硼酸镁晶须增强镁基复合材料界面及混杂行为研究
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摘要
镁基复合材料具有轻质高强高模等优点，在航空、航天、汽车及电子通讯等领域展现了广阔的应用前景。其中，晶须增强镁基复合材料，因其优越的力学性能而备受国内外研究者的关注。然而，晶须与基体的界面问题成为晶须增强镁基复合材料实际应用的关键瓶颈。论文以高性价比硼酸镁晶须为增强相，通过制备工艺及界面的优化设计，成功制备出硼酸镁晶须增强镁基复合材料，并对其微观结构、界面反应层的形成规律及机理和力学性能进行了系统的研究；揭示了MgO界面反应产物的组织形态对复合材料强化机制和断裂行为的影响规律；以此为基础，为进一步提升复合材料的综合性能，研究了碳化硼颗粒的混杂行为对复合材料微观组织和力学性能的影响规律，初步探讨了混杂复合材料的界面形成机制、强化机制及其断裂行为。
采用挤压铸造法，成功实现20vol.%硼酸镁晶须增强AZ91D镁基复合材料的制备。复合材料微观组织致密，硼酸镁晶须均匀地分布在镁合金基体中。复合材料的力学性能比基体合金有了明显提高，铸态试样的弯曲模量、弯曲强度和维氏硬度分别从42GPa、211MPa和56.5提高到50GPa、407MPa和120.7。
硼酸镁晶须表面无任何处理时，复合材料中晶须和基体合金界面洁净，未发生化学反应，具有良好的化学相容性。复合材料断口分析发现较多硼酸镁晶须出现脱粘的现象，说明硼酸镁晶须和基体的界面结合强度较低，不利于硼酸镁晶须充分发挥其增强效用。为了优化复合材料界面结构以提高力学性能，对硼酸镁晶须进行表面处理，制备三种具有不同微观形貌的膜层：Al(PO_3)_3膜层、ZnO膜层和TiO_2膜层。三种膜层硼酸镁晶须增强复合材料TEM界面微观结构分析表明，在复合材料的制备过程中三种膜层均与基体合金发生化学反应并形成具有不同微观结构的MgO界面反应层：涂覆Al(PO_3)_3膜层时，晶须/基体界面处MgO颗粒相对较为粗大，且随膜层厚度增加，MgO颗粒逐渐增大；涂覆ZnO膜层时，晶须/基体界面处呈现双层结构，即细小颗粒组成的MgO薄膜层上黏附着较粗大的MgO颗粒；涂覆TiO_2膜层时，晶须/基体界面处呈现织构化MgO组织。
Al(PO_3)_3、ZnO和TiO_2膜层硼酸镁晶须增强复合材料力学性能测试结果表明，MgO界面反应层厚度及其微观结构对复合材料的弯曲性能具有显著影响。其中，在Al(PO_3)_3膜层硼酸镁晶须增强复合材料中，弯曲强度随MgO界面反应层厚度的增加呈现先增加后减小的趋势，当MgO界面反应层的厚度约为25nm时，弯曲强度达到最高值467MPa，比无膜层处理时提高了15%。对比研究上述三种复合材料界面微观结构和力学性能可以发现：由ZnO膜层生成的细小MgO颗粒比Al(PO_3)_3膜层生成粗大MgO颗粒更能提高复合材料的弯曲性能，而由TiO_2膜层反应生成的织构化MgO能更进一步提高复合材料弯曲性能，其弯曲强度和弯曲模量达到568MPa和66GPa，分别比无膜层时提高了40%和32%。复合材料弯曲性能的提高主要归因于界面结合强度和载荷传递效率的提高。硼酸镁晶须增强复合材料中存在载荷传递强化、位错强化和细晶强化三种强化机制，它们使得复合材料具有较高的强度。并且随着复合材料界面结合强度的不断提高，载荷传递强化逐渐成为主要的强化机制。
为了进一步提升复合材料的综合性能，在采用Al(PO_3)_3膜层改善界面结合状态的基础上，提出了添加碳化硼颗粒混杂增强的新工艺。结果表明，碳化硼颗粒的混杂可以显著提高复合材料的力学性能。当碳化硼颗粒的混杂体积分数为4%时，复合材料的弯曲强度达到最高值593MPa，比具有相同界面结构的单一硼酸镁晶须增强复合材料提高了35%。
Magnesium matrix composites have exhibited the wide application prospect inaviation, aerospace, automobile and electrommunication fields ascribed to theiradvantages, such as low density, high specific strength and high specific modulus. Amongthem, whisker-reinforced magnesium matrix composites have been received intensiveinterests by the researchers at home and abroad due to their superior mechanical properties.However, interfacial problems between whisker and matrix have been the key bottleneckto the practical application of whisker-reinforced magnesium matrix composites. In thisstudy, the high cost-effective magnesium borate whisker (Mg2B2O5w) is used as thereinforcement. Magnesium matrix composite reinforced with Mg2B2O5w is successfullyfabricated by optimizing preparation technology and interfacial design. Themicrostructures, formation mechanism of the interfacial reaction layers, mechanicalproperties and strengthening mechanism of composites are studied systematically. Basedon these results, in order to further improve the mechanical properties of composites, thehybrid magnesium matrix composites reinforced with boron carbide particles (B4Cp) andMg2B2O5w are successfully prepared. The microstructures, mechanical properties andstrengthening mechanism of hybrid composites are explored.
