Mg对原位自生TiB2/Al-4.5Cu复合材料微观组织及力学性能的影响

采用Al-K₂TiF₆-KBF₄混合盐原位自生反应法,制备了不同Mg质量分数的3wt% TiB₂/Al-4.5Cu复合材料。采用SEM、TEM、HM硬度测试和室温拉伸等方法研究了Mg含量和多级热处理对3wt% TiB₂/Al-4.5Cu复合材料微观组织和力学性能的影响。微观组织观察发现:Mg质量分数为3wt%时,经过多级热处理后,TiB₂颗粒的团聚现象明显改善,反应生成的TiB₂颗粒平均尺寸约为130 nm,基体内伴随有大量弥散分布的纳米级颗粒,且α-Al的晶粒尺寸也明显减小。力学测试结果表明:多级热处理后,3wt% TiB₂/Al-4.5Cu复合材料的硬度和抗拉强度随Mg含量的增加而提高,但过量的Mg (≥4wt%)会造成TiB₂颗粒细化效果下降。分析表明:Mg的加入能够降低TiB₂/α-Al界面能,减少脆性相Al₃Ti、Al₂B的生成,并通过反应生成的MgAl₂O₄使界面结构变成TiB₂/MgAl₂O₄/α-Al,从而有效抑制了TiB₂的团聚,改善了TiB₂颗粒与Al液界面的润湿性,提高了形核率,进一步细化了α-Al晶粒尺寸。      

MgAl2O4:Mg荧光粉的合成及其发光性能

用超声辅助聚丙烯酰胺凝胶法合成了MgAl₂O₄:Mg荧光粉。在MgAl₂O₄体系中引入的Mg金属颗粒抑制了MgAl₂O₄相的形成,在900℃及以上的温度烧结MgAl₂O₄:Mg干凝胶粉末,镁颗粒氧化成MgO。Mg金属颗粒的引入使MgAl₂O₄:Mg荧光粉的形貌由细小的纳米颗粒变为方便面型;MgAl₂O₄:Mg荧光粉的颜色由在600℃烧结时的暗棕色变为在800℃烧结时的白色,在1000℃烧结时白色变暗。随着烧结温度的提高MgAl₂O₄:Mg荧光粉的能带先增大后略微减小。引入镁颗粒使荧光光谱中位于395和425 nm的两个荧光峰淬灭,在650、656和680 nm出现三个新的荧光发射峰,且随着烧结温度的提高发光强度减弱。金属颗粒的表面等离子体共振导致MgAl₂O₄主晶格荧光淬灭,缺陷能级使MgAl₂O₄:Mg荧光粉产生了新的荧光发射峰。     

Improvement of the tensile strength of Al18B4O33w/Al composite at elevated temperatures by change of interfacial state

In general, it is very difficult to obtain obviously reinforced effect in discontinuously reinforced aluminum matrix composites at the temperature above 400 °C. In the present study, we report an effective method to improve the high-temperature tensile strength of Al₁₈B₄O₃₃w/Al composite by change of interfacial state. The pure aluminum matrix composites reinforced by Al₁₈B₄O₃₃w with different ZnAl₂O₄ coating contents were fabricated by squeeze casting. The results indicate that ZnAl₂O₄ coating of the whiskers can effectively improve the high-temperature tensile strength of Al₁₈B₄O₃₃w/Al composite, although the tensile strength of the composite decreases with increasing the tensile temperature. On the basis of fractograph analysis, the fracture mechanism of the composites at elevated temperatures was investigated.     

超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料

以1Cr18Ni9Ti、Ti-6Al-4V为金属基底,通过在B4C+Ti体系中引入CrO_3+Al铝热剂,调整反应体系绝热温度依次为3 193、3 282、3 290及3 473K,采用超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料,发现随着反应绝热温度升高,陶瓷/金属界面区厚度不仅因金属熔深增加而增大,并且残存于界面上的Al_2O_3夹杂也随之增多。分别对B4C+Al体系与CrO_3+Al铝热剂进行配制、球磨活化、压制成坯并依次填料入坩埚后,发现残存于界面上的Al_2O_3夹杂完全消除,同时发现在TiB_2-TiC/1Cr18Ni9Ti界面上生成三维网络陶瓷/金属梯度复合结构,而在TiB_2-TiC/Ti-6Al-4V界面上形成跨尺度多层次梯度复合结构。     

Formation of Mg–Al–Ti/MgO composite via reduction of TiO2

This paper investigates the possibility of reduction of TiO₂ through the mechanical alloying of Mg and TiO₂ powders. Elemental Mg and Al powders were first mixed with TiO₂ according to the nominal composition of Mg5wt.%–Al17.15wt.%–TiO₂. The powder mixture was mechanically milled in a planetary ball mill for different durations. Two types of DSC curves have been observed. The unmilled powders showed no reaction when heated to about 500 °C, while an exothermic reaction in the mechanically milled powders was observed at about 390 °C. Further investigation of the heat treatment of the mechanically milled powders showed the complete disappearance of TiO₂ and the formation of MgAl₂O₄ after annealing at 400 °C, implying that reduction of TiO₂ has occurred via the mechanical activation and annealing processes.     

