燃烧合成过程中过渡金属碳化物、硼化物的生长行为
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摘要
过渡金属碳化物、硼化物由于具有许多优良的物理和化学性能，比如，高熔点、高硬度、高模量、高导电与导热性和高的化学稳定性等优点，在机械、化学和微电子领域被广泛应用，常用作高温陶瓷，高性能切削和耐磨工件，尤其是硬质合金中的增强相或复合材料中的增强体。众所周知，陶瓷颗粒的形貌和尺寸对陶瓷颗粒增强金属基复合材料的性能有着至关重要的影响。形状圆整的陶瓷颗粒增强金属基复合材料将比不规则形状的陶瓷颗粒增强金属基复合材料具有更好的综合性能。因此，研究陶瓷颗粒的生长形貌、生长机制及其控制因素，具有重要的理论和实际意义，将为实现陶瓷颗粒形貌的主动控制，发展先进的陶瓷颗粒增强金属基复合材料奠定必需的理论基础。此外，陶瓷晶体的非平衡生长动力学及其机制本身，就是晶体生长理论领域一个不断探索和深入研究的前沿与热点问题。事实上，由于燃烧合成陶瓷相是一个高温、快速、非线性、非稳态的传输过程（能量、质量和动量传输），同时，伴随着许多复杂的化学与物理现象，因此，影响陶瓷颗粒生长行为的因素是非常复杂的。目前，尽管国内外关于燃烧合成陶瓷颗粒的生长形貌开展了一些研究，也取得了一定进展，但是仅仅局限在燃烧动力学对陶瓷颗粒生长形貌影响规律的这个层面上，对陶瓷颗粒增强金属基复合材料制备过程中的关键基础理论问题，尤其是陶瓷颗粒的生长行为与机制缺乏系统、深入的研究。
因此，本论文研究不同燃烧合成体系（Al–Ti/Zr/Nb/Ta–C/B）反应过程中，陶瓷颗粒（TiC_x、ZrC_x、NbC_x、TaC_x、TiB_2、ZrB_2、NbB_(2x)、TaB_(2x)）的生长形貌及其演化过程；揭示不同陶瓷结构、不同动力学条件对燃烧合成陶瓷颗粒生长行为的影响规律；提出不同类型陶瓷的生长机制及其共性与个性规律。
本文的主要研究结果如下：
1)发现Al含量、碳源尺寸和原始反应物C/Ti摩尔比对Al–Ti–C体系SHS反应合成的TiC_x颗粒的生长形貌有着重要的影响；揭示出在SHS反应过程中，TiC_x颗粒的生长形貌随着计量比x值由低到高的演化规律为：从八面体→切角八面体→近球形→球形；建立了计量比与TiC_x颗粒生长形貌的关系，即当计量比x值较低时，TiC_x颗粒的生长形貌为八面体；当计量比x值较高时，TiC_x颗粒的生长形貌为切角八面体；当计量比x值进一步升高，TiC_x颗粒的生长形貌转变为近球形和球形。
2)揭示出SHS反应过程中，TiC_x颗粒的生长方式主要为{111}面的二维层状生长。提出了TiC_x的计量比x值是TiC_x颗粒生长形貌演化的主要控制因素：当生成的TiC_x的计量比x值较低时，{111}面非常稳定，TiC_x以八面体状形核生长；随着计量比x值的升高，{111}面的稳定性下降，{100}面逐渐显露，TiC_x颗粒的生长形貌由八面体转变为切角八面体；当燃烧温度高于TR≈1800°C时，{100}面发生热力学粗糙化转变，变为圆滑曲面，从而形成了近球形的TiC_x颗粒；随着TiC_x计量比x值的进一步升高，{100}圆滑曲面逐渐长大、连结，使得TiC_x颗粒变的越来越圆。
3)首次发现通过Al–Ti/Zr/Nb–B体系SHS反应合成的过渡金属硼化物的生长形貌存在形貌演化和生长成球形的必要条件是其计量比要存在一个较宽的区间：TiB_2和ZrB_2的计量比区间很窄，即使燃烧温度很高，它们的形貌没有发生明显的变化，均为六棱柱状。而NbB_(2x)的计量比区间很宽，因此，Al含量和原始反应物中的B/Nb摩尔比对合成的NbB_(2x)颗粒的生长形貌有着重要影响。揭示出在SHS反应过程中，NbB_(2x)颗粒的生长形貌随着计量比2x值由低到高的演化规律为：由六棱柱→多面体→近球形→球形；建立了计量比与NbB_(2x)颗粒生长形貌的关系，即在燃烧温度或B/Nb摩尔比较低时，反应生成的NbB_(2x)计量比较低，对应NbB_(2x)颗粒的生长形貌为规则的六棱柱；而在燃烧温度和B/Nb摩尔比较高时，反应生成的NbB_(2x)的计量比较高，对应NbB_(2x)颗粒的生长形貌多为近球形和球形。揭示出SHS反应过程中，TiB_2、ZrB_2和NbB_(2x)颗粒的生长方式均为{0001}和{1010}面的二维层状生长。
4)揭示出计量比2x值是NbB_(2x)颗粒生长形貌演化的主要控制因素，首次提出NbB_(2x)的球形生长机制：当计量比较低时，{0001}和{1010}面非常稳定，NbB_(2x)颗粒生长为六棱柱状；随着计量比的升高，{0001}和{1010}面的稳定性逐渐下降，{1101}面逐渐显露，NbB_(2x)颗粒的生长形貌由六棱柱转变为多面体；当燃烧温度很高，且超过一定值后，{1101}面发生粗糙化转变，变为圆滑曲面，从而导致NbB_(2x)颗粒由多面体转变为近球形；随着计量比的进一步升高，{1101}曲面逐渐长大，NbB_(2x)颗粒变的越来越圆。
5)提出了在燃烧合成过程中，过渡金属陶瓷TMCs（TiC_x、NbC_x、ZrC_x、TaC_x）、TMNs（TiNx）、TMDs（TiB_2、ZrB_2、NbB_(2x)、TaC2x）颗粒生长形貌演化的个性与共性规律。
ⅰ)共性规律：
提出了SHS反应合成TMCs、TMNs、TMDs生长形貌发生演化的必要条件是其计量比区间要宽；建立了SHS反应合成TMCs、TMNs、TMDs的计量比与生长形貌演化的关系；同时，揭示了燃烧温度对生长形貌球化动力学的影响规律，即随着化学计量比和燃烧温度由低到高，TMCs、TMNs、TMDs生长形貌的变化规律为：TMCs、TMNs：八面体→切角八面体→近球形→球形；TMDs：六棱柱→多面体→近球形→球形。
