ZrO2—30mol?O2陶瓷粉末的高能球磨过程

本文研究了ＺｒＯ２－３０ｍｏｌ％ＣｅＯ２陶瓷粉末的高能球磨过程，首先发现陶瓷材料在高能球磨过程中，有机械合金化（ＭＡ）发生。     

高能球磨制备TiB_2/TiC纳米复合粉体

研究了通过高能球磨制备ＴｉＢ２／ＴｉＣ纳米复合粉体的反应过程和机理,对粉体的显微结构进行了表征．实验结果表明,采用金属 Ｔｉ和 Ｂ４Ｃ为原料,在球磨过程中, ＴｉＣ先于 ＴｉＢ２形成．球磨５ｈ后Ｔｉ与Ｂ４Ｃ反应生成ＴｉＢ２和ＴｉＣ,在随后的长时间高能球磨过程中ＴｉＢ２和ＴｉＣ两相保持稳定．球磨 ３０ｈ后,直径约 ８ｎｍ的 ＴｉＣ纳米粒子分布在 １００～２００ ｎｍ的 ＴｉＢ２粒子中,形成均匀分布的纳米ＴｉＢ２／ＴｉＣ复合粉体．     

γ-Al2O3对CeO2-ZrO2固溶体形成能力的影响及其稳定性

运用XRD研究了γ-Al2O3与CeO2、ZrO2在高能球磨过程中和焙烧过程中的组织结构转变,重点研究了γ-Al2O3对CeO2-ZrO2体系固溶体形成能力的影响以及它们的稳定性问题。结果表明,CeO2和ZrO2在高能球磨过程中容易形成固溶体,但当γ-Al2O3跟CeO2、ZrO2一起加入进行高能球磨时,γ-Al2O3会在球磨过程中抑制CeO2和ZrO2之间的扩散,使其难于形成固溶体。同时,γ-Al2O3在球磨过程中也没有跟CeO2或ZrO2发生互溶。研究还发现,通过调整球磨顺序,先将CeO2与ZrO2球磨30h,再添加Al2O3并继续球磨30h,这样生成的复合球磨粉体由结构稳定的γ-Al2O3与CeO2-ZrO2固溶体组成。在该球磨产物中,γ-Al2O3对CeO2-ZrO2固溶体的热稳定性有一定的促进作用,CeO2-ZrO2固溶体反过来也稳定了γ-Al2O3的相结构,避免了γ-Al2O3在球磨过程中发生α相变以及因球磨而降低相变点的现象,明显提高了其热稳定性。     

高能球磨法制备纳米晶Zn铁氧体

用高能球磨法制备了纳米晶Ｚｎ铁氧体。通过样品的Ｍｏｅｓｓｂａｕｅｒ谱及ＸＲＤ谱的测定,研究了纳米晶的形成过程。结果表明：球磨的３ｈα－Ｆｅ２Ｏ３即与ＺｎＯ发生机械化学反应生成Ｚｎ铁氧体,这种反应是通过先形成α－Ｆｅ２Ｏ３－ＺｎＯ固溶体而进行的。制得的纳米晶铁氧体有一定的晶格畸变。     

机械化学反应法制备纳米晶TaC和TaSi2

采用ＸＲＤ，ＴＥＭ和ＳＥＭ研究了用机械化学反应法制备金属间化合物ＴａＣ和ＴａＳｉ２时的结构演变，结果表明：ＴａＣ和ＴａＳｉ２是通过互扩散由元素直接反应合成的，高能球磨引入的高密度缺陷和纳米界面大大促进了这一反应过程。     

表面诱导沉淀法制备Al2O3-ZrO2纳米复合粉体

采用表面诱导沉淀法,制备了Ａｌ２Ｏ３－ＺｒＯ２（１５ｖｏｌ％）纳米复合粉料,利用透射电子显微镜对其形貌进行了表征,结果表明：在ｐＨ＝５时,可以使ＺｒＯ２前驱体均匀地包裹在Ａｌ２Ｏ３颗粒表面,经过８００℃煅烧之后,Ａｌ２Ｏ３ｘ颗粒表面均匀地结合着粒径约为３０ｎｍ的ＺｒＯ２颗粒,ＺｒＯ２颗粒尺寸均匀,该粉体经过２４ｈ球磨和超声波处理之后,未发生ＺｒＯ２颗粒脱落现象,表明ＺｒＯ２颗粒与Ａｌ２Ｏ３颗粒表面     

