超高温陶瓷B-C-Si-Zr-O部分体系相关系的研究
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摘要
超高温陶瓷材料(UHTCs)是指在超高温环境下具有优良力学、热学、抗热震和抗氧化性能的以金属锆和铪的碳化物和硼化物为主的陶瓷材料。超高温陶瓷材料是新型空间飞行器及运载工具、战略导弹研制中的关键材料,在空间技术发展和国防现代化进程中占有不可替代的地位。有关UHTCs的研究是目前材料界新兴的焦点研究课题。本论文结合国家自然科学基金重点项目(No:50632070):超高温陶瓷相图、材料制备与微结构控制的研究,通过实验测定和相图计算方法(CALPHAD)对B-C-Si-Zr-O五元系的部分相平衡关系进行了系统的研究:
(1)重新评估了B-Zr和Si-Zr二元系的相图和热力学数据,运用CALPHAD技术重新对这两个体系进行了热力学优化与计算。所有计算结果都与实验数据吻合。
(2)应用合金法,采用DSC测试方法和X-射线粉末衍射分析,实验测得B-Si二元系富硅端共晶反应温度为1636K;1253 K下成分为7 at.%B-93at.%Si的合金相组成为:B_3Si和Si端际固溶体。通过评估最新文献中有关相图和热力学性质的实验信息,重新优化计算了B-Si二元系,计算相图和热力学性质与实验数据相一致。在此基础上,根据文献报道的B-C-Si三元系的相平衡关系和零变量反应信息,优化计算了B-C-Si三元系,获得了一组合理自洽的热力学参数。计算得到的B-C-Si三元系的垂直截面、等温截面和零变量反应均与报道数据结果相吻合。
(3)采用歧化反应方法制备了C-SiC-ZrC复合材料。实验确定了C-Si-Zr三元系在1473K的部分相平衡关系。根据本文实测和文献报道的相平衡关系的实验结果,优化计算了C-Si-Zr三元系。计算得到C-Si-Zr三元系的等温截面与实验结果相吻合。
(4)优化和计算了B-C-Zr三元系相图。其中假想化合物ZrC_2和ZrB的0K形成焓(~(0K)H_(Zr:C)~(ZrB_2)和~(0K)H_(Zr:B)~(ZrC_x))通过第一原理计算得到。计算得到的B-C-Zr三元系等温截面和垂直截面均与实验数据吻合较好,计算的部分零变量反应与文献报道的计算结果一致。在相图热力学计算和局部平衡原理的基础上,通过计算比较界面处局部平衡时各相形成驱动力的大小和考虑界面组元扩散的因素,较好地解释了文献报道的液态锆与碳化硼界面反应产物以及反应机理。
(5)采用合金法,借助金相、扫描电子显微镜和X-射线衍射分析等检测分析手段,实验测定了B-Si-Zr三元系在1253K下富Zr侧的相关系和电弧炉熔样的铸态相组成。根据本文实测数据和文献报道的相平衡关系和热力学数据,优化计算了B-Si-Zr三元系,获得了一组合理自洽的热力学参数。
(6)采用固相反应法烧结制备了33.33 at.%B_2O_3-66.67 at.%ZrO_2和60 at.%B_2O_3-40 at.%ZrO_2两个样品,分别在1073K和623K温度退火7天。X-射线衍射显示退火后的样品中只有m_ZrO_2和B_2O_3两个相,没有出现新相,表明该二元系不存在中间化合物。然后,通过评估文献中有关相图和热力学数据,优化计算了B_2O_3-SiO_2-ZrO_2三元系的三个边际赝二元体系,计算相图和热力学性质与实验数据相一致。在此基础上,结合计算得到的边际二元系的热力学参数,直接外推计算了B_2O_3-SiO_2-ZrO_2赝三元体系。
(7)采用最新报道的ZrO_2的晶格稳定性参数,采用双亚点阵离子溶液模型描述液相Gibbs能,成功优化和计算了Si-Zr-O、C-Si-O和C-Zr-O三元系。计算所得的Si-Zr-O和C-Si-O的等温截面与实验数据吻合较好。计算预测了C-Zr-O三元系的相关系图。
Ultra-high temperature ceramics(UHTCs) mainly refer to the early transition metal(e.g.,Zr,Hf) diborides or carbides with excellent mechanical,thermodynamic properties and thermal shock resistance, oxidation resistance under extremely high temperature conditions.The UHTCs are one class of key material in the study of new spacecraft and carrier and strategic missile,playing an important role in the development of space technology and modernization of national defense.At present, research with respect to UHTCs is an emerging focus in the field of materials.As part of the project "investigation of phase diagram,material preparation and microstructure control of UHTCs" supported financially by National Science Foundation of China(No.50632070),the partial phase equilibrium relationship of the B-C-Si-Zr-O quinary system was investigated through experimental measurements and CALPHAD approach in the present work.The thesis is comprised of seven parts:
(1) The binary B-Zr and Si-Zr systems have been reassessed using the CALPHAD method on the basis of the available experimental data. The self-consistent thermodynamic parameters formulating Gibbs energies of various phases in these two binary systems have been obtained.Thermodynamic properties of liquid phases and intermetallics and phase diagrams have been calculated,which are in reasonable agreement with the reported experimental data.
