Morphology and microstructure characterization of 95W-3.5Ni-1.5Fe powder prepared by mechanical alloying

Morphology and microstructure characterization of 95W-3.5Ni-1.5Fe powder prepared by mechanical alloying@Islam S.Humail$State Key Laboratory for Advanced Metals and Materials,Materials Science and Engineering School, University of Science and Technology B…     

低温球磨制备Mg-4%Ni-1%NiO储氢材料及其性能

采用低温球磨技术制备了Mg-4%Ni-1%NiO储氢材料,主要研究低温球磨时间对材料形貌结构以及储氢性能的影响.采用扫描电子显微镜(SEM)和X射线衍射(XRD)分析材料的形貌和相组成,采用压力-组成-温度(P-C-T)设备研究材料的储氢性能.结果表明:分别经过2、4和7 h球磨后,材料的相组成没有发生明显改变,只有极少量的Mg2Ni合金相生成.随着球磨时间的延长,材料的平均粒度逐渐下降,作为催化剂的Ni、NiO相逐渐揉进基体内部.伴随着上述变化,材料的活化性能、吸氢性能逐渐提高,球磨到7 h后材料仅需活化1次即可达到最大吸放氢速率,初始吸氢温度降为60℃,在4.0 MPa初始氢压和200℃下吸氢量为6.4%(质量分数),60s即可完成饱和吸氢量的80%,10min内完成饱和吸氢量的90%;材料的放氢性能则在球磨4 h后已经基本保持不变,0.1MPa下初始放氢温度为310℃,在350℃、0.1MPa下材料可在500s内释放饱和储氢量的80%.     

Preparation of CNT/AlSi10Mg composite powders by high-energy ball milling and their physical properties

This study investigated the effects of carbon nanotube (CNT) concentration on the micro-morphologies and laser absorption properties of CNT/AlSi10Mg composite powders produced by high-energy ball milling. A scanning electron microscope, X-ray diffractometer, laser particle size analyzer, high-temperature synchronous thermal analyzer, and UV/VIS/NIR spectrophotometer were used for the analysis of micrographs, phases, granulometric parameters, thermal properties, and laser absorption properties of the composite powders, respectively. The results showed that the powders gradually changed from flake- to granule-like morphology and the average particle size sharply decreased with increases in milling rotational speed and milling time. Moreover, a uniform dispersion of CNTs in AlSi10Mg powders was achieved only for a CNT content of 1.5wt%. Laser absorption values of the composite powders were also observed to gradually increase with the increase of CNT concentration, and different spectra displayed characteristic absorption peaks at a wavelength of approximately 826 nm.     

微硅粉固相反应制备莫来石粉体工艺

 以微硅粉和工业氧化铝为原料,在空气气氛下固相反应合成莫来石粉体。研究了煅烧温度和Al₂O₃/SiO₂的物质的量比对反应产物物相组成的影响,结果表明,当Al₂O₃ /SiO₂的物质的量比为3：2.5、煅烧温度为1450℃时,制备莫来石粉体质量分数达到最高,根据K值法计算其质量分数为95%。莫来石粉体平均粒径随球磨时间延长而逐渐减小,最终粉体平均粒径为0.58μm,比表面积为9.26m²/g,粒径分布由单峰分布演变为双峰分布,莫来石粉体颗粒形状不规则,以多边体状存在。     

Preparation of nano-sized Bi2Te3 thermoelectric material powders by cryogenic grinding

A novel method for rapid preparation of Bi2Te3 nano-sized powders with an average particle size of about 70 nm was developed.A starting powder mixture consisting of Bi2Te3 coarse particles of ～5 mm was...     

CuO纳米晶的一步超声室温固相合成及表征

在室温条件和超声波作用下,通过固相化学反应一步合成了CuO纳米晶,用粉末X射线衍射（XRD）及电子衍射法（ED）分析了固相产物的物相,用透射电镜（TEM）观测粒子的大小、形貌、粒径及粒径分布．结果表明,产物为颗粒大小均匀、晶粒形貌为近似球形粒状,平均粒径约为20nm的纳米晶,产率为93．1％．改变反应物、反应物配比、掺入惰性物质、加入微量溶剂或表面活性剂、研磨不同的时间等固相反应条件对合成CuO纳米晶的晶粒形貌、粒度和粒径分布有一定影响．     