AZ91D magnesium matrix composites reinforced with20vol.%Mg2B2O5w aresuccessfully prepared by the squeezing casting technology. The microstructure of the composite is dense, and Mg2B2O5w uniformly distributes in the matrix alloy. The additionof Mg2B2O5w can obviously improve the mechanical properties of the composite. Flexuralmodulus, flexural strength and micro-Vickes' hardness are improved from42GPa,211MPaand56.5to50GPa,407MPa and120.7, respectively.
The Mg2B2O5w/Mg interface is clean in the as-cast Mg2B2O5w/AZ91D compositesand is chemically stable at the casting temperature. Although, there is plenty of whiskersdebond in fracture surface of as-cast Mg2B2O5w/AZ91D composite. This observationindicates that the interfacial bonding strength between Mg2B2O5w and matrix is relativelylow. To further enhance the mechanical properties of composites, Al(PO_3)_3coating, ZnOcoating and TiO_2coating are formed on the surface of Mg2B2O5w by various surfacetreatment methods. The TEM analysis of interfacial microstructures in the threecomposites show that all these coatings react with the liquid matrix during the fabricationprocesses of composites. The MgO interfacial layers with different microstructures areformed including:
(a) for Al(PO_3)_3coating, MgO particles are relatively large and their size increaseswith the increase in coating thickness;
(b) for ZnO coating, there exist a thin bilayer structure which consists of fine MgOparticles and large MgO particles adhering to it;
(c) for TiO_2coating, the textured MgO interfacial layer is formed.
The mechanical properties results show the thickness and microstructures of the MgOinterfacial layers have significant influence on the flexural properties of composites. Withthe increase in Al(PO_3)_3coating thickness, the flexural strength ofMg2B2O5w/Al(PO_3)_3/AZ91D composite increases firstly and then decreases. When thethickness of the MgO interfacial layer in Mg2B2O5w/Al(PO_3)_3/AZ91D composite is about25nm, the flexural strength reaches the maximum467MPa, which is enhanced by15%compared with that of composite without any coating. The comparative study on interfacemicrostructures and mechanical properties of composites treated by three coatings show that: fine MgO particles introduced by ZnO coating can be much more effective toimprove the interfacial bonding strength and load transfer efficiency than large MgOparticles introduced by Al(PO_3)_3coating, and thus enhance the flexural properties ofcomposites. The textured MgO interfacial layer can most effectively increase the flexuralproperties of composites. The flexural strength and modulus are568MPa and66GPa,which are enhanced by40%and35%, respectively, compared with that of compositeswithout any coating. This is attributed to the increase in interfacial bonding strength andload transfer efficiency. Various strengthening mechanisms including load transferstrengthening, dislocation strengthening and fine-grain strengthening exist in magnesiummatrix composites reinforced with Mg2B2O5w. Load transfer is the main strengtheningmechanism when the interfacial bonding strength is relatively high.