ⅱ)个性规律：揭示出不具有较宽计量比区间的TiB_2和ZrB_2在燃烧合成过程中不存在生长形貌的演变过程。
6)揭示出使用碳纳米管（CNTs）作为碳源，能够明显增加Me (Cu/Al/Fe)–Ti–CNTs体系的反应活性，使传统的Cu/Al/Fe–Ti–C（石墨、碳黑）体系完全反应的最高金属含量由67.12wt.%Cu、46.65wt.%Al、77.4wt.%Fe提高到80wt.%Cu、70wt.%Al、80wt.%Fe；发现使用CNTs作为碳源，在高含量Me (Cu/Al/Fe)–Ti–CNTs体系，合成具有不同形状、纳米尺寸的TiC_x颗粒。
7)揭示出在Me (Cu/Al/Fe)–Ti–CNTs体系中，金属组元Me (Cu/Al/Fe)对TiC_x颗粒生长尺寸与形貌的影响规律与作用机制：在Fe–Ti–CNTs体系中，由于C在Fe熔体中溶解速度较快而扩散速度较慢，TiC_x颗粒在富[C]区域中快速形核、生长，因此，TiC_x具有较高的计量比，生长形貌多为立方体和近球状，且尺寸较大。反之，在Cu/Al–Ti–CNTs体系中，由于C在Cu/Al熔体中溶解速度较慢而扩散速度较快，TiC_x在十分贫[C]的环境下形核、生长，导致生成的TiC_x颗粒的计量比非常低，生长形貌多为八面体状，且尺寸较小。
总之，本文通过对不同体系燃烧合成过程中，过渡金属陶瓷颗粒的生长行为的研究，揭示了不同陶瓷结构、不同动力学条件对过渡金属陶瓷颗粒生长行为的影响规律；提出了不同类型陶瓷的生长机制及其共性与个性规律；为实现陶瓷颗粒形貌的主动控制，发展先进的陶瓷颗粒增强金属基复合材料奠定必需的理论基础。
Due to many excellent physical and chemical properties, such as high melting point,high hardness, high modulus, high thermal conductivity and high chemical stability,transition metal carbides and borides are widely used in mechanical, chemical andmicroelectronics applications. They are generally used as high–temperature ceramics,high–performance cutting and wear–resistant workpiece, especially reinforcing particles inthe cemented carbide or composite materials. As known, the morphology of the reinforcingceramic particles in the ceramic reinforced metal matrix composites has a critical impact ontheir properties. The matrix composites with round reinforcing particles have betterproperties than those with irregular shaped reinforcing particles. Therefore, it is of greatpractical significance to study the growth morphology, growth mechanism and thecontrolling factors for the ceramic particles. Moreover, the non–equilibrium growth kinetics(and mechanism) of the ceramics is also an important exploration and research direction inthe theoretical field of crystal growth. In fact, the combustion synthesis of ceramics is a hightemperature, fast, non–linear, non–steady–state transfer process, accompanied by numerouschemical and physical phenomena. Therefore, the factors influencing the growth behavior ofthe ceramics are very complicated. So far, there have been some work on the growthmorphology of the ceramic particles formed during combustion synthesis. However, thesework are mainly focused on the influencing regularity of the combustion kinetics on thegrowth morphology of the ceramic particles. The study on the underlying key theoreticalquestions during the fabrication of the ceramic–metal composites, especially the growthbehavior and mechanism of the ceramic particles, is rather limited.