微乳液辅助室温湿固相法制备纳米氧化锆及其表征

通过微乳液介质的辅助,以室温湿固相法成功制备了纳米氧化锆粉体,考察了微乳液、球磨速度和热处理温度对产物氧化锆的物相及粒径的影响;用X-射线衍射对产物的物相构成进行了分析,以透射电子显微镜观察了产物的粒径和形貌。结果表明:借助微乳液油相介质,利用室温湿固相法以150r/min的球磨速度,经过2 h研磨,并对球磨产物进行500℃、2h的热处理,能够获得粒径约为40nm的四方相氧化锆粉体。     

Characterization of 17-4PH stainless steel powders produced by supersonic gas atomization

17-4PH stainless steel powders were prepared using a supersonic nozzle in a close-coupled gas atomization system. The characteristics of powder particles were carried out by means of a laser particle size analyzer, scanning electron microscopy (SEM), and the X-ray diffraction (XRD) technique. The results show that the mass median particle diameter is about 19.15 μm. Three main types of surface microstructures are observed in the powders:well-developed dendrite, cellular, and cellular dendrite structure. The XRD measurements show that, as the particle size decreases, the amount of fcc phase gradually decreases and that of bcc phase increases. The cooling rate is inversely related to the particle size, i.e., it decreases with an increase in particle size.     

Structure evolution of Y2O3 nanoparticle/Fe composite during mechanical milling and annealing

Fe-25 wt% Y2O3composite powders have been fabricated by mechanical milling(MM) Fe powders of 100 μm in diameter and Y2O3nanoparticles in an argon atmosphere for the milling periods of4,8,12,24,36,and 48 h,respectively.The features of these powders were characterized by using X-ray diffraction(XRD),scanning electron microscopy(SEM),electron probe micro analyzer(EPMA) and transmission electron microscopy(TEM).The experimental results showed that the mean particle size and crystalline size of MM powders decreased with the milling time increasing.All the elements distributed homogenously inside the powders after 48 h of MM.The lattice constant of the matrix α-Fe kept constant with the milling time,and no solid solution took place during MM process.After 8 h of MM,the α-Fe in each powder became nanocrystalline.After 48 h of MM,Y2O3changes from nanostructure into amorphous structure,and the crystalline size of α-Fe further decreased to 10 nm.The Y2O3in the powders mechanically milled for 48 h kept the amorphous structure after being annealed at 400 1C,and starts to crystallize when the powders are annealed at 600 1C.The amorphous Y2O3contains a small amount of Fe,and crystalline FeYO3appears at 800 1C.     

Al-Ti-C体系自蔓延高温合成TiC的形态演变

利用真空自蔓延加热-加压装置,采用X射线衍射(X-ray diffraction,XRD)、扫描电镜(scanning electron microscope,SEM)及能谱(energy dispersive spectrum,EDS)等分析测试手段,研究了Al含量、粉末粒度及C/Ti(原子比,下同)对Al-Ti-C体系自蔓延点燃温度、产物相组成及TiC形态的影响。结果表明,Al含量对TiC的尺寸影响最大,随着Al含量由20%(质量分数,下同)增加到50%时,TiC颗粒的尺寸由3～5μm减小到0.7～0.8μm。C粉粒度和C/Ti对TiC的形貌影响最大,当C粉粒度小于75μm或C/Ti≥1时,TiC的形貌为近球形;然而当C粉粒度不小于75μm或C/Ti1时,TiC的形貌为八面体。     

Structural characterization of AA 2024-MoSi2 nanocomposite powders produced by mechanical milling

Nano-sized MoSi₂ powder was produced successfully from commercially available MoSi₂ by a mechanical milling process carried out for 100 h, and mechanical alloying was employed to synthesize AA 2024-MoSi₂ nanocomposites. The effects of MoSi2 reinforcement and mechanical milling on the structure, morphology, and iron contamination of the produced materials were investigated using X-ray diffraction, scanning electron microscopy, and atomic absorption spectrometry. It is revealed that the morphology of the aluminum alloy changes continuously during milling from spherical to plate-like, irregular, and finally equiaxed. The presence of MoSi₂ reinforcement accelerates the milling process and results in a smaller average particle size. The Williamson-Hall method determined that the crystallite size of the aluminum alloy in the composite powder is smaller than that of the unreinforced alloy at the same milling time and this size reaches 45 nm after 16 h milling time. The Fe contamination content is higher for the nanocomposite in comparison with the unreinforced alloy because of the wearing role of MoSi₂ hard particles.     