原位自生纳米Al2O3/Al-Zn-Cu复合材料的力学性能

将纳米ZnO粉末和Al粉球磨后冷压成Al-ZnO预制块,然后将其加到Al-Zn-Cu熔体中进行Al-ZnO原位反应,制备出纳米Al₂O₃颗粒增强Al-Zn-Cu基复合材料。能谱面扫描分析和透射电镜观察结果表明,复合材料由纳米Al₂O₃颗粒和Al₂Cu析出相两种颗粒/析出相组成。纳米Al₂O₃颗粒通过异质形核和晶界钉扎,细化了Al-Zn-Cu合金晶粒组织和Al₂Cu析出相。原位纳米Al₂O₃颗粒的生成提高了基体合金的拉伸性能,轧制+热处理使Al₂O₃/Al-Zn-Cu复合材料的拉伸强度比相同处理的基体合金提高约100%,总伸长率提高约98%。     

Effect of volume fraction of carbon fibers on wear behavior of Al/Al2O3/C hybrid metal matrix composites

Wear behavior of Al/Al₂O₃/C hybrid metal matrix composites fabricated by squeeze casting method was characterized. The effects of volume fraction of carbon fiber on wear behavior of hybrid composites was investigated. Wear behavior of Al/Al₂O₃/C composites was characterized by the dry spindle wear test under various sliding speeds.

The wear resistance of Al/Al₂O₃/C composites was remarkably improved over Al/Al₂O₃ composites by adding carbon fibers to Al/Al₂O₃/C composites. Specifically, at the intermediate sliding speed the wear resistance of Al/Al₂O₃/C composites containing 8 vol.% carbon fiber was found to be better than that of the rest of the carbon hybrid composites. From fractographic studies, damaged sections in wear surfaces of hybrid composites at intermediate sliding speed were not observed due to the formation of solid lubrication film. The solid lubrication film which was formed as a result of adding carbon fibers improved the wear resistance of carbon hybrid composites because this film reduced the high friction force between MMCs and counter material.     

Bi2O3助熔剂对CaO-B2O3-SiO2/Al2O3玻璃陶瓷复合材料性能的影响

以CaO-B₂O₃-SiO₂(CBS)玻璃粉体和Al₂O₃陶瓷粉体为原料,通过在CBS与Al₂O₃的质量比固定为50:50的玻璃-陶瓷复合材料中添加适量的Bi₂O₃作为烧结助熔剂,探讨了Bi₂O₃助熔剂对CBS/Al₂O₃复合材料的烧结性能、介电性能、抗弯强度和热膨胀系数的影响规律.研究表明:Bi₂O₃助熔剂能通过降低CBS玻璃的转变温度和黏度促进CBS/Al₂O₃复合材料的致密化进程,于880 ℃下烧结即能获得结构较致密、气孔较少的CBS/Al₂O₃复合材料.然而,过量添加Bi₂O₃将使玻璃的黏度过低,从而恶化CBS/Al₂O₃复合材料的烧结性能、介电性能及抗弯强度.当Bi₂O₃的添加量为CBS/Al₂O₃复合材料的1.5wt%时,于880 ℃下烧结即能获得最为致密的CBS/Al₂O₃复合材料,密度为2.82 g·cm^-3,这一材料具有良好的介电性能(介电常数为7.21,介电损耗为1.06×10^-3),抗弯强度为190.34 MPa,0~300 ℃的热膨胀系数为3.52×10^-6 K^-1.     

