ZrC-ZrB_2-SiC ceramic nanocomposites derived from a novel single-source precursor with high ceramic yield
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摘要
For the first time, ZrC-ZrB_2-SiC ceramic nanocomposites were successfully prepared by a single-source-precursor route, with allylhydridopolycarbosilane(AHPCS),triethylamine borane(TEAB),and bis(cyclopentadienyl) zirconium dichloride(Cp_2 ZrCl_2) as starting materials. The polymer-to-ceramic transformation and thermal behavior of obtained single-source precursor were characterized by means of Fourier transform infrared spectroscopy(FT-IR) and thermal gravimetric analysis(TGA). The results show that the precursor possesses a high ceramic yield about 85% at 1000 ℃.The phase composition and microstructure of formed ZrC-ZrB_2-SiC ceramics were investigated by means of X-ray diffraction(XRD) and high resolution transmission electron microscopy(HRTEM).Meanwhile, the weight loss and chemical composition of the resultant ZrC-ZrB_2-SiC nanocomposites were investigated after annealing at high temperature up to 1800 ℃. High temperature behavior with respect to decomposition as well as crystallization shows a promising high temperature stability of the formed ZrC-ZrB_2-SiC nanocomposites.
For the first time, ZrC-ZrB_2-SiC ceramic nanocomposites were successfully prepared by a single-source-precursor route, with allylhydridopolycarbosilane(AHPCS),triethylamine borane(TEAB),and bis(cyclopentadienyl) zirconium dichloride(Cp_2 ZrCl_2) as starting materials. The polymer-to-ceramic transformation and thermal behavior of obtained single-source precursor were characterized by means of Fourier transform infrared spectroscopy(FT-IR) and thermal gravimetric analysis(TGA). The results show that the precursor possesses a high ceramic yield about 85% at 1000 ℃.The phase composition and microstructure of formed ZrC-ZrB_2-SiC ceramics were investigated by means of X-ray diffraction(XRD) and high resolution transmission electron microscopy(HRTEM).Meanwhile, the weight loss and chemical composition of the resultant ZrC-ZrB_2-SiC nanocomposites were investigated after annealing at high temperature up to 1800 ℃. High temperature behavior with respect to decomposition as well as crystallization shows a promising high temperature stability of the formed ZrC-ZrB_2-SiC nanocomposites.
For the first time, ZrC-ZrB_2-SiC ceramic nanocomposites were successfully prepared by a single-source-precursor route, with allylhydridopolycarbosilane(AHPCS),triethylamine borane(TEAB),and bis(cyclopentadienyl) zirconium dichloride(Cp_2 ZrCl_2) as starting materials. The polymer-to-ceramic transformation and thermal behavior of obtained single-source precursor were characterized by means of Fourier transform infrared spectroscopy(FT-IR) and thermal gravimetric analysis(TGA). The results show that the precursor possesses a high ceramic yield about 85% at 1000 ℃.The phase composition and microstructure of formed ZrC-ZrB_2-SiC ceramics were investigated by means of X-ray diffraction(XRD) and high resolution transmission electron microscopy(HRTEM).Meanwhile, the weight loss and chemical composition of the resultant ZrC-ZrB_2-SiC nanocomposites were investigated after annealing at high temperature up to 1800 ℃. High temperature behavior with respect to decomposition as well as crystallization shows a promising high temperature stability of the formed ZrC-ZrB_2-SiC nanocomposites.
引文
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[9]Zhou H,Gao L,Wang Z,et al.Zr B2-Si C oxidation protective coating on C/C composites prepared by vapor silicon infiltration process.J Am Ceram Soc 2010,93:915-919.
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[19]Wang L,Jiang W,Chen L.Rapidly sintering nanosized Si Cparticle reinforced Ti C composites by the spark plasma sintering(SPS)technique.J Mater Sci 2004,39:4515-4519.
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[24]Cheng J,Wang X,Wang H,et al.Preparation and high-temperature behaviour of Hf C-Si C nanocomposites derived from a non-oxygen single-source-precursor.J Am Ceram Soc 2017,100:5044-5055.
[25]Cai T,Qiu W-F,Liu D,et al.Synthesis of soluble poly-yne polymers containing zirconium and silicon and corresponding conversion to nanosized Zr C/Si C composite ceramics.Dalton Trans 2013,42:4285-4290.
[26]Lu Y,Chen F,An P,et al.Polymer precursor synthesis of Ta C-Si C ultrahigh temperature ceramic nanocomposites.RSC Adv 2016,6:88770-88776.