表面诱导沉淀法制备Al2O3-ZrO2纳米复合粉体

采用表面诱导沉淀法,制备了Ａｌ_２Ｏ_３－ＺｒＯ_２（１５ｖｏｌ％）纳米复合粉料,利用透射电子显微镜对其形貌进行了表征．结果表明：在ｐＨ＝５时,可以使ＺｒＯ_２前驱体均匀地包裹在Ａｌ_２Ｏ_３颗粒表面,经过８００℃煅烧之后,Ａｌ_２Ｏ_３颗粒表面均匀地结合着粒径约为３０ｎｍ的ＺｒＯ_２颗粒,ＺｒＯ_２颗粒尺寸均匀．该粉体经过２４ｈ球磨和超声波处理之后,未发生ＺｒＯ_２颗粒脱落现象,表明ＺｒＯ_２颗粒与Ａｌ_２Ｏ_３颗粒表面结合紧密．     

ZrO2亚微粉的搅动球磨研究

用自制的实验室小型搅动球磨机对工业ＺｒＯ＿２粉进行了球磨参数的正交试验，同时进行了搅动球磨与振动球磨动力学的对比实验，得出了两者的动力学回归方程为：０．５５７－０．１６８１ｇｔ０．７６０－０．２２２１ｇｔ研究认为，在球磨诸参数中，影响粒度显著性按以下顺序递减：球磨时间→搅棒转速→球径→球料比。研究同时得出，尽管振动球磨已是一种高效强力球磨方法，其研磨效率远高于普通滚动球磨，但仍数倍、甚至数１０倍地低于搅动球磨。在给定参数下，搅动球磨ｌｈ即可获得～０．５μｍ的ＺｒＯ＿２粉，而用振动球磨却需１６ｈ。     

STUDY FOR MECHANICAL ALLOYING OF Fe─M BY MOSSBAUER SPECTROSCOPY

将Ｆｅ－Ｍ（Ｍ＝Ｃ５ＳｉＯ２Ａｌ２Ｏ３）混合物在Ａｒ中高能球磨５６ｇ后测量Ｍｏｓｂａｕｅｒ谱，结果表明，（Ｆｅ）２－（ＳｉＯ２）１仍为Ｆｅ和ＳｉＯ２的机械混合物：（Ｆｅ）６－（Ｃ）３已完全合金化，生成两种Ｆｅ３Ｃ；（Ｆｅ）２－（Ａｌ２Ｏ３）１则成为Ｆｅ（７３％），尖晶石型的ＦｅＡｌ２Ｏ４）２２％），ｑｑｎｔＦｅ的团聚族（５％）和Ａｌ２Ｏ３的混合物。     

球磨促进碳热还原反应合成氮化铝研究

研究了高能球磨氧化铝和细化和机械力化学作用及球磨对碳热还原反应合成氮化铝（ＡｌＮ）的影响。结果表明：经高能球磨细化后的氧化铝（Ａｌ２Ｏ３）,相对于原始粉末,反应生成的ＡｌＮ 较大提高,且随着球磨时间增加,ＡｌＮ生成量增大。用灰色关联分析方法比较了几种球磨效应对碳热还原反应的作用,发现粉末的晶粒尺雨与反应的关联度最大,表明球磨晶粒细化作用是球磨促进碳热还原反应的最主要原因。     

Mg2Ni纳米晶储氢材料的机械合金化制备工艺研究

利用机械合金化方法制备了Mg2Ni纳米晶粉末,根据不同球磨参数下样品的X射线衍射结果,分析了球磨过程中相组成、粉末晶粒度等的变化,研究了球磨时间、球磨转速、过程控制剂等工艺条件对粉末晶粒度、机械合金化程度的影响.结果表明:在较高的转速下进行循环变速运行并加入合适的过程控制剂可以使生成Mg2Ni的时间提前,完全合金化的过程缩短,得到的Mg2Ni晶粒度为10nm左右.对Mg2Ni纳米晶粉末进行了初步的贮氢性能研究,结果表明:机械合金化制备的样品在室温下即可吸氢,贮氢性能较之传统材料有较大改善.     