(2) Based on the critically assessed B-Si phase diagram,one alloy of Sirich side was selected and the temperature associated with the eutectic reaction was measured to be 1636 K by DSC.And the phase relations of alloy 7at.%B-93at.%Si at 1253K have been investigated by XRD method.The experimental result shows that this alloy consists of two phases,B_3Si and silicon solution.The B-Si system has been reassessed using a regular substitutional model for the liquid.This improved description can be used with confidence to obtain descriptions for higher order alloys.Thermodynamic description for the B-C-Si system has been developed based on critically reviewed experimental data.The calculated phase diagrams are in good agreement with available experimental data.
(3) The reaction between Zr and SiC at 1473K in vacuum has been studied.A layered structure was observed after high temperature reactions between Zr and SiC complex.ZrC_x was formed next to the SiC.Thermodynamic description of the C-Si-Zr system was developed based on its constituent binaries and critically reviewed experimental data.The high-temperature Zr_5Si_3 phase and the ternary compound Zr_5Si_3C_x were described as one phase,using the model (Zr)_5(Si)_3(C,Va)_1.Reasonable agreement between the calculated and experimental data was achieved.
(4) The phase diagram of B-C-Zr ternary system was thermodynamically assessed.Adopting the enthalpy of formation data at 0 K calculated by first-principles method for assumed compounds ZrC_2 and ZrB (~(0K)H_(Zr:C)~(ZrB_2) and ~(0K)H_(Zr:B)~(ZrC_x)),the calculated isothermal and isoplethic sections agree well with those of experiments,so do the most of the calculated invariant reactions.In order to simulate the solidification path of the ternary alloy,Scheil-Gulliver model has been employed. The solidification products are obtained by calculation coupling with experimental works.The calculation results show that the experiments can be simulated satisfactorily.
(5) By means of annealing method,metallography,scanning electron microscopy(SEM) and X-ray diffraction analysis(XRD),the isothermal section of Zr-rich region at 1253 K and phase constitution of the electric-arc melted cast-state sample were determined.On the basis of experimental information of the phase equilibrium relationship and thermodynamic properties from experimental measurement and literature report,the B-Si-Zr temary system was assessed and a set of thermodynamic parameters was obtained to reasonably describe the Gibbs energy of all the phases.
(6) Powder samples 33.33 at.%B_2O_3-66.67 at.%ZrO_2 and 60 at.% B_2O_3-40 at.%ZrO_2 were sintered and prepared with solid state reaction,followed by annealing at 1073 K and 623 K,respectively, for seven days.As is shown from the X-ray diffraction analysis,there were only two phases m_ZrO_2 and B_2O_3 and no intermetallic compound existed in the binary system.Then,three constitutional pseudo-binary systems in the B_2O_3-SiO_2-ZrO_2 system were optimized by evaluating the experimental information of phase diagram and thermodynamic properties in literatures with which the calculated results agreed well.Incorporating the optimized thermodynamic parameters of the constitutional binary systems,the B_2O_3-SiO_2-ZrO_2 pseudo-ternary system was extrapolated.