片状纳米Al2O3/环氧树脂复合材料的制备及性能

采用水热法制备片状纳米Al₂O₃,经过偶联剂改性后与环氧树脂复合,通过溶液混合法制备了不同填充量的片状纳米Al₂O₃/环氧树脂复合材料,研究了片状纳米Al₂O₃用量对片状纳米Al₂O₃/环氧树脂复合材料介电性能和热性能的影响,利用SEM对复合材料的断口形貌进行了表征。结果表明: 片状纳米Al₂O₃在环氧树脂基体中分散良好;随着片状纳米Al₂O₃填充量的增加,复合材料的起始热分解温度升高、介电强度增大,当片状纳米Al₂O₃的填充量为7wt%时,复合材料的介电强度为 29.58 kV/mm,比纯环氧树脂的介电强度提高了30%;复合材料的介电常数(3.8~4.5)和介电损耗(0.015)比纯环氧树脂稍有增大,但仍维持在较好的介电性能范围内。     

Effects of TiO/Al ratio on microstructures and mechanical properties of TiAl base composites

Effects of TiO₂/Al ratio on the microstructures and mechanical properties of in situ Al₂O₃/TiAl based composites were investigated. The results indicate that the as-sintered products consist of grains of nearly lamellar ?₂ + ? structure with a dispersion of randomly oriented Al₂O₃ particles. A 43.9Ti-38.6Al-17.5TiO₂-nNb₂O₅ system was compared to 57.46Ti-36.78Al-5.76TiO₂-nNb₂O₅ system. The lamellar spacing of the products increases and the ?₂ phase volume decreases with decreasing TiO₂/Al ratio. For each system, as the volume of ?₂ phase increases, the average lamellar spacing decreases. Strength increases with an increasing TiO₂/Al ratio due to the amount of ?₂ phase. Al₂O₃ phase increases with increasing TiO₂/Al ratio. Toughness increases with decreasing TiO₂/Al ratio. When the Nb₂O₅ content is smaller than 6 wt.%, the lamellar spacing plays an important role in toughness than the Al₂O₃ content. When the Nb₂O₅ content is larger than 6 wt.%, the Al₂O₃ content exhibits significantly increases the values of toughness than lamellar spacing.     

Abrasive wear of Al2O3-reinforced aluminium-based MMCs

The effects of volume fraction, Al₂O₃ particle size and effects of porosity in the composites on the abrasive wear resistance of compo-casting Al alloy MMCs have been studied for different abrasive conditions. It was seen that porosity in the composites is proportional to particle content. In addition, process variables like the stirring speed, and the position and diameter of the stirrer affect of the porosity content in a way similar to that observed for particle content. In addition, the abrasive wear rates of composites decreased more rapidly with increase in Al₂O₃ volume fraction in tests performed over 80 grade SiC abrasive paper than in tests conducted over 220 grade SiC abrasive paper. Furthermore, the wear rates decreased with increase in Al₂O₃ size for the composites containing the same amount of Al₂O₃. Hence, it is deduced that aluminium alloy composites reinforced with larger Al₂O₃ particles are more effective against abrasive wear than those reinforced with smaller Al₂O₃ particles. At the same time the results show that the beneficial effects of hard Al₂O₃ particles on wear resistance far surpassed that of the sintered porosity in the compocasting metal-matrix composites (MMCs). Nevertheless, the fabrication of composites containing soft particles such as graphite favors a reduction in the friction coefficient. For this reason graphite and copper were used in the matrix in different amounts to detect their effect on wear resistance. Finally, it was seen that wear rate of the composites decreased considerably with graphite additions.     

Photoelectric currents in thin Al2O3 films

The photoconductivity in the 1–6 eV energy range was measured for Al₂O₃ prepared in three different ways with Mg, Al and Au counterelectrodes. C-V curves were taken on Al---Al₂O₃---p-Si and Au---Al₂O₃---p-Si devices. The leakage currents of Na---Al₂O₃---Al sandwiches were measured. From these measurements the barrier at the metal-oxide conduction band was found to be 3.5 ± 0.2 eV for Al. The photoconductivity with a threshold of about 2 eV is shown not to be due to the emitting metal electrodes for all three metals used. This threshold is independent of the work function of the counterelectrode.     

Fe/Al2O3复合材料的制备和性能

用石墨埋烧方法制备Fe/Al₂O₃复合材料,对其力学性能和微观结构进行了分析。结果表明:Fe/Al₂O₃复合材料的弯曲强度与断裂韧性均随Al₂O₃含量的升高先升高后降低,当Al₂O₃含量（质量分数）为70%时,其弯曲强度与断裂韧性分别达到602.49 MPa和9.33 MPa·m¹/2,其硬度随Al₂O₃含量先降低后升高。在烧结过程中在Fe颗粒周围形成一种成分为FeO与FeAl₂O₄的壳体,在壳体与Fe颗粒之间存在微裂纹缺陷。壳体的形成和壳体与金属颗粒间的微裂纹钝化了外部应力,从而提高了复合材料的韧性。     