Synthesis of MoSi2 by Mechanical Alloying

The microstructure evolution of mechanical alloyed Mo-66.7%Si powder using the high-energy ball mill has been studied by X-ray diffraction and scanning electron microscopy. The results showed that MoSi2 can be synthesized by MA of Mo-66.7%Si powder mixtures. Cold welding behavior between Mo and Si powders plays an important role in the preparation of MoSi2 by the MA.     

含镁铝尖晶石的铝酸钙水泥的合成与流变特性

在1400℃和1500℃温度下合成了不同配比的铝酸钙水泥(CMA)。检测结果显示, 当温度升高时镁铝尖晶石的粒径由5 μm生长到15 μm。合成温度达到1400℃时, 镁铝尖晶石晶粒呈团簇状并分布在铝酸钙晶粒周围; 当合成温度升高至1500℃时, 镁铝尖晶石晶粒穿插在铝酸钙晶粒中。另外, 随着水泥中镁铝尖晶石含量的增加, 水泥的凝结时间延长, 同时粘度下降。相应的, 水泥储能模量和流动点的大小分别为0.15 MPa和4.44%。提高镁铝尖晶石相的含量或增大铝酸钙晶粒尺寸会减弱水泥水化时絮凝结构的强度。     

Fabrication of Mg2Si thermoelectric materials by mechanical alloying and spark-plasma sintering process

A mixture of pure Mg and Si powders with an atomic ratio 2:1 has been subjected to mechanical alloying (MA) at room temperature to prepare the Mg2Si thermoelectric material. Mg2Si intermetallic compound with a grain size of 50 nm can be obtained by MA of Mg66.7Si33.3 powders for 60 hours and subsequently annealed at 620 degrees C. Consolidation of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies up to 800-900 degrees C under 50 MPa. The shrinkage of consolidated samples during SPS was significant at about 250 degrees and 620 degrees C. X-ray diffraction data shows that the SPS compact from 60 h MA powders consolidated up to 800 degrees C consists of only nanocrystalline Mg2Si compound with a grain size of 100 nm.     

电场激活燃烧合成( TiB2)PNi/Ni3Al/ Ni功能梯度材料

采用电场激活压力辅助合成技术(FAPAS)制备了(TiB₂)_PNi/(TiB₂)_PNi₃Al/Ni₃Al/Ni梯度材料,主要研究电场激活燃烧合成过程中电场对材料合成及层界面扩散连接的作用。分析了梯度材料各层的界面微观组织及相组成和材料的硬度分布。结果表明,采用FAPAS 技术结合机械合金化工艺制备的(TiB₂)_PNi/(TiB₂)_PNi₃Al/Ni₃Al/Ni 功能梯度材料具有快速、简便和组织均匀密实的特点。梯度材料的陶瓷复合层、Ni₃Al层和Ni板的界面区产生成分的互扩散,形成了良好的冶金结合。从Ni板到陶瓷复合层的硬度呈梯度分布。     

Giant and Broadband Multiphoton Absorption Nonlinearities of a 2D Organometallic Perovskite Ferroelectric

