Ti_3AlC_2可加工导电陶瓷及其铜基复合材料的研制
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摘要
本文以Ti、Al、C元素粉末为原料,详细阐述了采用机械合金化法制备三元层状可加工陶瓷Ti_3AlC_2;同时,采用热处理工艺对机械合金化后混合粉体进行提纯以获得高纯Ti_3AlC_2粉体,为Ti_3AlC_2粉体材料的制备提供了新的技术途径。另外,采用机械合金化结合放电等离子烧结技术制备Ti_3AlC_2块体,解决了Ti_3AlC_2块体制备的关键科学问题即烧结温度较高或保温时间较长等。利用合成的高纯Ti_3AlC_2粉体与Cu制备出具有优异性能的Cu/Ti_3AlC_2金属陶瓷复合材料,并研究了其磨损行为。
通过系统地研究机械合金化参数、原料配比和掺杂Si对合成Ti_3AlC_2的影响,优化并给出了机械合金化法制备Ti_3AlC_2的最佳工艺参数,合成混合粉体中Ti_3AlC_2的含量最高可达95.1wt.%。球磨粉体的热处理研究结果表明,对不同球磨参数下获得的不同Ti_3AlC_2含量的球磨混合粉体在热处理温度为1000℃,保温时间为10min均可合成纯度>99wt.%的高纯Ti_3AlC_2粉体;适当延长球磨时间对随后热处理得到高纯的Ti_3AlC_2粉体几乎没有影响,但球磨时间过长,反而不利于合成高纯的Ti_3AlC_2粉体。此外,采用机械活化放电等离子烧结技术可以在低温合成高纯、甚至单相的Ti_3AlC_2或Ti3Al(Si)C2固溶体块体。放电等离子烧结制备Cu/Ti_3AlC_2复合材料发现,在较低的烧结温度,Ti_3AlC_2与Cu便发生微弱的反应,并且这种反应随保温时间的延长和烧结温度的升高,反应变得剧烈;反应主要是通过Ti_3AlC_2中的Al和Cu的相互扩散完成的,由于Cu的诱发作用,导致Ti_3AlC_2失去Al原子而分解为TiC,而Al扩散并固溶到Cu基体中形成Cu-Al合金,使复合材料具有高的强度。在磨损过程中,随Ti_3AlC_2含量的增加,Cu/Ti_3AlC_2复合材料的耐磨性明显增强。
Recently, Ti_3AlC_2 (titanium aluminum carbide) attracts increasing interest owing to its unique properties. It is a new structural/functional material, combining unusual properties of both metals and ceramics. Such as good electrical and thermal conductivity, high strength and modulus, high thermal shock, high-temperature oxidation resistance, low density, and being machainable with conventional high-speed tools without lubrication. In addition, in contrast to the normal brittle ceramics, Ti_3AlC_2 exhibits some abnormal room-temperature compressive plasticity. Due to above excellent properties, the applications of this material are very potential. For example, it can be used as a high-temperature structural material, and also to process abrasion-resistant components and rotating parts, and so on.
However, Ti_3AlC_2 has a very narrow zone of stability in Ti-Al-C ternary phase diagram, therefore, preparation of high purity Ti_3AlC_2 has been the difficulties of its research. Since 1994, a variety of sintering methods were used to synthesize Ti_3AlC_2. Such as hot isostatic pressing (HIP), hot-pressing (HP), self-propagating high temperature synthesis (SHS), spark plasma sintering (SPS). Though high-purity, even single-phase Ti_3AlC_2 were synthesized, higher synthesis temperatures, longer holding time were required in these methods.
