球磨工艺对原位合成纳米级TiB的影响（英文）

球磨工艺对球磨粉末及其烧结组织的微观结构和形态都有重要的影响。本实验采用低能和高能球磨2种方式对Ti-7Al-0.2B(质量分数,%)合金粉末进行球磨,研究球磨过程中粉末组织和形态的变化,并将球磨后的粉末进行热压烧结,研究不同球磨方式对烧结组织中原位合成TiB增强相形态的影响。研究结果表明:低能球磨过程中,粉末颗粒间有机械合金化发生,其烧结组织中生成的TiB为细长态,在基体中分布均匀,没有联结的粗晶或成簇生长现象。对于高能球磨,粉末颗粒细化效果明显,颗粒平均尺寸降至1μm,球磨过程中除了机械合金化还形成了Ti(Al)过饱和固溶体,并在球磨后期形成了非晶结构。经高能球磨的粉末烧结后,组织中生成了均匀分布的纳米级TiB晶须。     

球磨工艺对原位合成纳米级TiB的影响

球磨工艺对球磨粉末及其烧结组织的微观结构和形态都有重要的影响。本实验采用低能和高能球磨两种方式对Ti-Al-0.2B wt.%合金粉末进行球磨,研究球磨过程中粉末组织和形态的变化,并将球磨后的粉末进行热压烧结,研究不同球磨方式对烧结组织中原位合成TiB增强相形态的影响。研究结果表明：低能球磨过程中粉末颗粒间有机械合金化发生,其烧结组织中生成的TiB为细长态,在基体中分布均匀,没有联结的粗晶或成簇生长现象。对于高能球磨,粉末颗粒细化效果明显,颗粒平均尺寸降至1 μm,球磨过程中除了机械合金化还形成了Ti(Al)过饱和固溶体,并在球磨后期形成了非晶结构。经高能球磨的粉末烧结后,组织中生成了均匀分布的纳米级TiB晶须。     

高能球磨工艺对CNTs/Cu复合粉末与材料性能的影响

采用卧式高能球磨和机械合金化工艺制备了纳米碳管增强铜基(CNTs/Cu)复合粉体,并采用真空冷压烧结法制备出CNTs/Cu复合材料。研究了高能球磨工艺参数对复合粉体与材料性能的影响,包括球磨时间和搅拌轴转速对复合粉体粒度、松装密度的影响,及其对该复合材料力学性能的影响。结果表明,高能球磨技术有利于CNTs与铜的界面结合和机械合金化。高能球磨的最佳工艺条件为搅拌轴线速度为4.2/5.4 m/s和球磨时间为2~4h,得到的CNTs/Cu复合粉体中位径11.76μm,松装密度1.356 g/cm3。CNTs/Cu复合材料的致密度达94%,硬度达92 HB,抗拉强度达138 MPa。     

高能球磨工艺对Cu-10Cr-0.5Al2O3组织与性能的影响

利用高能球磨方法对Cu-10Cr-0.5Al2O3(质量分数,%)混合粉末进行预处理,采用电场活化烧结技术对球磨粉末进行烧结,运用XRD、SEM、硬度、断裂强度和电导率等测试方法研究球磨时间对Cu-10Cr-0.5Al2O3复合粉末烧结前后组织和性能的影响.结果表明随着球磨时间的增加,Cu晶粒更加细化,第二相分布更加弥散,以致烧结材料的强度和硬度逐渐增大,球磨20h后,烧结样品的强度和硬度分别达到952MPa和285HV;由于晶粒细化、高度弥散的第二相以及铜相的晶格畸变加强对电子的散射作用,烧结试样的电导率也随球磨时间的延长而逐渐下降,球磨20h后,烧结样品的电导率下降到51%(IACS).     

Cu-Sn-Bi合金在球磨和烧结过程中的组织演变

采用机械合金化法制备出Cu-10%Sn-5%Bi合金粉末,然后将其压制成型并进行烧结,制备成合金块体;利用X射线衍射(XRD)和扫描电镜(SEM)等分析手段,研究Cu-Sn-Bi合金在高能球磨和烧结过程中组织结构的变化。结果表明:高能球磨可以扩展Cu-Bi互不溶体系的固溶度,且在球磨过程中形成的Cu_6Sn_5相为亚稳定相,随着球磨时间延长会先形成而后发生分解,分解后的Sn将固溶到Cu中;同时在450 r/min球磨40 h后,Sn、Bi基本完全融入Cu中,形成Cu的过饱和固溶体。在烧结过程中,Bi从Cu中脱溶,细小弥散分布在Cu基体中。在700℃二次烧结后,Cu-Sn-Bi合金显微组织良好,具有相对较好的力学性能。     

球磨工艺对原位合成Al2O3/TiAl复合材料性能的影响

采用不同的球磨时间和球料比,实现了Ti、Al、TiO2和Nb2O5粉末的机械合金化,并以其为原料采用放电等离子烧结(SPS)技术制备了Al2O/TiAl复合材料.利用扫描电镜(SEM)和X射线衍射(XRD)等对球磨后粉末的形貌、大小、相组成以及其烧结后复合材料的组织进行了观察分析.结果 表明:球磨时间和球料比对粉体的形貌、尺寸和均匀度均存在影响,但延长球磨时间有利于粉体的机械合金化,而球料比对合金化程度影响较小.将球料比5∶1,球磨6h后的粉体在1000℃、40 MPa真空环境下烧结10 min,制备了Al2O3/TiAl复合材料,其显微组织主要由γ-TiAl、α2-Ti3Al、Al3Nb,以及分布在基体晶界处的Al2O3组成,压缩强度为1476 MPa,硬度为490 HV.     

