TiAl_3/Ti_3AlC_2/Al_2O_3复合材料制备及其耐铝液熔蚀—磨损性能研究
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摘要
在冶金、化工、航空航天及汽车等领域，高温腐蚀性环境当中承受动载的关键零部件往往因腐蚀-磨损的作用而失效，从而造成巨大的经济损失。当前，对于腐蚀-磨损的研究多集中于材料在腐蚀性气体、溶液或颗粒冲刷条件下的加速流失，而对于材料在高温金属熔体当中的熔蚀-磨损失效行为研究鲜有报道。
本文针对材料在腐蚀性极强的高温铝液当中的熔蚀-磨损失效现象，采用机械球磨+反应热压工艺制备出Ti_3AlC_2+Al_2O_3两相原位内生增强的TiAl_3基复合材料，并利用自行研制的高温熔蚀-磨损试验机对H13钢及TiAl_3/Ti_3AlC_2/Al_2O_3复合材料在750℃铝液当中的熔蚀-磨损行为进行了对比研究，同时，探讨了材料在高温铝液当中的熔蚀-磨损机理。主要研究结果和创新如下：
1.复合材料的原位合成机理：反应热压过程中当Al熔化以后，Al与TiO_2即迅速发生放热反应生成TiAl_3与中间产物TiO，随着温度升高Al_2O_3逐渐在TiAl_3晶界上析出，当到达高温段后TiAl_3与TiC反应逐渐生成Ti_3AlC_2。其总的反应式为：3TiO_2+11Al+2TiC→2TiAl_3+Ti_3AlC_2+2Al_2O_3反应热压过程中由于瞬间放热而产生部分液相，导致试样内部出现瞬时的颗粒重排及熔体浸渗，从而实现瞬间液相致密。球磨50h后的Al/TiO_2/TiC复合粉末经1250℃/50MPa保温10min烧结后可以得到组织均匀细小、致密的TiAl_3/Ti_3AlC_2/Al_2O_3复合材料。
2.复合材料中TiAl_3与Al_2O_3呈两相互贯通的空间网络状增强结构，同时Ti_3AlC_2相的引入极大地提升了复合材料的综合力学性能：室温三点弯曲强度、断裂韧性及压缩强度分别为658.9MPa、7.9MPa/m1/2和1742.0MPa，且在1000℃下的高温压缩强度为604.1MPa。Ti_3AlC_2+Al_2O_3协同增强的TiAl_3复合材料存在多种增韧机制：包括Ti_3AlC_2和Al_2O_3颗粒的剥离，Ti_3AlC_2相导致的裂纹偏转及桥接，以及Ti_3AlC_2颗粒的变形及层裂。
3.在700~900℃下循环氧化50h后，复合材料表面只生成Al_2O_3单层膜，而在1000℃下氧化时其表面氧化膜为Al_2O_3与金红石型TiO_2的混合物。尽管氧化膜并不致密，复合材料在700~1000℃温度区间内仍表现出优异的抗高温循环氧化性能。
4.铝液熔蚀-磨损行为研究表明：对“以生成界面金属间化合物为典型腐蚀特征”的典型耐磨材料如H13钢这一类材料，界面金属间化合物的生成速度、性质及其与基体界面的结合情况对其在铝液当中的熔蚀-磨损性能的影响很大。H13钢在铝液当中熔蚀-磨损的材料流失量远高于其单纯腐蚀与单纯磨损条件下材料流失量之和。在本文不同实验条件下，其熔蚀-磨损体积损失约为133~407mm3/h，熔蚀与磨损二者的交互作用率均不小于93.9%。
5.相对H13钢而言，TiAl_3/Ti_3AlC_2/Al_2O_3复合材料的耐铝液熔蚀-磨损性能提高了几十甚至上百倍，其在750℃铝液当中的熔蚀-磨损体积损失仅为0.84~7.53mm3/h。在低载荷或者低转速条件下，复合材料甚至表现出负的交互作用，其最大交互作用率约为47.5%。这一方面是由于复合材料在铝液当中腐蚀时不生成其它界面产物，而仅为极少量Ti元素的溶解；另一方面则是由于TiAl_3基体与Al_2O_3二者所形成的空间网络状结构改善了复合材料在铝液当中的耐磨损性能。
In the field of metallurgical, chemical, aerospace and automotive, corrosion-weardamage to the key components used in high temperature corrosive environment which underdynamic loading often results in tremendous economic losses. Many researches have focusedon the accelerated degradation of materials in corrosive gas, solution or particle erosionconditions. However, the corrosion-wear behavior of materials in high temperature metal melthas been rarely reported.