In this paper, Ti, Al and C were selected as raw materials. Preparation of layered machinable ternary ceramics Ti_3AlC_2 by mechanical alloying is detailed for the first time; at the same time, the milled powders were heated treatment in order to obtain high-purity Ti_3AlC_2 powder. In addition, high-purity, even single-phase Ti_3AlC_2 bulks were synthesized by mechanical alloying and spark plasma sintering for the first time. The key scientific problems on preparation of Ti_3AlC_2 are solved, e.g. higher sintering temperature or longer holding time. High-purity Ti_3AlC_2 powder and Cu powder are used to synthesize Cu/ Ti_3AlC_2 metal-ceramic composites with excellent properties, and wear behavior is investigated. The major research efforts of the present study are as follows:
(1) Research on preparation of Ti_3AlC_2 powder by mechanical alloying
Effects of mechanical alloying parameters, raw material ratio and Si addition on preparation of Ti_3AlC_2 by mechanical alloying were investigated systematically. XRD, SEM, EDX and TEM are used to identity phase and observed microstructure. The study results show that high content Ti_3AlC_2 was successfully obtained after ball milling of powder mixture at 600 rpm, charge ratio of 5:1 only for 3 h. The milled products consist of powder and a coarse granule with 8 mm in diameter, and both are mainly composed of Ti_3AlC_2 with TiC as impurity. It is believed that a mechanically induced self-propagating reaction (MSR) was triggered to form Ti_3AlC_2 and TiC during mechanical alloying process. Through adjusting mechanical alloying parameters and raw material ratio, the best process is as follows: the rotation speed is set as 600 rpm, and the weight ratio of balls to powders is 5:1, milling time is 3.5h. The obtained Ti_3AlC_2 content is 92.2 wt.%. Adding a small amount of Si in the starting material remarkably improves the content of Ti_3AlC_2 in the final products. High-content Ti_3AlC_2 powders with a phase purity of 94.2 wt.% and 95.1 wt.%could be fabricated by mechanical alloying of 3Ti/Al/0.1Si/2C and 3Ti/Al/0.1Si/1.8C, respectively.
(2) Research on preparation of high-purity Ti_3AlC_2 powder by heating treatment the mechanically alloyed mixture
High-purity Ti_3AlC_2 powder (99 wt.%) is obtained by heating treatment the mechanically alloyed mixture. The best raw material ratio, heat treatment temperature and holding time is Ti:Al:C=3:1.1:1.8, 1000℃, 10 min, respectively. In addition, powder of lower content Ti_3AlC_2 was heated treatment in the same ball-milling process, high-purity Ti_3AlC_2 powder was also obtained. However, longer milling time doesn’t obtained high-purity Ti_3AlC_2 powder. When the milled powders with appropriate Si addition are heated treatment at 1000℃, high-purity Ti3Al(Si)C2 solid solution powder is synthesized. And Si atoms substitute for Al atoms in solid solution distribute unevenly.
(3) Preparation of Ti_3AlC_2 bulk by mechanically activated spark plasma sintering
3Ti/xAl/2C(x=1, 1.1, 1.2, 1.3) raw material powders were milled at 400 rpm for 9 h and 9.5 h, respectively. For mixed powders of milling for 9 h, no new phase was formed, it was called no-phase transformation group. For mixed powders of milling for 9.5 h, Ti_3AlC_2 and TiC were formed, it was called phase transformation group. The milled powders of both groups were selected to spark plasma sintered. And dual activation mechanism of low temperature synthesis of high purity, even single-phase Ti_3AlC_2 is explored the mechanical alloying and spark plasma sintering (MA-SPS).
For no-phase transformation group, high-purity and dense Ti_3AlC_2 was synthesized at lower sintering temperature by spark plasma sintering of mechanically milled elemental powders. It was found that elemental powders mechanically milled to superfine sizes and excess Al in the starting materials can obviously decrease sintering temperature for the synthesis of Ti_3AlC_2 during subsequent SPS. For mechanically milled mixtures of composition 3Ti/1.1Al/2C and 3Ti/1.2Al/2C in molar ratio, Ti_3AlC_2 with a purity of >99 wt.% and a relative density of >98% were obtained at 1100℃and 1050℃for 10 min, respectively. The reaction path for the formation of Ti_3AlC_2 is revealed as follows: Ti, Al and C mixtures induced chemical reactions to form TiC, Ti-Al intermetallics like Ti3Al and TiAl, and carbide Ti3AlC at low temperature of 600℃; the amorphous C further diffused in the Ti-Al intermetallics to form carbide Ti2AlC at elevated temperature; at last, the reactions between Ti2AlC and TiC yielded Ti_3AlC_2.