高能球磨法制备Fe-C超细晶/纳米晶粉末的研究

采用高能球磨法制备出了平均颗粒尺寸为纳米级的超细Fe-C粉末。利用SEM、XRD等分析手段研究了球磨时间和转速对Fe-C超细晶/纳米晶粉末颗粒形貌、尺寸和合金化效果的影响。结果表明,Fe-C超细晶/纳米晶粉末的过程中,颗粒尺寸随球磨时间和转速的增加而得到有效细化。当球料比为20:1、转速350r/min、球磨70 h时,颗粒细化效果最好。将球磨后平均颗粒尺寸为纳米级的粉末进行SPS烧结,烧结温度700℃时,能实现烧结体完全致密,并可有效避免晶粒的长大,该烧结体材料抗压强度达2800MPa。     

机械合金化结合内氧化法制备Al2O3/Cu复合材料

Al2O3/Cu复合材料具有高的强度和高的导电性及优良的抗电弧性能,广泛应用于电子封装材料、电极和电触头材料。采用机械合金化制备亚稳态的Cu-Al-Cu2O合金粉末,经压制成型后,采用新型内氧化工艺进行烧结处理,得到高强度高导电的Cu/Al2O3复合材料。结果表明:机械球磨96h,Al原子已完全固溶于Cu的晶格中。经1183K内氧化处理4h试样组织均匀致密,Al2O3颗粒弥散分布在铜基体上,其硬度高,电导率高。     

原位反应合成TiN／Al2O3复合材料

以Al和TiO2为初始原料，经高能球磨及热压烧结工艺，原位合成了TiN／Al2O3复合材料。利用DTA，XRD及SEM等方法结合热力学计算，研究了该粉体的高能球磨过程和球磨粉体在后续热处理中的物相形成及转化规律。同时研究了以高能球磨及热压烧结工艺所制备的复合材料的力学性能和显微结构。结果表明：在球磨过程中粉料吸附并溶解了N2气，在后续热处理中原位反应形成了Ti2AlN相，当温度升高到一定程度时分解形成TiN，这有助于材料的致密化并使其力学性能提高。球磨粉体在1300℃、30MPa、保温、保压60min热压烧结条件下，可得到性能优异的TiN/Al2O3复合材料，该材料的抗弯强度为850MPa，断裂韧性为5．7MPa·m^1/2。     

电子封接用钼铜材料的制备

通过扫描电镜、透射电镜及X射线衍射等对Mo-Cu复合粉末的粉末形貌、合金化程度及烧结后合金组织结构进行分析,研究了高能球磨后Mo-Cu材料的显微组织及其与陶瓷热膨胀性能匹配的关系。结果表明,采用高能球磨机械合金化和氢气气氛烧结工艺制备的Mo-Cu复合材料,相对密度在98%以上,在室温至700℃热膨胀系数与陶瓷差值在8%。     

Relationship between powder characteristic and internal oxidation of Al in Cu-Al pre-alloyed powders

Since Cu-Al powder characteristics have important effects on the preparation of Cu/Al2O3 composite, the apparent activation energy of Al internal oxidation reac- tion in Cu-Al pre-alloyed powders with different characteristics was calculated in the present investigation. The microstructure and properties of the synthesized Cu/Al2O3 were studied. The results show that high-energy milling can obviously promote in- ternal oxidation of Al in Cu-Al powders in the same solid solubility. At the same milling condit...     

纳米晶W-La2O3电极材料的形成与烧结行为

通过高能球磨将一定成分的W，La2O3粉研磨成纳米粉，在真空热压炉中将其烧结为块体的纳米晶电极材料。利用X射线衍射仪(XRD)、透射电镜(TEM)和扫描电镜(SEM)等手段分析晶粒的变化情况。结果表明，烧结的致密化主要在于纳米颗粒的重排，而不是传统的扩散；烧结过程中出现晶粒长大现象，但长大有限；机械研磨产生的内应变、某些杂质元素的存在等对烧结有促进作用。     

稀土La对Al2O3/Cu复合材料组织与性能的影响

利用机械合金化法结合放电等离子烧结制备Al2O3/Cu铜基复合材料,采用XRD、SEM、硬度、抗拉强度和电导率等测试研究La含量对Al2O3/Cu复合粉末和烧结材料组织及性能的影响。结果表明:添加0.05%的稀土La有利于机械合金化过程中Cu晶粒的细化和Al2O3颗粒的弥散分布,从而提高烧结材料的显微硬度和抗拉强度。烧结材料的导电率随着La含量的增加先升后降,当La的质量分数为0.10%时,Al2O3/Cu复合材料的导电率提高11.3%IACS。     