To further enhance the overall performance of composites, on the basis of improvingthe interfacial microstructure, the B4Cp is added into Mg2B2O5w and the hybridcomposites are fabricated. The results show that the hybrid of B4Cp remarkably enhancesthe mechanical properties of the composites. The flexural strength reaches the maximum593MPa when the volume fraction of B4Cp is4%, which are improved by35%comparedwith single Mg2B2O5w-reinforced composite.
采用挤压铸造法，成功实现20vol.%硼酸镁晶须增强AZ91D镁基复合材料的制备。复合材料微观组织致密，硼酸镁晶须均匀地分布在镁合金基体中。复合材料的力学性能比基体合金有了明显提高，铸态试样的弯曲模量、弯曲强度和维氏硬度分别从42GPa、211MPa和56.5提高到50GPa、407MPa和120.7。
硼酸镁晶须表面无任何处理时，复合材料中晶须和基体合金界面洁净，未发生化学反应，具有良好的化学相容性。复合材料断口分析发现较多硼酸镁晶须出现脱粘的现象，说明硼酸镁晶须和基体的界面结合强度较低，不利于硼酸镁晶须充分发挥其增强效用。为了优化复合材料界面结构以提高力学性能，对硼酸镁晶须进行表面处理，制备三种具有不同微观形貌的膜层：Al(PO_3)_3膜层、ZnO膜层和TiO_2膜层。三种膜层硼酸镁晶须增强复合材料TEM界面微观结构分析表明，在复合材料的制备过程中三种膜层均与基体合金发生化学反应并形成具有不同微观结构的MgO界面反应层：涂覆Al(PO_3)_3膜层时，晶须/基体界面处MgO颗粒相对较为粗大，且随膜层厚度增加，MgO颗粒逐渐增大；涂覆ZnO膜层时，晶须/基体界面处呈现双层结构，即细小颗粒组成的MgO薄膜层上黏附着较粗大的MgO颗粒；涂覆TiO_2膜层时，晶须/基体界面处呈现织构化MgO组织。
Al(PO_3)_3、ZnO和TiO_2膜层硼酸镁晶须增强复合材料力学性能测试结果表明，MgO界面反应层厚度及其微观结构对复合材料的弯曲性能具有显著影响。其中，在Al(PO_3)_3膜层硼酸镁晶须增强复合材料中，弯曲强度随MgO界面反应层厚度的增加呈现先增加后减小的趋势，当MgO界面反应层的厚度约为25nm时，弯曲强度达到最高值467MPa，比无膜层处理时提高了15%。对比研究上述三种复合材料界面微观结构和力学性能可以发现：由ZnO膜层生成的细小MgO颗粒比Al(PO_3)_3膜层生成粗大MgO颗粒更能提高复合材料的弯曲性能，而由TiO_2膜层反应生成的织构化MgO能更进一步提高复合材料弯曲性能，其弯曲强度和弯曲模量达到568MPa和66GPa，分别比无膜层时提高了40%和32%。复合材料弯曲性能的提高主要归因于界面结合强度和载荷传递效率的提高。硼酸镁晶须增强复合材料中存在载荷传递强化、位错强化和细晶强化三种强化机制，它们使得复合材料具有较高的强度。并且随着复合材料界面结合强度的不断提高，载荷传递强化逐渐成为主要的强化机制。
为了进一步提升复合材料的综合性能，在采用Al(PO_3)_3膜层改善界面结合状态的基础上，提出了添加碳化硼颗粒混杂增强的新工艺。结果表明，碳化硼颗粒的混杂可以显著提高复合材料的力学性能。当碳化硼颗粒的混杂体积分数为4%时，复合材料的弯曲强度达到最高值593MPa，比具有相同界面结构的单一硼酸镁晶须增强复合材料提高了35%。
Magnesium matrix composites have exhibited the wide application prospect inaviation, aerospace, automobile and electrommunication fields ascribed to theiradvantages, such as low density, high specific strength and high specific modulus. Amongthem, whisker-reinforced magnesium matrix composites have been received intensiveinterests by the researchers at home and abroad due to their superior mechanical properties.However, interfacial problems between whisker and matrix have been the key bottleneckto the practical application of whisker-reinforced magnesium matrix composites. In thisstudy, the high cost-effective magnesium borate whisker (Mg2B2O5w) is used as thereinforcement. Magnesium matrix composite reinforced with Mg2B2O5w is successfullyfabricated by optimizing preparation technology and interfacial design. Themicrostructures, formation mechanism of the interfacial reaction layers, mechanicalproperties and strengthening mechanism of composites are studied systematically. Basedon these results, in order to further improve the mechanical properties of composites, thehybrid magnesium matrix composites reinforced with boron carbide particles (B4Cp) andMg2B2O5w are successfully prepared. The microstructures, mechanical properties andstrengthening mechanism of hybrid composites are explored.