For phase transformation group, fully dense bulks Ti_3AlC_2 with > 99 wt.% phase purity were obtained at the relatively low temperature and appropriate holding times by subsequent spark plasma sintering of mechanically alloyed powders from a starting mixtures of composition Ti:Al:C = 3:1.1:2 in molar ratio. But with the increasing holding time, the typical layered grain sizes of Ti_3AlC_2 increased and the Vickers hardness decreased. In addition, single-phase Ti_3AlC_2 and Ti3Al(Si)C2 solid solution were obtained by sintering the milled 3Ti/(1.1-y)Al/ySi/1.8C(y=0, 0.1, 0.2, 0.3) powder at 1000℃for 10 min. With Si content increasing, the Vickers hardness increased.
(4) Preparation of Cu/Ti_3AlC_2 composites and wear behavior
High-purity Ti_3AlC_2 powder was selected to prepare Cu/Ti_3AlC_2 composites, and to study the wear behavior. Friction and wear properties and wear mechanism of Cu/Ti_3AlC_2 composites at different content Ti_3AlC_2 and test load. The results show that Ti_3AlC_2 and Cu occurred reaction at lower temperature. Moreover, this reaction became increasing serious with increasing sintering temperature. The reaction was mainly completed through diffusion of Al in Ti_3AlC_2 and Cu. As a result of the induced function of Cu, resulting in the loss of Al atoms in Ti_3AlC_2 decomposed into TiC. And Al diffused into Cu matrix to form Cu-Al alloy. During the wear process, Wear mechanism of copper is mainly plough wear and adhesive wear. With increasing Ti_3AlC_2 content, Cu/Ti_3AlC_2 composite wear rate and friction coefficient decreased, wear resistance was improved significantly. When volume fraction of Ti_3AlC_2 is lower (5-10vol.%), The wear mechanism is mainly adhesive wear, at the same time, accompanying by abrasive wear; With volume fraction of Ti_3AlC_2 further increasing (15-30vol.%), Furrows of the worn surface has become shallow and small, reducing the surface roughness. At the load of 100N, wear resistance of Cu/30vol.% Ti_3AlC_2 composites is the best.
In a word, the studies of this paper provide a new technical path and the process parameters as reference for preparation of Ti_3AlC_2 powder and bulk material. The work in this paper is of rather available values in theory and practical application.
通过系统地研究机械合金化参数、原料配比和掺杂Si对合成Ti_3AlC_2的影响,优化并给出了机械合金化法制备Ti_3AlC_2的最佳工艺参数,合成混合粉体中Ti_3AlC_2的含量最高可达95.1wt.%。球磨粉体的热处理研究结果表明,对不同球磨参数下获得的不同Ti_3AlC_2含量的球磨混合粉体在热处理温度为1000℃,保温时间为10min均可合成纯度>99wt.%的高纯Ti_3AlC_2粉体;适当延长球磨时间对随后热处理得到高纯的Ti_3AlC_2粉体几乎没有影响,但球磨时间过长,反而不利于合成高纯的Ti_3AlC_2粉体。此外,采用机械活化放电等离子烧结技术可以在低温合成高纯、甚至单相的Ti_3AlC_2或Ti3Al(Si)C2固溶体块体。放电等离子烧结制备Cu/Ti_3AlC_2复合材料发现,在较低的烧结温度,Ti_3AlC_2与Cu便发生微弱的反应,并且这种反应随保温时间的延长和烧结温度的升高,反应变得剧烈;反应主要是通过Ti_3AlC_2中的Al和Cu的相互扩散完成的,由于Cu的诱发作用,导致Ti_3AlC_2失去Al原子而分解为TiC,而Al扩散并固溶到Cu基体中形成Cu-Al合金,使复合材料具有高的强度。在磨损过程中,随Ti_3AlC_2含量的增加,Cu/Ti_3AlC_2复合材料的耐磨性明显增强。
Recently, Ti_3AlC_2 (titanium aluminum carbide) attracts increasing interest owing to its unique properties. It is a new structural/functional material, combining unusual properties of both metals and ceramics. Such as good electrical and thermal conductivity, high strength and modulus, high thermal shock, high-temperature oxidation resistance, low density, and being machainable with conventional high-speed tools without lubrication. In addition, in contrast to the normal brittle ceramics, Ti_3AlC_2 exhibits some abnormal room-temperature compressive plasticity. Due to above excellent properties, the applications of this material are very potential. For example, it can be used as a high-temperature structural material, and also to process abrasion-resistant components and rotating parts, and so on.