The aim of the present investigation is to mainly understand the corrosion-wear damagebehavior of materials in the highly corrosive molten aluminum. According to the target, anin-situ Ti_3AlC_2and Al_2O_3cooperatively reinforced TiAl_3composite was synthesized from amechanically milled powder mixture by using an in situ reaction/hot pressing method. Thecorrosion-wear behaviors of TiAl_3/Ti_3AlC_2/Al_2O_3composite and H13tool steel in a moltenaluminum at750oC were investigated using a self-developed high temperaturecorrosion-wear test apparatus. The corrosion-wear mechanisms of these two materials werecompared and discussed. The main results and innovation are as follows:
1. Based on the detailed analysis, the synthesis mechanism of TiAl_3/Ti_3AlC_2/Al_2O_3composite is proposed as follows: after the melting of Al, Al and TiO_2reacted immediately toform TiAl_3and the transitional phase TiO. Subsequently, Al_2O_3precipitated on the grainboundary of TiAl_3with the increasing of temperature. When reached the high temperaturesection, TiAl_3and TiC reacted to form Ti_3AlC_2. The total reaction is defined as:3TiO_2+11Al+2TiC→2TiAl_3+Ti_3AlC_2+2Al_2O_3Due to the large amount of heat released in a very short time by the exothermic reaction, thesample internally generated transient liquid phase, which leading to instantaneous particlerearrangement and melt infiltration and resulting in a transient liquid phase dense. A fullydense Ti_3AlC_2/Al_2O_3/TiAl_3composite with homogeneous and fine microstructure wasfabricated from50h-milled Al-TiO_2-TiC powder mixture at1250oC and50MPa for10min.
2. Due to the introduction of Ti_3AlC_2phase and the interpenetrating structure of TiAl_3matrix and Al_2O_3reinforcement, the composite achieved three-point bending strength,fracture toughness and compressive strength of~658.9MPa,~7.9MPa/m1/2and~1742.0MPa,respectively. And the high compressive strength could be maintained of604.1MPa even at1000oC. The toughening of composite are primarily attributed to pull-out of the Ti_3AlC_2andAl_2O_3particles, crack deflection and crack bridging by the Ti_3AlC_2phase and as well as the deformation and delamination of Ti_3AlC_2particles.
3. The investigation of50h cyclic oxidation behavior of composite at elevatedtemperature showed that the scales on composite are only Al_2O_3at700~900oC, while Al_2O_3and rutile TiO_2at1000oC. Though the oxidation scales are not dense, composite still exhibitsexcellent cyclic oxidation resistance in the temperature range of700~1000oC.
4. A typical feature of materials corroded in molten aluminum is to generatedintemetallic compound layer between the substrate and molten aluminum. H13tool steel is atypical representative of these materials, so the corrosion-wear behavior of H13tool steel isinvestigated detailed. The results show that the corrosion-wear resistance of materials isdepended on the formation rate and characterization of intermetallic compound layer, as wellas the combination between the substrate and intermetallic zone. The corrosion-wear lossesare much higher than the simple sum of materials losses under plain corrosion and plain wear.The corrosion-wear volume loss of H13tool steel is about133~407mm3/h, and the synergyratio of corrosion-wear is not less than93.9%under the explored condition.
5. Compared with H13tool steel, the corrosion-wear resistance of TiAl_3/Ti_3AlC_2/Al_2O_3composite has improved significantly. The corrosion-wear volume loss of composite is only0.84~7.53mm3/h, which is dozens or even hundreds times less than that of H13. Under thecondition of low load or low velocity, the composite even exhibits negative synergy, and thehighest synergy ratio of corrosion-wear is47.5%. This is partly due to no intermetalliccompound formed in the interface, but just a little Ti dissolved into the molten aluminumwhen the composite corroded in Al melt. On the other hand, the interpenetrating structure ofTiAl_3matrix and Al_2O_3reinforcement improve the wear resistance of composite in moltenaluminum.