Therefore, in this thesis, the growth behaviors of the ceramic particles (TiC_x, ZrC_x,NbC_x, TaC_x, TiB2, ZrB2, NbB2xand TaB2x) formed in the combustion systems ofAl–Ti/Zr/Nb/Ta–C/B were studied; the influencing regularity of the ceramic structures andthe kinetics conditions on the growth behavior of the ceramic particles were revealed; thegrowth mechanisms of different ceramic particles and their commonness and individuality were discussed.
The main results are as follows:
1) It was found that the Al content, carbon source and reactant C/Ti molar ratio haveimportant effects on the growth morphology of the TiC_xparticles formed in the Al–Ti–Csystem; The morphology evolution regularity of the TiC_xparticles with the increasingstoichiometry during the SHS was suggested as from octahedron→truncated–octahedron→sphere–like→sphere; The relationship between the growth morphology of the TiC_xand its stoichiometry was established, that is, in the case of quite low stoichiometry, theTiC_xparticles grow to octahedron, while in the case of relatively high stoichiometry, theTiC_xparticles grow to truncated–octahedron, and when the stoichiometry furtherincreases, the TiC_xparticles grow to sphere–like and sphere.
2) The growth mode of the TiC_xparticles during the SHS was suggested as thetwo–dimensional layer growth on the {111} surfaces. The main controlling factor of thegrowth morphology of the TiC_xparticles was suggested as the stoichiometry: When thestoichiometry of the formed TiC_xis very low, the {111} surfaces are quite stable, and theTiC_xparticles nucleate and grow as octahedron. With the increase in the stoichiometry,the {111} surfaces become less–stable, and the {100} surfaces begain to be exposed.Then, the shapes of the TiC_xparticles change from octahedron to truncated–octahedron.If the combustion temperature is higher than TR≈1800°C, the {100} surfaces undergoa roughening transition and become round, which makes the TiC_xbecome thespherical–like particles. With the further increase in the stoichiometry or combustiontemperature, the {100} surface grow up gradually, and the TiC_xparticles become moreand more round.