[27]Li Y,Han W,Li H,et al.Synthesis of nano-crystalline Zr B2/Zr C/Si C ceramics by liquid precursors.Mater Lett2012,68:101-103.
[28]Colombo P,Mera G,Riedel R,et al.Polymer-derived ceramics:40 years of research and innovation in advanced ceramics.J Am Ceram Soc 2010,93:1805-1837.
[29]Yu Z,Huang M,Fang Y,et al.Modification of a liquid polycarbosilane with 9-BBN as a high-ceramic-yield precursor for Si C.React Funct Polym 2010,70:334-339.
[30]Yu Z,Yang L,Min H,et al.Single-source-precursor synthesis of high temperature stable Si C/C/Fe nanocomposites from a processable hyperbranched polyferrocenylcarbosilane with high ceramic yield.J Mater Chem C 2014,2:1057-1067.
[31]Yu Z,Yang L,Zhan J,et al.Preparation,cross-linking and ceramization of AHPCS/Cp2Zr Cl2 hybrid precursors for Si C/Zr C/C composites.J Eur Ceram Soc 2012,32:1291-1298.
[32]Wen Q,Feng Y,Yu Z,et al.Microwave absorption of Si C/Hf Cx N1-x/C ceramic nanocomposites with Hf Cx N1-x-carbon core-shell particles.J Am Ceram Soc2016,99:2655-2663.
[33]Li S,Zhang L,Huang M,et al.In situ synthesis and microstructure characterization of Ti C-Ti B2-Si C ultrafine composites from hybrid precursor.Mater Chem Phys 2012,133:946-953.
[34]Yu Z,Pei Y,Lai S,et al.Single-source-precursor synthesis,microstructure and high temperature behavior of Ti C-Ti B2-Si C ceramic nanocomposites.Ceram Int 2017,43:5949-5956.
[35]Amorós P,Beltrán D,Guillem C,et al.Synthesis and characterization of Si C/MC/C ceramics(M=Ti,Zr,Hf)starting from totally non-oxidic precursors.Chem Mater2002,14:1585-1590.
[36]Drezdzon MA.The Manipulation of Air Sensitive Compounds.Chichester:John Wiley&Sons,1986.
[37]Huang TH,Yu ZJ,He XM,et al.One-pot synthesis and characterization of a new,branched polycarbosilane bearing allyl groups.Chin Chem Lett 2007,18:754-757.
[38]Bianchini D,Barsan MM,Butler IS,et al.Vibrational spectra of silsesquioxanes impregnated with the metallocene catalyst bis(η5-cyclopentadienyl)zirconium(IV)dichloride.Spectrochim Acta A 2007,68:956-969.
[39]Cho M-S,Kim B-H,Kong J-I,et al.Synthesis,catalytic Si-Si dehydrocoupling,and thermolysis of polyvinylsilanes[CH2CH(Si H2X)]n(X=H,Ph).J Organomet Chem 2003,685:99-106.
[40]Corey JY,Rooney SM.Reactions of symmetrical and unsymmetrical disilanes in the presence of Cp2MCl2/nBu Li(M=Ti,Zr,Hf).J Organomet Chem 1996,521:75-91.
[41]Horá?ek M,Pinkas J,Gyepes R,et al.Reactivity of Si Me2H substituents in permethylated titanocene complexes:Dehydrocoupling and ethene hydrosilylation.Organometallics 2008,27:2635-2642.
[42]Takahashi T,Hasegawa M,Suzuki N,et al.Zirconiumcatalyzed highly regioselective hydrosilation reaction of alkenes and X-ray structures of silyl(hydrido)zirconocene derivatives.J Am Chem Soc 1991,113:8564-8566.
[43]Mocaer D,Pailler R,Naslain R,et al.Si-C-N ceramics with a high microstructural stability elaborated from the pyrolysis of new polycarbosilazane precursors.Part I:The organic/inorganic transition.J Mater Sci 1993,28:2615-2631.
[44]Zaheer M,Schmalz T,Motz G,et al.Polymer derived non-oxide ceramics modified with late transition metals.Chem Soc Rev 2012,41:5102-5116.
[2]Pi H,Fan S,Wang Y.C/Si C-Zr B2-Zr C composites fabricated by reactive melt infiltration with Zr Si2 alloy.Ceram Int 2012,38:6541-6548.
[3]Li Q,Dong S,Wang Z,et al.Fabrication and properties of3-D Cf/Si C-Zr C composites,using Zr C precursor and polycarbosilane.J Am Ceram Soc 2012,95:1216-1219.