AZ91D magnesium matrix composites reinforced with20vol.%Mg2B2O5w aresuccessfully prepared by the squeezing casting technology. The microstructure of the composite is dense, and Mg2B2O5w uniformly distributes in the matrix alloy. The additionof Mg2B2O5w can obviously improve the mechanical properties of the composite. Flexuralmodulus, flexural strength and micro-Vickes' hardness are improved from42GPa,211MPaand56.5to50GPa,407MPa and120.7, respectively.
The Mg2B2O5w/Mg interface is clean in the as-cast Mg2B2O5w/AZ91D compositesand is chemically stable at the casting temperature. Although, there is plenty of whiskersdebond in fracture surface of as-cast Mg2B2O5w/AZ91D composite. This observationindicates that the interfacial bonding strength between Mg2B2O5w and matrix is relativelylow. To further enhance the mechanical properties of composites, Al(PO_3)_3coating, ZnOcoating and TiO_2coating are formed on the surface of Mg2B2O5w by various surfacetreatment methods. The TEM analysis of interfacial microstructures in the threecomposites show that all these coatings react with the liquid matrix during the fabricationprocesses of composites. The MgO interfacial layers with different microstructures areformed including:
(a) for Al(PO_3)_3coating, MgO particles are relatively large and their size increaseswith the increase in coating thickness;
(b) for ZnO coating, there exist a thin bilayer structure which consists of fine MgOparticles and large MgO particles adhering to it;
(c) for TiO_2coating, the textured MgO interfacial layer is formed.
The mechanical properties results show the thickness and microstructures of the MgOinterfacial layers have significant influence on the flexural properties of composites. Withthe increase in Al(PO_3)_3coating thickness, the flexural strength ofMg2B2O5w/Al(PO_3)_3/AZ91D composite increases firstly and then decreases. When thethickness of the MgO interfacial layer in Mg2B2O5w/Al(PO_3)_3/AZ91D composite is about25nm, the flexural strength reaches the maximum467MPa, which is enhanced by15%compared with that of composite without any coating. The comparative study on interfacemicrostructures and mechanical properties of composites treated by three coatings show that: fine MgO particles introduced by ZnO coating can be much more effective toimprove the interfacial bonding strength and load transfer efficiency than large MgOparticles introduced by Al(PO_3)_3coating, and thus enhance the flexural properties ofcomposites. The textured MgO interfacial layer can most effectively increase the flexuralproperties of composites. The flexural strength and modulus are568MPa and66GPa,which are enhanced by40%and35%, respectively, compared with that of compositeswithout any coating. This is attributed to the increase in interfacial bonding strength andload transfer efficiency. Various strengthening mechanisms including load transferstrengthening, dislocation strengthening and fine-grain strengthening exist in magnesiummatrix composites reinforced with Mg2B2O5w. Load transfer is the main strengtheningmechanism when the interfacial bonding strength is relatively high.
To further enhance the overall performance of composites, on the basis of improvingthe interfacial microstructure, the B4Cp is added into Mg2B2O5w and the hybridcomposites are fabricated. The results show that the hybrid of B4Cp remarkably enhancesthe mechanical properties of the composites. The flexural strength reaches the maximum593MPa when the volume fraction of B4Cp is4%, which are improved by35%comparedwith single Mg2B2O5w-reinforced composite.
引文
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