(7) Using the latest lattice stability parameter of ZrO_2,two-sublattice ionic solution model was adopted to describe the Gibbs energy of liquid phases,and then Si-Zr-O,C-Si-O and C-Zr-O ternary systems were assessed successfully.The calculated isothermal sections of Si-Zr-O and C-Si-O agreed well with those of experiments and the phase diagram of C-Zr-O ternary system was predicted through calculations.
(1)重新评估了B-Zr和Si-Zr二元系的相图和热力学数据,运用CALPHAD技术重新对这两个体系进行了热力学优化与计算。所有计算结果都与实验数据吻合。
(2)应用合金法,采用DSC测试方法和X-射线粉末衍射分析,实验测得B-Si二元系富硅端共晶反应温度为1636K;1253 K下成分为7 at.%B-93at.%Si的合金相组成为:B_3Si和Si端际固溶体。通过评估最新文献中有关相图和热力学性质的实验信息,重新优化计算了B-Si二元系,计算相图和热力学性质与实验数据相一致。在此基础上,根据文献报道的B-C-Si三元系的相平衡关系和零变量反应信息,优化计算了B-C-Si三元系,获得了一组合理自洽的热力学参数。计算得到的B-C-Si三元系的垂直截面、等温截面和零变量反应均与报道数据结果相吻合。
(3)采用歧化反应方法制备了C-SiC-ZrC复合材料。实验确定了C-Si-Zr三元系在1473K的部分相平衡关系。根据本文实测和文献报道的相平衡关系的实验结果,优化计算了C-Si-Zr三元系。计算得到C-Si-Zr三元系的等温截面与实验结果相吻合。
(4)优化和计算了B-C-Zr三元系相图。其中假想化合物ZrC_2和ZrB的0K形成焓(~(0K)H_(Zr:C)~(ZrB_2)和~(0K)H_(Zr:B)~(ZrC_x))通过第一原理计算得到。计算得到的B-C-Zr三元系等温截面和垂直截面均与实验数据吻合较好,计算的部分零变量反应与文献报道的计算结果一致。在相图热力学计算和局部平衡原理的基础上,通过计算比较界面处局部平衡时各相形成驱动力的大小和考虑界面组元扩散的因素,较好地解释了文献报道的液态锆与碳化硼界面反应产物以及反应机理。
(5)采用合金法,借助金相、扫描电子显微镜和X-射线衍射分析等检测分析手段,实验测定了B-Si-Zr三元系在1253K下富Zr侧的相关系和电弧炉熔样的铸态相组成。根据本文实测数据和文献报道的相平衡关系和热力学数据,优化计算了B-Si-Zr三元系,获得了一组合理自洽的热力学参数。
(6)采用固相反应法烧结制备了33.33 at.%B_2O_3-66.67 at.%ZrO_2和60 at.%B_2O_3-40 at.%ZrO_2两个样品,分别在1073K和623K温度退火7天。X-射线衍射显示退火后的样品中只有m_ZrO_2和B_2O_3两个相,没有出现新相,表明该二元系不存在中间化合物。然后,通过评估文献中有关相图和热力学数据,优化计算了B_2O_3-SiO_2-ZrO_2三元系的三个边际赝二元体系,计算相图和热力学性质与实验数据相一致。在此基础上,结合计算得到的边际二元系的热力学参数,直接外推计算了B_2O_3-SiO_2-ZrO_2赝三元体系。
(7)采用最新报道的ZrO_2的晶格稳定性参数,采用双亚点阵离子溶液模型描述液相Gibbs能,成功优化和计算了Si-Zr-O、C-Si-O和C-Zr-O三元系。计算所得的Si-Zr-O和C-Si-O的等温截面与实验数据吻合较好。计算预测了C-Zr-O三元系的相关系图。
Ultra-high temperature ceramics(UHTCs) mainly refer to the early transition metal(e.g.,Zr,Hf) diborides or carbides with excellent mechanical,thermodynamic properties and thermal shock resistance, oxidation resistance under extremely high temperature conditions.The UHTCs are one class of key material in the study of new spacecraft and carrier and strategic missile,playing an important role in the development of space technology and modernization of national defense.At present, research with respect to UHTCs is an emerging focus in the field of materials.As part of the project "investigation of phase diagram,material preparation and microstructure control of UHTCs" supported financially by National Science Foundation of China(No.50632070),the partial phase equilibrium relationship of the B-C-Si-Zr-O quinary system was investigated through experimental measurements and CALPHAD approach in the present work.The thesis is comprised of seven parts:
(1) The binary B-Zr and Si-Zr systems have been reassessed using the CALPHAD method on the basis of the available experimental data. The self-consistent thermodynamic parameters formulating Gibbs energies of various phases in these two binary systems have been obtained.Thermodynamic properties of liquid phases and intermetallics and phase diagrams have been calculated,which are in reasonable agreement with the reported experimental data.