干混合对硬质合金组织结构的影响

采用扫描电镜,通过对WC原料粉末、脱蜡压坯断口与表面、合金抗弯强度样品断口与合金烧结体表面微观形貌以及合金金相组织的观察,研究了干混合对硬质合金组织结构的影响。结果表明,干混合只对压坯成形过程中粉末颗粒的压制行为与烧结过程中合金的致密化行为产生影响,不会对烧结过程中的合金化行为产生影响。压坯中的大孔洞与未压好等压制缺陷以及显著的元素分布不均匀现象难以通过液相烧结得到有效消除,会继续保留至合金中。采用干混合工艺制备合金,合金晶粒均匀、粗大,接近原料粉末的电镜观测粒度。     

Relationship between powder characteristic and internal oxidation of AI in Cu-AI pre-alloyed powders

Since Cu-AI powder characteristics have important effects on the preparation of Cu/AI203 composite, the apparent activation energy of Al internal oxidation reac-tion in Cu-AI pre-alloyed powders with different characteristics was calculated in the present investigation. The microstructure and properties of the synthesized Cu/AI2O3were studied. The results show that high-energy milling can obviously promote in-ternal oxidation of AI in Cu-AI powders in the same solid solubility. At the same milling conditions and internal oxidation parameters, the solid solution of AI in Cu either in low or high amount will result in the poor microstructure and properties of the Cu/AI2O3 composite. Subsequently, when high-energy milling and internal oxidation are synchronously used to prepare the Cu/AI2O3 composite, there should be an appropriate solubility and milling effect for the pre-alloyed powders.     

Solid state and liquid phase sintering of mechanically activated W–20 wt.% Cu powder mixture

W–20 wt.% Cu powder mixture was mechanically alloyed by high-energy ball milling for various times and the effect of mechanical alloying (MA) on the sintering response of the composite compacts was investigated. The densification, microstructure, hardness and electrical conductivity after solid phase sintering (SPS) and liquid phase sintering (LPS) were examined. It was shown that the microstructure of mechanically alloyed powder profoundly influence the sintering response, i.e. a meaningful relationship between the sintering kinetics and the milling time was observed. It is suggested that MA disintegrates the W–W particle networks and increases the contribution of solid phase sintering (SPS) of nanostructured Cu and W particles on the densification. Higher hardness and conductivity were achieved by prolonged MA and SPS, indicating a lower W–W contiguity of the milled powders compared with the conventionally prepared W–Cu composite. On the other hand, depression of the melting temperature of copper up to 145 °C was noticed by affording a prolonged MA. The lower melting temperature and finer distribution of the Cu particles in the W matrix enhanced the densification during LPS and improved the homogeneity and properties of the final product.     

ZrB2-Al2O3复合粉体的制备及应用综述

以ZrO2（或ZrOCl2·8H2O）、B2O3（或H3BO3）和工业Al粉为原料,在氩（氮）气气氛中合成了ZrB2-Al2O3复合粉体,较佳的摩尔配比为ZrO2（ZrOCl2·8H2O）：H3BO3：Al=3：6：20。自蔓延高温合成法、微波法以及高能球磨法合成的复合粉体晶粒细小,具有良好的成型性和烧结性。ZrB2-Al2O3复合粉体可用来制备高性能陶瓷以及作为含碳耐火材料的添加剂来提高材料的抗氧化性和抗侵蚀性,此复合粉体在磨料磨具工业也有广阔的应用前景。     

Cu-15wt%Cr复合粉末机械合金化及稀土掺杂研究

以Cu、Cr和稀土粉末为原料,采用机械合金化法制备Cu-15wt%Cr和Cu-15wt%Cr-RE复合粉末.利用X射线衍射仪、扫描电镜研究了球磨过程粉末的显微组织结构,测量不同球磨时间粉末的显微硬度.结果表明:随着球磨时间的延长,Cr在Cu中的固溶度显著提高,晶粒不断细化和微应变增加,导致粉末微观硬度的提高.在球磨过程中添加一定量的稀土可以促进机械合金化效果.     

Microstructure and properties of copper composite containing in situ NbC reinforcement: Effects of milling speed

This paper presents a study on the effects of milling speed on the properties of in situ copper-based composite produced by mechanical alloying followed by cold pressing and sintering. A powdered mixture of copper, niobium and graphite with the composition of Cu–30%NbC was milled at various speeds (100, 200, 300 and 400 rpm). The NbC phase started to precipitate in the as-milled powder after 30 h milling at 400 rpm and the formation was completed after sintering at 950 °C. Enhancements of NbC phase formation with a reduction in Cu crystallite size were observed with the increase of milling speed. Density, hardness and electrical conductivity of the sintered composite were evaluated. An increase in milling speed resulted in an increase in sintered density and hardness but a reduction of electrical conductivity. The changes in the properties were correlated to the formation of NbC phase and refinement of copper and niobium carbide crystallite size since higher milling speed is associated with higher kinetic energy per hit.