3) It was found firstly that necessary condition for the existence of the morphologyevolution and spherical growth shape for the transition metal diborides formed duringthe SHS in Al–Ti/Zr/Nb–B systems is there must exist a wide stoichiometric range. Forthe borides (TiB_2and ZrB_2) with no wide stoichiometric ranges, even the combustiontemperature becomes quite high, their shapes don’t change considerably and keep beingthe hexagonal–prisms, while for NbB_(2x)with a wide stoichiometric range, itsmorphology changes significantly with the Al content and the reactant B/Nb molar ratio;The morphology evolution regularity of the NbB_(2x)particles during the SHS with theincreasing stoichiometry was suggested as from hexagonal–prisms→polyhedron→sphere–like→sphere; The relationship between the growth morphology of the NbB_(2x)and its stoichiometry was established, that is, in the case of low stoichiometry, the NbB_(2x)particles grow to hexagonal–prisms, while in the case of high stoichiometry, the NbB_(2x)particles grow to sphere–like and sphere. The growth mode of the TiB_2, ZrB_2and NbB_(2x)particles during the SHS was suggested as the two–dimensional layer growth on the {0001}and {1010}surfaces.
4) The main controlling factor of the growth morphology of the NbB_(2x)particles wassuggested as the stoichiometry, and the spherical growth mechanism of the NbB_(2x)particles was firstly proposed: When the stoichiometry is low, the {0001}and {1010}surfaces are very stable, and the NbB_(2x)particles grow to the hexagonal–prisms. With theincrease in the stoichiometry, and stability of the {0001}and {1010}surfaces isgradually decreased; while the {1101}surfaces gradually emerge. Then, the NbB_(2x)particles change their shapes from hexagonal–prism to polyhedron. When thecombustion temperature is high and exceeds a certain value, the {1101}surfacescomposed with the side–facets of the growth steps are rourhed and become round,inducing the formation of the spherical–like NbB_(2x)particles. With the further increase inthe stoichiometry, the NbB_(2x)particles become more and more round.
5) The commonness and individuality of the morphology evolution of the transition metalcarbides (TiC_x, ZrC_x, NbC_xand TaC_x), nitrides (TiNx) and borides (TiB_2, ZrB_2, NbB_(2x)and TaC2x) during the SHS were summarized.
ⅰ) Commonness:The necessary condition for the morphology evolution of the TMCs, TMNs andTMDs particles during the SHS was suggested as the wide stoichiometric ranges; Therelationship between the growth morphology and their stoichiometry was establishedand the effect of the combustion temperature on the spherical kinetics of the growthmorphology was revealed, that is, with the increase in the combustion temperature andstoichiometry, the morphology of the TMCs and TMNs evolves from octahedron→truncated–octahedron→sphere–like→sphere, and that of the TMDs evolves fromhexagonal–prisms→polyhedron→sphere–like→sphere.
ⅱ) Individuality:For the borides (TiB_2and ZrB_2) with no wide stoichiometric ranges, there is nomorphology evolution for them during the SHS.
6) It was disclosed that the reactive activity of the Me (Cu/Al/Fe)–Ti–CNTs systems can begreatly increased with using CNTs as carbon source, and the higheat metal contents forthe complete raction during the SHS were increased from67.12wt.%Cu,46.65wt.%Aland77.4wt.%Fe to80wt.%Cu,70wt.%Al and80wt.%Fe, respectively; With usingthe CNTs as carbon source, the nano TiC_xparticles with different shapes can besynthesized in the Me (Cu/Al/Fe)–Ti–CNTs systems with high metal contents.
7) The influence regularity and affect mechanism of the metal component on the size andmorphology of the TiC_xparticles formed in the Me (Cu/Al/Fe)–Ti–CNTs systems weredisclosed: In the Fe–Ti–CNTs system, because of the fast dissolution rate but the low diffusion rate of carbon in Fe, the TiC_xparticles form in the [C]–rich regions and growrapidly to relatively larger sizes. Moreover, the stoichiometry of these formed TiC_xparticles in the Fe melt is relatively high and thus their growth shapes are cube andsphere–like. In the Cu–and Al–Ti–CNTs systems, the CNTs dissolve more slowlybecause of the poor chemical reactivity. In this case, the TiC_xforms and grows under acondition of [C] scarcity. Hence, the TiC_xparticles grown in these two melts are withrelatively small sizes, and the TiC_xstoichiometry formed at the combustion stage is low,and accordingly, the TiC_xgrowth shape is octahedron.