(2) Based on the critically assessed B-Si phase diagram,one alloy of Sirich side was selected and the temperature associated with the eutectic reaction was measured to be 1636 K by DSC.And the phase relations of alloy 7at.%B-93at.%Si at 1253K have been investigated by XRD method.The experimental result shows that this alloy consists of two phases,B_3Si and silicon solution.The B-Si system has been reassessed using a regular substitutional model for the liquid.This improved description can be used with confidence to obtain descriptions for higher order alloys.Thermodynamic description for the B-C-Si system has been developed based on critically reviewed experimental data.The calculated phase diagrams are in good agreement with available experimental data.
(3) The reaction between Zr and SiC at 1473K in vacuum has been studied.A layered structure was observed after high temperature reactions between Zr and SiC complex.ZrC_x was formed next to the SiC.Thermodynamic description of the C-Si-Zr system was developed based on its constituent binaries and critically reviewed experimental data.The high-temperature Zr_5Si_3 phase and the ternary compound Zr_5Si_3C_x were described as one phase,using the model (Zr)_5(Si)_3(C,Va)_1.Reasonable agreement between the calculated and experimental data was achieved.
(4) The phase diagram of B-C-Zr ternary system was thermodynamically assessed.Adopting the enthalpy of formation data at 0 K calculated by first-principles method for assumed compounds ZrC_2 and ZrB (~(0K)H_(Zr:C)~(ZrB_2) and ~(0K)H_(Zr:B)~(ZrC_x)),the calculated isothermal and isoplethic sections agree well with those of experiments,so do the most of the calculated invariant reactions.In order to simulate the solidification path of the ternary alloy,Scheil-Gulliver model has been employed. The solidification products are obtained by calculation coupling with experimental works.The calculation results show that the experiments can be simulated satisfactorily.
(5) By means of annealing method,metallography,scanning electron microscopy(SEM) and X-ray diffraction analysis(XRD),the isothermal section of Zr-rich region at 1253 K and phase constitution of the electric-arc melted cast-state sample were determined.On the basis of experimental information of the phase equilibrium relationship and thermodynamic properties from experimental measurement and literature report,the B-Si-Zr temary system was assessed and a set of thermodynamic parameters was obtained to reasonably describe the Gibbs energy of all the phases.
(6) Powder samples 33.33 at.%B_2O_3-66.67 at.%ZrO_2 and 60 at.% B_2O_3-40 at.%ZrO_2 were sintered and prepared with solid state reaction,followed by annealing at 1073 K and 623 K,respectively, for seven days.As is shown from the X-ray diffraction analysis,there were only two phases m_ZrO_2 and B_2O_3 and no intermetallic compound existed in the binary system.Then,three constitutional pseudo-binary systems in the B_2O_3-SiO_2-ZrO_2 system were optimized by evaluating the experimental information of phase diagram and thermodynamic properties in literatures with which the calculated results agreed well.Incorporating the optimized thermodynamic parameters of the constitutional binary systems,the B_2O_3-SiO_2-ZrO_2 pseudo-ternary system was extrapolated.
(7) Using the latest lattice stability parameter of ZrO_2,two-sublattice ionic solution model was adopted to describe the Gibbs energy of liquid phases,and then Si-Zr-O,C-Si-O and C-Zr-O ternary systems were assessed successfully.The calculated isothermal sections of Si-Zr-O and C-Si-O agreed well with those of experiments and the phase diagram of C-Zr-O ternary system was predicted through calculations.
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