Multiphoton absorption (MPA) has been utilized for important technological applications. High-order multiphoton harvesting (e.g., five-photon absorption, 5PA) exhibits unique properties that could benefit biophotonics. Within this field, perovskite oxide ferroelectrics (e.g., BaTiO₃) enable low-order optical nonlinearities of 2PA/3PA processes. However, it is challenging to obtain efficient, high-order 5PA effects. Herein, for the first time, giant and broadband MPA properties are presented in the 2D hybrid perovskite ferroelectric (IA)₂(MA)₂Pb₃Br₁₀ ( 1 ; IA = isoamylammonium and MA = methylammonium), where multiphoton-excited optical nonlinearities related to different MPA mechanisms over a broadband range of 550–2400 nm are observed. Strikingly, its 5PA absorption cross-section (σ₅) reaches up to 1.2 × 10⁻¹³² cm¹⁰ s⁴ photon⁻⁴ (at 2400 nm), almost 10 orders larger than some state-of-the-art organic molecules and a record-high value among all known ferroelectrics. This unprecedented 5PA effect results from the quantum-confined motif of inorganic trilayer sheets (wells) and organic cations (barriers) in 1 . Moreover, its large ferroelectric polarization of 5 µC cm⁻² could promote modulation of MPA effects under external electric fields. As far as it is known, this is the first report on giant, broadband high-order MPA properties in ferroelectrics, which provides potential, novel electric-ordered materials for next-generation biophotonic applications.     

Microstructures and metastable phases produced in cold sintered blocks by mechanical alloying of NiAl-TiB2

The microstructure of cold sintered blocks formed on the mechanical alloying (MA) of NiAl-TiB₂ have been investigated by means of transmission electron microscopy (TEM). The results reveal that the blocks consisted of -NiAl with a B2 ordered structure and TiB₂, Al₂O₃ particles in addition to other metastable phases. The distribution of the phases and good bonding between them suggest that a sintering process occurred in-situ at low temperature in the later stage of the MA. The observed high density of dislocations and strong reaction between these dislocations and ceramic particles can explain the good toughness and high microhardness of the block. Minor crystalline and amorphous metastable phases have been found. A cold-sintering mechanism to form the block based on the metastable phase distribution has been proposed.     

Formation of B2 intermetallic NiAl and FeAl by mechanical alloying

Nanostructud B2 intermetallic compounds NiAl and FeAl have been prepared by mechanical alloying (MA) the elemental powder mixtures and subsequent heating. The structural evolution during MA was monitored by in situ thermal analysis and X-ray diffraction (XRD). The final products were characterized by transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The results show that the nanocrystalline intermetallic compound NiAl, which is difficult to disorder by milling, was synthesized directly after an exothermic explosive reaction; whereas FeAl compound was formed after a thermal process of asmilled Fe(Al) solid solution obtained through interdiffusion during MA. The large heat of formation of NiAl compound is the main driving force for the exothermic explosive reaction, and the difference in diffusivity between NiAl system and FeAl system is suggested to be the main cause of the different behaviors of formation between NiAl and FeAl compounds by MA.     

Methylammonium cation deficient surface for enhanced binding stability at TiO<Subscript>2</Subscript>/CH<Subscript>3</Subscript>NH<Subscript>3</Subscript>PbI<Subscript>3</Subscript> interface

Heterojunction interfaces in perovskite solar cells play an important role in enhancing their photoelectric properties and stability.Till date,the precise lattice arrangement at TiO2/CH3NH3PbI3 heterojunction interfaces has not been investigated clearly.Here,we examined a TiO2/CH3NH3PbI3 interface and found that a heavy atomic layer exists in such interfaces,which is attributed to the vacancies of methylammonium (MA) cation groups.Further,first-principles calculation results suggested that an MA cation-deficient surface structure is beneficial for a strong heterogeneous binding between TiO2 and CH3NH3PbI3 to enhance the interface stability.Our research is helpful for further understanding the detailed interface atom arrangements and provides references for interfacial modification in perovskite solar cells.     

复合包覆SrAl_2O_4:Eu~(2+),Dy~(3+)发光粉的生产工艺

以马来酸酐(MA)和吲哚啉螺苯并吡喃(SP)为原料,在SrAl2O4∶Eu2+,Dy3+(SAO-ED)发光粉的表面进行复合包覆制备MA-SP-SAO-ED复合发光粉,探讨MA与SP的质量比、MA和SP的加入顺序对复合发光粉性能的影响,并用扫描电镜表征复合发光粉的表面涂层。结果表明,当MA和SP同时加入SAO-ED二氯甲烷溶液中,总加入量为SAO-ED发光粉质量的10%,且MA与SP的质量比为6∶1时,复合发光粉具有较好的耐水、光致发光和光致变色等性能;在SAO-ED发光粉表面包覆了均匀致密涂层。