However, Ti_3AlC_2 has a very narrow zone of stability in Ti-Al-C ternary phase diagram, therefore, preparation of high purity Ti_3AlC_2 has been the difficulties of its research. Since 1994, a variety of sintering methods were used to synthesize Ti_3AlC_2. Such as hot isostatic pressing (HIP), hot-pressing (HP), self-propagating high temperature synthesis (SHS), spark plasma sintering (SPS). Though high-purity, even single-phase Ti_3AlC_2 were synthesized, higher synthesis temperatures, longer holding time were required in these methods.
In this paper, Ti, Al and C were selected as raw materials. Preparation of layered machinable ternary ceramics Ti_3AlC_2 by mechanical alloying is detailed for the first time; at the same time, the milled powders were heated treatment in order to obtain high-purity Ti_3AlC_2 powder. In addition, high-purity, even single-phase Ti_3AlC_2 bulks were synthesized by mechanical alloying and spark plasma sintering for the first time. The key scientific problems on preparation of Ti_3AlC_2 are solved, e.g. higher sintering temperature or longer holding time. High-purity Ti_3AlC_2 powder and Cu powder are used to synthesize Cu/ Ti_3AlC_2 metal-ceramic composites with excellent properties, and wear behavior is investigated. The major research efforts of the present study are as follows:
(1) Research on preparation of Ti_3AlC_2 powder by mechanical alloying
Effects of mechanical alloying parameters, raw material ratio and Si addition on preparation of Ti_3AlC_2 by mechanical alloying were investigated systematically. XRD, SEM, EDX and TEM are used to identity phase and observed microstructure. The study results show that high content Ti_3AlC_2 was successfully obtained after ball milling of powder mixture at 600 rpm, charge ratio of 5:1 only for 3 h. The milled products consist of powder and a coarse granule with 8 mm in diameter, and both are mainly composed of Ti_3AlC_2 with TiC as impurity. It is believed that a mechanically induced self-propagating reaction (MSR) was triggered to form Ti_3AlC_2 and TiC during mechanical alloying process. Through adjusting mechanical alloying parameters and raw material ratio, the best process is as follows: the rotation speed is set as 600 rpm, and the weight ratio of balls to powders is 5:1, milling time is 3.5h. The obtained Ti_3AlC_2 content is 92.2 wt.%. Adding a small amount of Si in the starting material remarkably improves the content of Ti_3AlC_2 in the final products. High-content Ti_3AlC_2 powders with a phase purity of 94.2 wt.% and 95.1 wt.%could be fabricated by mechanical alloying of 3Ti/Al/0.1Si/2C and 3Ti/Al/0.1Si/1.8C, respectively.
(2) Research on preparation of high-purity Ti_3AlC_2 powder by heating treatment the mechanically alloyed mixture
High-purity Ti_3AlC_2 powder (99 wt.%) is obtained by heating treatment the mechanically alloyed mixture. The best raw material ratio, heat treatment temperature and holding time is Ti:Al:C=3:1.1:1.8, 1000℃, 10 min, respectively. In addition, powder of lower content Ti_3AlC_2 was heated treatment in the same ball-milling process, high-purity Ti_3AlC_2 powder was also obtained. However, longer milling time doesn’t obtained high-purity Ti_3AlC_2 powder. When the milled powders with appropriate Si addition are heated treatment at 1000℃, high-purity Ti3Al(Si)C2 solid solution powder is synthesized. And Si atoms substitute for Al atoms in solid solution distribute unevenly.