调控Al2O3晶型控制MgAl2O4:Mn4+荧光粉中Mn价态研究

Mn⁴⁺激活红光荧光粉是白光半导体发光二极管(wLEDs)领域当前研究热点之一。Mn⁴⁺离子²E→⁴A₂跃迁在铝酸盐中的最短发光波长是在MgAl₂O₄中实现的651 nm发光, 由于其结构中含有形成四面体或八面体配位的两种阳离子格位(Mg²⁺/Al³⁺), 易造成所掺杂锰元素存在多种价态(+2/+4/+3等)。本研究通过改变起始原料中Al₂O₃的晶型(γ/α比例)及退火处理来调控锰离子在MgAl₂O₄晶格中的占据格位, 对其主要存在价态实现调控。采用荧光光谱和紫外-可见-近红外漫反射光谱技术来表征所合成荧光粉中Mn离子的价态及其演变。研究发现, 高α/(α+γ)比铝源促进Mn²⁺形成, 而低α/(α+γ)比铝源促进Mn⁴⁺形成。通过使用高活性纳米γ-Al₂O₃为铝源, 有效抑制了锰离子在MgAl₂O₄中Mg²⁺格位的占据及Mn²⁺离子的形成, 经空气中1550 ℃保温5 h的一次高温热处理即可制备出在可见光区只有Mn⁴⁺红光发光的高纯高亮度MgAl₂O₄:Mn⁴⁺荧光粉。氧化铝晶型影响锰离子掺杂格位和掺杂价态的本质规律是: 氧化铝活性决定实际固溶掺杂反应步骤, 进而影响锰离子掺杂格位和价态。本研究提出的反应步骤调控作为反应气氛、电荷补偿剂、反应温度三种调控方法外的一种新方法, 为Mn⁴⁺激活铝酸盐荧光粉中锰离子掺杂价态调控提供了新思路。     

球磨-转喷微注法制备纳米Al2O3颗粒/Al(7075)复合材料的组织及磨损特性

采用球磨-转喷微注相结合的新工艺制备纳米Al₂O₃颗粒(Al₂O_3p)/Al(7075)复合材料,设计一种转喷微注装置,该装置能将连续、微量的纳米Al₂O_3p注入到Al熔体中。观察纳米Al₂O₃增强相对Al(7075)基体合金材料微观组织的影响,并测试Al(7075)基体和纳米Al₂O_3p/Al(7075)复合材料的磨损特性。对纳米Al₂O_3p/Al(7075)复合材料和Al(7075)基体在不同载荷(15 N、25 N和35 N)下的磨损特性进行对比研究。结果表明:球磨-转喷微注法制备的纳米Al₂O_3p/Al(7075)复合材料晶粒较小,且增强相在基体中分布均匀且结合良好;随着载荷增大,纳米Al₂O_3p/Al(7075)复合材料磨损量的上升趋势慢于Al(7075)基体。载荷为35 N时,纳米Al₂O_3p/Al(7075)复合材料的磨损量较Al(7075)基体少,磨屑尺寸较小,其耐磨性能明显改善,这主要得益于纳米Al₂O_3p的支撑作用和材料的细晶强化作用。      

Improvements in mechanical properties of TiB2 ceramics tool materials by the dispersion of Al2O3 particles

TiB₂–Al₂O₃ composites with Ni–Mo as sintering aid have been fabricated by a hot-press technique at a lower temperature of 1530 °C for 1 h, and the mechanical properties and microstructure were investigated. The microstructure consists of dispersed Al₂O₃ particles in a fine-grained TiB₂ matrix. The addition of Al₂O₃ increases the fracture toughness up to 6.02 MPa m^1/2 at an amount of 40 vol.% Al₂O₃ and the flexural strength up to 913.86 MPa at an amount of 10 vol.% Al₂O₃. The improved flexural strength of the composites is a result of higher density than that of monolithic TiB₂. The increase of fracture toughness is a result of crack bridging by the metal grains on the boundaries, and crack deflection by weak grain boundaries due to the bad wetting characters between Ni–Mo and Al₂O₃.     