In summary, in this thesis, the growth behaviors of the ceramic particles (TiC_x, ZrC_x,NbC_x, TaC_x, TiB_2, ZrB_2, NbB_(2x)and TaB_(2x)) formed in the combustion systems ofAl–Ti/Zr/Nb/Ta–C/B were studied; the influencing regularity of the ceramic structures andthe kinetics conditions on the growth behavior of the ceramic particles was revealed; thegrowth mechanisms of different ceramic particles and their commonness and individualitywere suggested, which lays the necessary theoretical basis for the active control of theceramic particle morphology and the development of advanced ceramic particles reinforcedmetal matrix composites.
因此，本论文研究不同燃烧合成体系（Al–Ti/Zr/Nb/Ta–C/B）反应过程中，陶瓷颗粒（TiC_x、ZrC_x、NbC_x、TaC_x、TiB_2、ZrB_2、NbB_(2x)、TaB_(2x)）的生长形貌及其演化过程；揭示不同陶瓷结构、不同动力学条件对燃烧合成陶瓷颗粒生长行为的影响规律；提出不同类型陶瓷的生长机制及其共性与个性规律。
本文的主要研究结果如下：
1)发现Al含量、碳源尺寸和原始反应物C/Ti摩尔比对Al–Ti–C体系SHS反应合成的TiC_x颗粒的生长形貌有着重要的影响；揭示出在SHS反应过程中，TiC_x颗粒的生长形貌随着计量比x值由低到高的演化规律为：从八面体→切角八面体→近球形→球形；建立了计量比与TiC_x颗粒生长形貌的关系，即当计量比x值较低时，TiC_x颗粒的生长形貌为八面体；当计量比x值较高时，TiC_x颗粒的生长形貌为切角八面体；当计量比x值进一步升高，TiC_x颗粒的生长形貌转变为近球形和球形。
2)揭示出SHS反应过程中，TiC_x颗粒的生长方式主要为{111}面的二维层状生长。提出了TiC_x的计量比x值是TiC_x颗粒生长形貌演化的主要控制因素：当生成的TiC_x的计量比x值较低时，{111}面非常稳定，TiC_x以八面体状形核生长；随着计量比x值的升高，{111}面的稳定性下降，{100}面逐渐显露，TiC_x颗粒的生长形貌由八面体转变为切角八面体；当燃烧温度高于TR≈1800°C时，{100}面发生热力学粗糙化转变，变为圆滑曲面，从而形成了近球形的TiC_x颗粒；随着TiC_x计量比x值的进一步升高，{100}圆滑曲面逐渐长大、连结，使得TiC_x颗粒变的越来越圆。
3)首次发现通过Al–Ti/Zr/Nb–B体系SHS反应合成的过渡金属硼化物的生长形貌存在形貌演化和生长成球形的必要条件是其计量比要存在一个较宽的区间：TiB_2和ZrB_2的计量比区间很窄，即使燃烧温度很高，它们的形貌没有发生明显的变化，均为六棱柱状。而NbB_(2x)的计量比区间很宽，因此，Al含量和原始反应物中的B/Nb摩尔比对合成的NbB_(2x)颗粒的生长形貌有着重要影响。揭示出在SHS反应过程中，NbB_(2x)颗粒的生长形貌随着计量比2x值由低到高的演化规律为：由六棱柱→多面体→近球形→球形；建立了计量比与NbB_(2x)颗粒生长形貌的关系，即在燃烧温度或B/Nb摩尔比较低时，反应生成的NbB_(2x)计量比较低，对应NbB_(2x)颗粒的生长形貌为规则的六棱柱；而在燃烧温度和B/Nb摩尔比较高时，反应生成的NbB_(2x)的计量比较高，对应NbB_(2x)颗粒的生长形貌多为近球形和球形。揭示出SHS反应过程中，TiB_2、ZrB_2和NbB_(2x)颗粒的生长方式均为{0001}和{1010}面的二维层状生长。
4)揭示出计量比2x值是NbB_(2x)颗粒生长形貌演化的主要控制因素，首次提出NbB_(2x)的球形生长机制：当计量比较低时，{0001}和{1010}面非常稳定，NbB_(2x)颗粒生长为六棱柱状；随着计量比的升高，{0001}和{1010}面的稳定性逐渐下降，{1101}面逐渐显露，NbB_(2x)颗粒的生长形貌由六棱柱转变为多面体；当燃烧温度很高，且超过一定值后，{1101}面发生粗糙化转变，变为圆滑曲面，从而导致NbB_(2x)颗粒由多面体转变为近球形；随着计量比的进一步升高，{1101}曲面逐渐长大，NbB_(2x)颗粒变的越来越圆。
5)提出了在燃烧合成过程中，过渡金属陶瓷TMCs（TiC_x、NbC_x、ZrC_x、TaC_x）、TMNs（TiNx）、TMDs（TiB_2、ZrB_2、NbB_(2x)、TaC2x）颗粒生长形貌演化的个性与共性规律。
ⅰ)共性规律：
提出了SHS反应合成TMCs、TMNs、TMDs生长形貌发生演化的必要条件是其计量比区间要宽；建立了SHS反应合成TMCs、TMNs、TMDs的计量比与生长形貌演化的关系；同时，揭示了燃烧温度对生长形貌球化动力学的影响规律，即随着化学计量比和燃烧温度由低到高，TMCs、TMNs、TMDs生长形貌的变化规律为：TMCs、TMNs：八面体→切角八面体→近球形→球形；TMDs：六棱柱→多面体→近球形→球形。
ⅱ)个性规律：揭示出不具有较宽计量比区间的TiB_2和ZrB_2在燃烧合成过程中不存在生长形貌的演变过程。