(3) Preparation of Ti_3AlC_2 bulk by mechanically activated spark plasma sintering
3Ti/xAl/2C(x=1, 1.1, 1.2, 1.3) raw material powders were milled at 400 rpm for 9 h and 9.5 h, respectively. For mixed powders of milling for 9 h, no new phase was formed, it was called no-phase transformation group. For mixed powders of milling for 9.5 h, Ti_3AlC_2 and TiC were formed, it was called phase transformation group. The milled powders of both groups were selected to spark plasma sintered. And dual activation mechanism of low temperature synthesis of high purity, even single-phase Ti_3AlC_2 is explored the mechanical alloying and spark plasma sintering (MA-SPS).
For no-phase transformation group, high-purity and dense Ti_3AlC_2 was synthesized at lower sintering temperature by spark plasma sintering of mechanically milled elemental powders. It was found that elemental powders mechanically milled to superfine sizes and excess Al in the starting materials can obviously decrease sintering temperature for the synthesis of Ti_3AlC_2 during subsequent SPS. For mechanically milled mixtures of composition 3Ti/1.1Al/2C and 3Ti/1.2Al/2C in molar ratio, Ti_3AlC_2 with a purity of >99 wt.% and a relative density of >98% were obtained at 1100℃and 1050℃for 10 min, respectively. The reaction path for the formation of Ti_3AlC_2 is revealed as follows: Ti, Al and C mixtures induced chemical reactions to form TiC, Ti-Al intermetallics like Ti3Al and TiAl, and carbide Ti3AlC at low temperature of 600℃; the amorphous C further diffused in the Ti-Al intermetallics to form carbide Ti2AlC at elevated temperature; at last, the reactions between Ti2AlC and TiC yielded Ti_3AlC_2.
For phase transformation group, fully dense bulks Ti_3AlC_2 with > 99 wt.% phase purity were obtained at the relatively low temperature and appropriate holding times by subsequent spark plasma sintering of mechanically alloyed powders from a starting mixtures of composition Ti:Al:C = 3:1.1:2 in molar ratio. But with the increasing holding time, the typical layered grain sizes of Ti_3AlC_2 increased and the Vickers hardness decreased. In addition, single-phase Ti_3AlC_2 and Ti3Al(Si)C2 solid solution were obtained by sintering the milled 3Ti/(1.1-y)Al/ySi/1.8C(y=0, 0.1, 0.2, 0.3) powder at 1000℃for 10 min. With Si content increasing, the Vickers hardness increased.
(4) Preparation of Cu/Ti_3AlC_2 composites and wear behavior
High-purity Ti_3AlC_2 powder was selected to prepare Cu/Ti_3AlC_2 composites, and to study the wear behavior. Friction and wear properties and wear mechanism of Cu/Ti_3AlC_2 composites at different content Ti_3AlC_2 and test load. The results show that Ti_3AlC_2 and Cu occurred reaction at lower temperature. Moreover, this reaction became increasing serious with increasing sintering temperature. The reaction was mainly completed through diffusion of Al in Ti_3AlC_2 and Cu. As a result of the induced function of Cu, resulting in the loss of Al atoms in Ti_3AlC_2 decomposed into TiC. And Al diffused into Cu matrix to form Cu-Al alloy. During the wear process, Wear mechanism of copper is mainly plough wear and adhesive wear. With increasing Ti_3AlC_2 content, Cu/Ti_3AlC_2 composite wear rate and friction coefficient decreased, wear resistance was improved significantly. When volume fraction of Ti_3AlC_2 is lower (5-10vol.%), The wear mechanism is mainly adhesive wear, at the same time, accompanying by abrasive wear; With volume fraction of Ti_3AlC_2 further increasing (15-30vol.%), Furrows of the worn surface has become shallow and small, reducing the surface roughness. At the load of 100N, wear resistance of Cu/30vol.% Ti_3AlC_2 composites is the best.
In a word, the studies of this paper provide a new technical path and the process parameters as reference for preparation of Ti_3AlC_2 powder and bulk material. The work in this paper is of rather available values in theory and practical application.
引文
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