特高压气体绝缘金属封闭开关设备用Al2O3/环氧树脂复合材料的非等温固化动力学及蠕变性能

针对特高压气体绝缘金属封闭开关设备（GIS）用Al₂O₃/环氧树脂（EP）复合材料,采用非等温差示扫描量热（DSC）法研究了Al₂O₃/EP复合材料的固化行为,对其DSC曲线进行分峰处理,利用等转化率方法求得不同反应阶段的表观活化能。根据Málek判据得到Al₂O₃/EP复合材料的固化行为符合的模型类型,并求得不同反应阶段的各个动力学参数及固化动力学方程。利用SEM观察Al₂O₃/EP复合材料的微观形貌,通过动态热力学分析仪（DMA）分析其动态热力学性能和高温蠕变性能,利用时温等效预测了Al₂O₃/EP复合材料的长时蠕变行为。结果表明,DSC热流曲线表现为双峰分布;Al₂O₃/EP复合材料的两个反应阶段的表观活化能分别为35.3 kJ/mol及48.1 kJ/mol,Sestak-Berggren自催化模型能够很好地描述Al₂O₃/EP复合材料体系在不同固化阶段的固化行为。Al₂O₃颗粒均匀分散于树脂基体中,填料的加入使裂纹发生偏转。Al₂O₃/EP复合材料的储能模量（E'）随温度的升高而降低,损耗因子（tanδ）峰值对应的玻璃化转变温度（T_g）为120.03℃。Al₂O₃/EP复合材料的抗蠕变性能随着拉伸应力和温度的增加而减弱,随着时间的延长,其蠕变速率减小。      

Al2O3基多孔隔热材料表面Al2O3/MoSi2涂层的制备及其性能

采用刷涂法在Al₂O₃基多孔隔热材料表面制备Al₂O₃/MoSi₂涂层,涂层以硅溶胶作为粘结剂,纳米Al₂O₃与Al₂O₃纤维作为耐高温组分,MoSi₂为高发射率组分。通过SEM、XRD对Al₂O₃/MoSi₂涂层微观表面结构、物相组成进行分析。研究纳米Al₂O₃与Al₂O₃纤维的质量比和MoSi₂含量对Al₂O₃/MoSi₂涂层耐温性能的影响,并对Al₂O₃/MoSi₂涂层的抗热震性能、发射率进行表征。结果表明,当纳米Al₂O₃与Al₂O₃纤维的质量比小于1∶1时,热考核后Al₂O₃/MoSi₂涂层表面无裂纹产生;当纳米Al₂O₃与Al₂O₃纤维的质量比在1∶2~1∶4之间时,Al₂O₃/MoSi₂涂层中的纤维网络较完整。MoSi₂的含量为20%时,Al₂O₃/MoSi₂涂层抗热震实验循环25次后表面保持完好,热考核后在2.5~25 μm波段的平均发射率在0.85左右,具有较高的发射率。      

Controllable formation of Er–Yb codoped Al2O3 films by the non-aqueous sol–gel method

1 mol%Er³⁺–10 mol%Yb³⁺ codoped Al₂O₃ thin films have been prepared on thermally oxidized SiO₂/Si(110) substrates by a dip-coating process in the non-aqueous sol–gel method from the hydrolysis of aluminum isopropoxide [Al(OC₃H₇)₃] under isopropanol environment. Addition of N,N-dimethylformamide (DMF) as a drying control chemical additive (DCCA) into the sol suppresses formation of the cracks in the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films when the rare-earth ion is doped with a high doping concentration. Homogeneous, smooth and crack-free Er³⁺–Yb³⁺ codoped Al₂O₃ thin films form at the conditions by a molar ratio of 1:1 for DMF:Al(OC₃H₇)₃. A strong photoluminescence spectrum with a broadband extending from 1.400 to 1.700 µm centered at 1.533 µm is obtained for the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films, which is unrelated to the addition of DMF. Controllable formation of the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films may be explained by the fact that the DMF assisted the deprotonation process of Al–OH at the surfaces of gel particles, resulting in enhancement of the degree of polymerization of sols and improvement of the mechanical properties of gel thin films.     

原位气相生长法制备碳纳米管/Al2O3陶瓷复合材料

以Al₂O₃陶瓷成型体为基体,通过化学气相反应在陶瓷体内原位生长碳纳米管（CNTs）,制备出CNTs/Al₂O₃陶瓷复合材料。结果表明,Al₂O₃陶瓷体中均匀分布有可观量的多壁CNTs,碳管根部嵌于Al₂O₃晶粒间并从晶粒表面生长出。在Al₂O₃陶瓷成型体中原位生长CNTs需严格控制生长条件,尤其是生长温度（850℃）,温度过高和过低都难以长出CNTs,此外造孔剂、碳源和催化剂也影响CNTs的原位生长。对原位生长的CNTs/Al₂O₃复合体进一步高温烧结获得致密化的复合材料,其导电率达3.7 S/m,较纯Al₂O₃提高13个数量级。在陶瓷成型体中原位生长CNTs是一步法制备CNTs/陶瓷复合材料的新方法,可用于发展高性能的结构陶瓷和具有导电导热等多功能特性的新型陶瓷复合材料。