本文针对材料在腐蚀性极强的高温铝液当中的熔蚀-磨损失效现象，采用机械球磨+反应热压工艺制备出Ti_3AlC_2+Al_2O_3两相原位内生增强的TiAl_3基复合材料，并利用自行研制的高温熔蚀-磨损试验机对H13钢及TiAl_3/Ti_3AlC_2/Al_2O_3复合材料在750℃铝液当中的熔蚀-磨损行为进行了对比研究，同时，探讨了材料在高温铝液当中的熔蚀-磨损机理。主要研究结果和创新如下：
1.复合材料的原位合成机理：反应热压过程中当Al熔化以后，Al与TiO_2即迅速发生放热反应生成TiAl_3与中间产物TiO，随着温度升高Al_2O_3逐渐在TiAl_3晶界上析出，当到达高温段后TiAl_3与TiC反应逐渐生成Ti_3AlC_2。其总的反应式为：3TiO_2+11Al+2TiC→2TiAl_3+Ti_3AlC_2+2Al_2O_3反应热压过程中由于瞬间放热而产生部分液相，导致试样内部出现瞬时的颗粒重排及熔体浸渗，从而实现瞬间液相致密。球磨50h后的Al/TiO_2/TiC复合粉末经1250℃/50MPa保温10min烧结后可以得到组织均匀细小、致密的TiAl_3/Ti_3AlC_2/Al_2O_3复合材料。
2.复合材料中TiAl_3与Al_2O_3呈两相互贯通的空间网络状增强结构，同时Ti_3AlC_2相的引入极大地提升了复合材料的综合力学性能：室温三点弯曲强度、断裂韧性及压缩强度分别为658.9MPa、7.9MPa/m1/2和1742.0MPa，且在1000℃下的高温压缩强度为604.1MPa。Ti_3AlC_2+Al_2O_3协同增强的TiAl_3复合材料存在多种增韧机制：包括Ti_3AlC_2和Al_2O_3颗粒的剥离，Ti_3AlC_2相导致的裂纹偏转及桥接，以及Ti_3AlC_2颗粒的变形及层裂。
3.在700~900℃下循环氧化50h后，复合材料表面只生成Al_2O_3单层膜，而在1000℃下氧化时其表面氧化膜为Al_2O_3与金红石型TiO_2的混合物。尽管氧化膜并不致密，复合材料在700~1000℃温度区间内仍表现出优异的抗高温循环氧化性能。
4.铝液熔蚀-磨损行为研究表明：对“以生成界面金属间化合物为典型腐蚀特征”的典型耐磨材料如H13钢这一类材料，界面金属间化合物的生成速度、性质及其与基体界面的结合情况对其在铝液当中的熔蚀-磨损性能的影响很大。H13钢在铝液当中熔蚀-磨损的材料流失量远高于其单纯腐蚀与单纯磨损条件下材料流失量之和。在本文不同实验条件下，其熔蚀-磨损体积损失约为133~407mm3/h，熔蚀与磨损二者的交互作用率均不小于93.9%。
5.相对H13钢而言，TiAl_3/Ti_3AlC_2/Al_2O_3复合材料的耐铝液熔蚀-磨损性能提高了几十甚至上百倍，其在750℃铝液当中的熔蚀-磨损体积损失仅为0.84~7.53mm3/h。在低载荷或者低转速条件下，复合材料甚至表现出负的交互作用，其最大交互作用率约为47.5%。这一方面是由于复合材料在铝液当中腐蚀时不生成其它界面产物，而仅为极少量Ti元素的溶解；另一方面则是由于TiAl_3基体与Al_2O_3二者所形成的空间网络状结构改善了复合材料在铝液当中的耐磨损性能。
In the field of metallurgical, chemical, aerospace and automotive, corrosion-weardamage to the key components used in high temperature corrosive environment which underdynamic loading often results in tremendous economic losses. Many researches have focusedon the accelerated degradation of materials in corrosive gas, solution or particle erosionconditions. However, the corrosion-wear behavior of materials in high temperature metal melthas been rarely reported.
