2.18	2.75	0.286	0.764
1500	633.52	1805.60	2.15	2.77	0.288	0.756

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