6)揭示出使用碳纳米管（CNTs）作为碳源，能够明显增加Me (Cu/Al/Fe)–Ti–CNTs体系的反应活性，使传统的Cu/Al/Fe–Ti–C（石墨、碳黑）体系完全反应的最高金属含量由67.12wt.%Cu、46.65wt.%Al、77.4wt.%Fe提高到80wt.%Cu、70wt.%Al、80wt.%Fe；发现使用CNTs作为碳源，在高含量Me (Cu/Al/Fe)–Ti–CNTs体系，合成具有不同形状、纳米尺寸的TiC_x颗粒。
7)揭示出在Me (Cu/Al/Fe)–Ti–CNTs体系中，金属组元Me (Cu/Al/Fe)对TiC_x颗粒生长尺寸与形貌的影响规律与作用机制：在Fe–Ti–CNTs体系中，由于C在Fe熔体中溶解速度较快而扩散速度较慢，TiC_x颗粒在富[C]区域中快速形核、生长，因此，TiC_x具有较高的计量比，生长形貌多为立方体和近球状，且尺寸较大。反之，在Cu/Al–Ti–CNTs体系中，由于C在Cu/Al熔体中溶解速度较慢而扩散速度较快，TiC_x在十分贫[C]的环境下形核、生长，导致生成的TiC_x颗粒的计量比非常低，生长形貌多为八面体状，且尺寸较小。
总之，本文通过对不同体系燃烧合成过程中，过渡金属陶瓷颗粒的生长行为的研究，揭示了不同陶瓷结构、不同动力学条件对过渡金属陶瓷颗粒生长行为的影响规律；提出了不同类型陶瓷的生长机制及其共性与个性规律；为实现陶瓷颗粒形貌的主动控制，发展先进的陶瓷颗粒增强金属基复合材料奠定必需的理论基础。
Due to many excellent physical and chemical properties, such as high melting point,high hardness, high modulus, high thermal conductivity and high chemical stability,transition metal carbides and borides are widely used in mechanical, chemical andmicroelectronics applications. They are generally used as high–temperature ceramics,high–performance cutting and wear–resistant workpiece, especially reinforcing particles inthe cemented carbide or composite materials. As known, the morphology of the reinforcingceramic particles in the ceramic reinforced metal matrix composites has a critical impact ontheir properties. The matrix composites with round reinforcing particles have betterproperties than those with irregular shaped reinforcing particles. Therefore, it is of greatpractical significance to study the growth morphology, growth mechanism and thecontrolling factors for the ceramic particles. Moreover, the non–equilibrium growth kinetics(and mechanism) of the ceramics is also an important exploration and research direction inthe theoretical field of crystal growth. In fact, the combustion synthesis of ceramics is a hightemperature, fast, non–linear, non–steady–state transfer process, accompanied by numerouschemical and physical phenomena. Therefore, the factors influencing the growth behavior ofthe ceramics are very complicated. So far, there have been some work on the growthmorphology of the ceramic particles formed during combustion synthesis. However, thesework are mainly focused on the influencing regularity of the combustion kinetics on thegrowth morphology of the ceramic particles. The study on the underlying key theoreticalquestions during the fabrication of the ceramic–metal composites, especially the growthbehavior and mechanism of the ceramic particles, is rather limited.