[4]Fahrenholtz WG,Hilmas GE,Talmy IG,et al.Refractory diborides of zirconium and hafnium.J Am Ceram Soc 2007,90:1347-1364.
[5]Miller-Oana M,Neff P,Valdez M,et al.Oxidation behavior of aerospace materials in high enthalpy flows using an oxyacetylene torch facility.J Am Ceram Soc 2015,98:1300-1307.
[6]Jiang DL.Fine Ceramics Materials.Beijing:Substance Press,2000.(in Chinese)
[7]Lucas R,Davis CE,Clegg WJ,et al.Elaboration of Zr C-Si C composites by spark plasma sintering using polymer-derived ceramics.Ceram Int 2014,40:15703-15709.
[8]Wang H,Chen X,Gao B,et al.Synthesis and characterization of a novel precursor-derived Zr C/Zr B2ultra-high-temperature ceramic composite.Appl Organomet Chem 2013,27:79-84.
[9]Zhou H,Gao L,Wang Z,et al.Zr B2-Si C oxidation protective coating on C/C composites prepared by vapor silicon infiltration process.J Am Ceram Soc 2010,93:915-919.
[10]Shi X-H,Huo J-H,Zhu J-L,et al.Ablation resistance of Si C-Zr C coating prepared by a simple two-step method on carbon fiber reinforced composites.Corros Sci 2014,88:49-55.
[11]Dong ZJ,Liu SX,Li XK,et al.Influence of infiltration temperature on the microstructure and oxidation behavior of Si C-Zr C ceramic coating on C/C composites prepared by reactive melt infiltration.Ceram Int 2015,41:797-811.
[12]Hu C,Niu Y,Huang S,et al.In-situ fabrication of Zr B2-Si C/Si C gradient coating on C/C composites.JAlloys Compd 2015,646:916-923.
[13]Li L,Li H,Li Y,et al.A Si C-Zr B2-Zr C coating toughened by electrophoretically-deposited Si C nanowires to protect C/C composites against thermal shock and oxidation.Appl Surf Sci 2015,349:465-471.
[14]Gleiter H.Nanostructured materials:State of the art and perspectives.Nanostruct Mater 1995,6:3-14.
[15]Sawaguchi A,Toda K,Niihara K.Mechanical and electrical properties of silicon nitride-silicon carbide nanocomposite material.J Am Ceram Soc 1991,74:1142-1144.
[16]Ionescu E,Kleebe H-J,Riedel R.Silicon-containing polymer-derived ceramic nanocomposites(PDC-NCs):Preparative approaches and properties.Chem Soc Rev 2012,41:5032-5052.
[17]Wang X-G,Zhang G-J,Xue J-X,et al.Reactive hot pressing of Zr C-Si C ceramics at low temperature.J Am Ceram Soc 2013,96:32-36.
[18]Wu W-W,Zhang G-J,Kan Y-M,et al.Reactive hot pressing of Zr B2-Si C-Zr C ultra high-temperature ceramics at 1800℃.J Am Ceram Soc 2006,89:2967-2969.
[19]Wang L,Jiang W,Chen L.Rapidly sintering nanosized Si Cparticle reinforced Ti C composites by the spark plasma sintering(SPS)technique.J Mater Sci 2004,39:4515-4519.
[20]Sarin P,Driemeyer PE,Haggerty RP,et al.In situ studies of oxidation of Zr B2 and Zr B2-Si C composites at high temperatures.J Eur Ceram Soc 2010,30:2375-2386.
[21]Yuan J,Hapis S,Breitzke H,et al.Single-source-precursor synthesis of hafnium-containing ultrahigh-temperature ceramic nanocomposites(UHTC-NCs).Inorg Chem 2014,53:10443-10455.
[22]Wen Q,Xu Y,Xu B,et al.Single-source-precursor synthesis of dense Si C/Hf Cx N1-x-based ultrahigh-temperature ceramic nanocomposites.Nanoscale 2014,6:13678-13689.
[23]Cai T,Liu D,Qiu WF,et al.Polymer precursor-derived Hf C-Si C ultrahigh-temperature ceramic nanocomposites.JAm Ceram Soc 2018,101:20-24.
[24]Cheng J,Wang X,Wang H,et al.Preparation and high-temperature behaviour of Hf C-Si C nanocomposites derived from a non-oxygen single-source-precursor.J Am Ceram Soc 2017,100:5044-5055.