The aim of the present investigation is to mainly understand the corrosion-wear damagebehavior of materials in the highly corrosive molten aluminum. According to the target, anin-situ Ti_3AlC_2and Al_2O_3cooperatively reinforced TiAl_3composite was synthesized from amechanically milled powder mixture by using an in situ reaction/hot pressing method. Thecorrosion-wear behaviors of TiAl_3/Ti_3AlC_2/Al_2O_3composite and H13tool steel in a moltenaluminum at750oC were investigated using a self-developed high temperaturecorrosion-wear test apparatus. The corrosion-wear mechanisms of these two materials werecompared and discussed. The main results and innovation are as follows:
1. Based on the detailed analysis, the synthesis mechanism of TiAl_3/Ti_3AlC_2/Al_2O_3composite is proposed as follows: after the melting of Al, Al and TiO_2reacted immediately toform TiAl_3and the transitional phase TiO. Subsequently, Al_2O_3precipitated on the grainboundary of TiAl_3with the increasing of temperature. When reached the high temperaturesection, TiAl_3and TiC reacted to form Ti_3AlC_2. The total reaction is defined as:3TiO_2+11Al+2TiC→2TiAl_3+Ti_3AlC_2+2Al_2O_3Due to the large amount of heat released in a very short time by the exothermic reaction, thesample internally generated transient liquid phase, which leading to instantaneous particlerearrangement and melt infiltration and resulting in a transient liquid phase dense. A fullydense Ti_3AlC_2/Al_2O_3/TiAl_3composite with homogeneous and fine microstructure wasfabricated from50h-milled Al-TiO_2-TiC powder mixture at1250oC and50MPa for10min.
2. Due to the introduction of Ti_3AlC_2phase and the interpenetrating structure of TiAl_3matrix and Al_2O_3reinforcement, the composite achieved three-point bending strength,fracture toughness and compressive strength of~658.9MPa,~7.9MPa/m1/2and~1742.0MPa,respectively. And the high compressive strength could be maintained of604.1MPa even at1000oC. The toughening of composite are primarily attributed to pull-out of the Ti_3AlC_2andAl_2O_3particles, crack deflection and crack bridging by the Ti_3AlC_2phase and as well as the deformation and delamination of Ti_3AlC_2particles.
3. The investigation of50h cyclic oxidation behavior of composite at elevatedtemperature showed that the scales on composite are only Al_2O_3at700~900oC, while Al_2O_3and rutile TiO_2at1000oC. Though the oxidation scales are not dense, composite still exhibitsexcellent cyclic oxidation resistance in the temperature range of700~1000oC.
4. A typical feature of materials corroded in molten aluminum is to generatedintemetallic compound layer between the substrate and molten aluminum. H13tool steel is atypical representative of these materials, so the corrosion-wear behavior of H13tool steel isinvestigated detailed. The results show that the corrosion-wear resistance of materials isdepended on the formation rate and characterization of intermetallic compound layer, as wellas the combination between the substrate and intermetallic zone. The corrosion-wear lossesare much higher than the simple sum of materials losses under plain corrosion and plain wear.The corrosion-wear volume loss of H13tool steel is about133~407mm3/h, and the synergyratio of corrosion-wear is not less than93.9%under the explored condition.
5. Compared with H13tool steel, the corrosion-wear resistance of TiAl_3/Ti_3AlC_2/Al_2O_3composite has improved significantly. The corrosion-wear volume loss of composite is only0.84~7.53mm3/h, which is dozens or even hundreds times less than that of H13. Under thecondition of low load or low velocity, the composite even exhibits negative synergy, and thehighest synergy ratio of corrosion-wear is47.5%. This is partly due to no intermetalliccompound formed in the interface, but just a little Ti dissolved into the molten aluminumwhen the composite corroded in Al melt. On the other hand, the interpenetrating structure ofTiAl_3matrix and Al_2O_3reinforcement improve the wear resistance of composite in moltenaluminum.
引文
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