Therefore, in this thesis, the growth behaviors of the ceramic particles (TiC_x, ZrC_x,NbC_x, TaC_x, TiB2, ZrB2, NbB2xand TaB2x) formed in the combustion systems ofAl–Ti/Zr/Nb/Ta–C/B were studied; the influencing regularity of the ceramic structures andthe kinetics conditions on the growth behavior of the ceramic particles were revealed; thegrowth mechanisms of different ceramic particles and their commonness and individuality were discussed.
The main results are as follows:
1) It was found that the Al content, carbon source and reactant C/Ti molar ratio haveimportant effects on the growth morphology of the TiC_xparticles formed in the Al–Ti–Csystem; The morphology evolution regularity of the TiC_xparticles with the increasingstoichiometry during the SHS was suggested as from octahedron→truncated–octahedron→sphere–like→sphere; The relationship between the growth morphology of the TiC_xand its stoichiometry was established, that is, in the case of quite low stoichiometry, theTiC_xparticles grow to octahedron, while in the case of relatively high stoichiometry, theTiC_xparticles grow to truncated–octahedron, and when the stoichiometry furtherincreases, the TiC_xparticles grow to sphere–like and sphere.
2) The growth mode of the TiC_xparticles during the SHS was suggested as thetwo–dimensional layer growth on the {111} surfaces. The main controlling factor of thegrowth morphology of the TiC_xparticles was suggested as the stoichiometry: When thestoichiometry of the formed TiC_xis very low, the {111} surfaces are quite stable, and theTiC_xparticles nucleate and grow as octahedron. With the increase in the stoichiometry,the {111} surfaces become less–stable, and the {100} surfaces begain to be exposed.Then, the shapes of the TiC_xparticles change from octahedron to truncated–octahedron.If the combustion temperature is higher than TR≈1800°C, the {100} surfaces undergoa roughening transition and become round, which makes the TiC_xbecome thespherical–like particles. With the further increase in the stoichiometry or combustiontemperature, the {100} surface grow up gradually, and the TiC_xparticles become moreand more round.
3) It was found firstly that necessary condition for the existence of the morphologyevolution and spherical growth shape for the transition metal diborides formed duringthe SHS in Al–Ti/Zr/Nb–B systems is there must exist a wide stoichiometric range. Forthe borides (TiB_2and ZrB_2) with no wide stoichiometric ranges, even the combustiontemperature becomes quite high, their shapes don’t change considerably and keep beingthe hexagonal–prisms, while for NbB_(2x)with a wide stoichiometric range, itsmorphology changes significantly with the Al content and the reactant B/Nb molar ratio;The morphology evolution regularity of the NbB_(2x)particles during the SHS with theincreasing stoichiometry was suggested as from hexagonal–prisms→polyhedron→sphere–like→sphere; The relationship between the growth morphology of the NbB_(2x)and its stoichiometry was established, that is, in the case of low stoichiometry, the NbB_(2x)particles grow to hexagonal–prisms, while in the case of high stoichiometry, the NbB_(2x)particles grow to sphere–like and sphere. The growth mode of the TiB_2, ZrB_2and NbB_(2x)particles during the SHS was suggested as the two–dimensional layer growth on the {0001}and {1010}surfaces.