[25]Cai T,Qiu W-F,Liu D,et al.Synthesis of soluble poly-yne polymers containing zirconium and silicon and corresponding conversion to nanosized Zr C/Si C composite ceramics.Dalton Trans 2013,42:4285-4290.
[26]Lu Y,Chen F,An P,et al.Polymer precursor synthesis of Ta C-Si C ultrahigh temperature ceramic nanocomposites.RSC Adv 2016,6:88770-88776.
[27]Li Y,Han W,Li H,et al.Synthesis of nano-crystalline Zr B2/Zr C/Si C ceramics by liquid precursors.Mater Lett2012,68:101-103.
[28]Colombo P,Mera G,Riedel R,et al.Polymer-derived ceramics:40 years of research and innovation in advanced ceramics.J Am Ceram Soc 2010,93:1805-1837.
[29]Yu Z,Huang M,Fang Y,et al.Modification of a liquid polycarbosilane with 9-BBN as a high-ceramic-yield precursor for Si C.React Funct Polym 2010,70:334-339.
[30]Yu Z,Yang L,Min H,et al.Single-source-precursor synthesis of high temperature stable Si C/C/Fe nanocomposites from a processable hyperbranched polyferrocenylcarbosilane with high ceramic yield.J Mater Chem C 2014,2:1057-1067.
[31]Yu Z,Yang L,Zhan J,et al.Preparation,cross-linking and ceramization of AHPCS/Cp2Zr Cl2 hybrid precursors for Si C/Zr C/C composites.J Eur Ceram Soc 2012,32:1291-1298.
[32]Wen Q,Feng Y,Yu Z,et al.Microwave absorption of Si C/Hf Cx N1-x/C ceramic nanocomposites with Hf Cx N1-x-carbon core-shell particles.J Am Ceram Soc2016,99:2655-2663.
[33]Li S,Zhang L,Huang M,et al.In situ synthesis and microstructure characterization of Ti C-Ti B2-Si C ultrafine composites from hybrid precursor.Mater Chem Phys 2012,133:946-953.
[34]Yu Z,Pei Y,Lai S,et al.Single-source-precursor synthesis,microstructure and high temperature behavior of Ti C-Ti B2-Si C ceramic nanocomposites.Ceram Int 2017,43:5949-5956.
[35]Amorós P,Beltrán D,Guillem C,et al.Synthesis and characterization of Si C/MC/C ceramics(M=Ti,Zr,Hf)starting from totally non-oxidic precursors.Chem Mater2002,14:1585-1590.
[36]Drezdzon MA.The Manipulation of Air Sensitive Compounds.Chichester:John Wiley&Sons,1986.
[37]Huang TH,Yu ZJ,He XM,et al.One-pot synthesis and characterization of a new,branched polycarbosilane bearing allyl groups.Chin Chem Lett 2007,18:754-757.
[38]Bianchini D,Barsan MM,Butler IS,et al.Vibrational spectra of silsesquioxanes impregnated with the metallocene catalyst bis(η5-cyclopentadienyl)zirconium(IV)dichloride.Spectrochim Acta A 2007,68:956-969.
[39]Cho M-S,Kim B-H,Kong J-I,et al.Synthesis,catalytic Si-Si dehydrocoupling,and thermolysis of polyvinylsilanes[CH2CH(Si H2X)]n(X=H,Ph).J Organomet Chem 2003,685:99-106.
[40]Corey JY,Rooney SM.Reactions of symmetrical and unsymmetrical disilanes in the presence of Cp2MCl2/nBu Li(M=Ti,Zr,Hf).J Organomet Chem 1996,521:75-91.
[41]Horá?ek M,Pinkas J,Gyepes R,et al.Reactivity of Si Me2H substituents in permethylated titanocene complexes:Dehydrocoupling and ethene hydrosilylation.Organometallics 2008,27:2635-2642.
[42]Takahashi T,Hasegawa M,Suzuki N,et al.Zirconiumcatalyzed highly regioselective hydrosilation reaction of alkenes and X-ray structures of silyl(hydrido)zirconocene derivatives.J Am Chem Soc 1991,113:8564-8566.
[43]Mocaer D,Pailler R,Naslain R,et al.Si-C-N ceramics with a high microstructural stability elaborated from the pyrolysis of new polycarbosilazane precursors.Part I:The organic/inorganic transition.J Mater Sci 1993,28:2615-2631.
[44]Zaheer M,Schmalz T,Motz G,et al.Polymer derived non-oxide ceramics modified with late transition metals.Chem Soc Rev 2012,41:5102-5116.