4) The main controlling factor of the growth morphology of the NbB_(2x)particles wassuggested as the stoichiometry, and the spherical growth mechanism of the NbB_(2x)particles was firstly proposed: When the stoichiometry is low, the {0001}and {1010}surfaces are very stable, and the NbB_(2x)particles grow to the hexagonal–prisms. With theincrease in the stoichiometry, and stability of the {0001}and {1010}surfaces isgradually decreased; while the {1101}surfaces gradually emerge. Then, the NbB_(2x)particles change their shapes from hexagonal–prism to polyhedron. When thecombustion temperature is high and exceeds a certain value, the {1101}surfacescomposed with the side–facets of the growth steps are rourhed and become round,inducing the formation of the spherical–like NbB_(2x)particles. With the further increase inthe stoichiometry, the NbB_(2x)particles become more and more round.
5) The commonness and individuality of the morphology evolution of the transition metalcarbides (TiC_x, ZrC_x, NbC_xand TaC_x), nitrides (TiNx) and borides (TiB_2, ZrB_2, NbB_(2x)and TaC2x) during the SHS were summarized.
ⅰ) Commonness:The necessary condition for the morphology evolution of the TMCs, TMNs andTMDs particles during the SHS was suggested as the wide stoichiometric ranges; Therelationship between the growth morphology and their stoichiometry was establishedand the effect of the combustion temperature on the spherical kinetics of the growthmorphology was revealed, that is, with the increase in the combustion temperature andstoichiometry, the morphology of the TMCs and TMNs evolves from octahedron→truncated–octahedron→sphere–like→sphere, and that of the TMDs evolves fromhexagonal–prisms→polyhedron→sphere–like→sphere.
ⅱ) Individuality:For the borides (TiB_2and ZrB_2) with no wide stoichiometric ranges, there is nomorphology evolution for them during the SHS.
6) It was disclosed that the reactive activity of the Me (Cu/Al/Fe)–Ti–CNTs systems can begreatly increased with using CNTs as carbon source, and the higheat metal contents forthe complete raction during the SHS were increased from67.12wt.%Cu,46.65wt.%Aland77.4wt.%Fe to80wt.%Cu,70wt.%Al and80wt.%Fe, respectively; With usingthe CNTs as carbon source, the nano TiC_xparticles with different shapes can besynthesized in the Me (Cu/Al/Fe)–Ti–CNTs systems with high metal contents.
7) The influence regularity and affect mechanism of the metal component on the size andmorphology of the TiC_xparticles formed in the Me (Cu/Al/Fe)–Ti–CNTs systems weredisclosed: In the Fe–Ti–CNTs system, because of the fast dissolution rate but the low diffusion rate of carbon in Fe, the TiC_xparticles form in the [C]–rich regions and growrapidly to relatively larger sizes. Moreover, the stoichiometry of these formed TiC_xparticles in the Fe melt is relatively high and thus their growth shapes are cube andsphere–like. In the Cu–and Al–Ti–CNTs systems, the CNTs dissolve more slowlybecause of the poor chemical reactivity. In this case, the TiC_xforms and grows under acondition of [C] scarcity. Hence, the TiC_xparticles grown in these two melts are withrelatively small sizes, and the TiC_xstoichiometry formed at the combustion stage is low,and accordingly, the TiC_xgrowth shape is octahedron.
In summary, in this thesis, the growth behaviors of the ceramic particles (TiC_x, ZrC_x,NbC_x, TaC_x, TiB_2, ZrB_2, NbB_(2x)and TaB_(2x)) formed in the combustion systems ofAl–Ti/Zr/Nb/Ta–C/B were studied; the influencing regularity of the ceramic structures andthe kinetics conditions on the growth behavior of the ceramic particles was revealed; thegrowth mechanisms of different ceramic particles and their commonness and individualitywere suggested, which lays the necessary theoretical basis for the active control of theceramic particle morphology and the development of advanced ceramic particles reinforcedmetal matrix composites.
引文
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