Pseudo-<Emphasis Type="Italic">in-situ</Emphasis> stir casting: a new method for production of aluminum matrix composites with bimodal-sized B<Subscript>4</Subscript>C reinforcement

A new method was applied to produce an Al-0.5wt%Ti-0.3wt%Zr/5vol%B₄C composite via stir casting with the aim of characterizing the microstructure of the resulting composite. For the production of the composite, large B₄C particles (larger than 75 μm) with no pre-heating were added to the stirred melt. Reflected-light microscopy, X-ray diffraction, scanning electron microscopy, field-emission scanning electron microscopy, laser particle size analysis, and image analysis using the Clemex software were performed on the cast samples for microstructural analysis and phase detection. The results revealed that as a consequence of thermal shock, B₄C particle breakage occurred in the melt. The mechanism proposed for this phenomenon is that the exerted thermal shock in combination with the low thermal shock resistance of B₄C and large size of the added B₄C particles were the three key parameters responsible for B₄C particle breakage. This breakage introduced small particles with sizes less than 10 μm and with no contamination on their surfaces into the melt. The mean particle distance measured via image analysis was approximately 60 μm. The coefficient of variation index, which was used as a measure of particle distribution homogeneity, showed some variations, indicating a relatively homogeneous distribution.     

Characterization of MCrAlY/nano-Al2O3 nanocomposite powder produced by high-energy mechanical milling as feedstock for high-velocity oxygen fuel spraying deposition

Al2O3 nanoparticles and MCrAlY/nano-Al2O3 nanocomposite powder (M = Ni, Co, or NiCo) were produced using high-energy ball milling. The MCrAlY/nano-Al2O3 coating was deposited by selecting an optimum nanocomposite powder as feedstock for high-velocity oxy-gen fuel thermal spraying. The morphological and microstructural examinations of the Al2O3 nanoparticles and the commercial MCrAlY and MCrAlY/nano-Al2O3 nanocomposite powders were investigated using X-ray diffraction analysis, field-emission scanning electron microscopy coupled with electron dispersed spectroscopy, and transmission electron microscopy. The structural investigations and Williamson–Hall res-ults demonstrated that the ball-milled Al2O3 powder after 48 h has the smallest crystallite size and the highest amount of lattice strain among the as-received and ball-milled Al2O3 owing to its optimal nanocrystalline structure. In the case of developing MCrAlY/nano-Al2O3 nanocompos-ite powder, the particle size of the nanocomposite powders decreased with increasing mechanical-milling duration of the powder mixture.     

机械合金化制备碳化钛纳米粉体的合成机理研究

本研究中,以金属钛(Ti)粉与环己烷为原料,利用机械合金化制备了碳化钛(TiC)纳米粉体。利用X射线衍射并结合Rietveld精修对球磨产物进行定性与定量分析;借助透射电子显微镜对产物进行形貌与元素以及结晶性进行分析;对球磨过程中TiC的合成机理进行了研究。结果表明,球磨产物中主相为TiC,另有少量残留的氢化钛(TiH2)与Ti;所制备TiC粉体易于团聚、颗粒度均匀、结晶性良好;TiC合成机理属于扩散型机制。     

球形氧化镍粉末对乙醇的电催化性能的研究

通过水热-热分解法制备球形介孔氧化镍粉末,并采用X射线衍射、扫描电镜、透射电镜和比表面积仪对氧化镍粉末的形貌和结构进行表征;通过循环伏安法、计时电流法和电化学阻抗谱的测试,系统研究该种粉末在碱性介质中对乙醇的电催化氧化活性.结果表明：所得到的氧化镍粉末为球形,比表面积为35 m2·g-1,平均孔径为15.88 nm;该粉末对乙醇具有良好的催化活性,氧化电流随乙醇浓度和扫描速率的增大而增大,在0.60 V电位下保持1000 s,球形多孔氧化镍对乙醇氧化催化的电流衰减率为0.075%,稳定性比较好.循环伏安法、计时电流法和电化学阻抗谱测试表明,球形介孔NiO/玻碳电极( NiO/GCE)对乙醇的催化氧化反应机理为扩散控制.     

低温合成TiO2/Fe3O4磁载光催化剂的光催化性能研究

采用化学共沉淀法合成的磁性纳米Fe₃O₄为磁核,以钛酸四丁酯为原料,通过溶胶-凝胶法,在较低温度下合成了TiO₂/Fe₃O₄磁性光催化剂。利用XRD、TEM、SEM-EDX等分析方法对合成催化剂的相组成、形貌、粒度、元素分布等进行了表征;研究了不同焙烧温度及TiO₂/Fe₃O₄比例对降解罗丹明B光催化活性及磁分离回收性能的影响。结果表明,在100、300和450 ℃焙烧温度下磁性光催化剂的催化活性依次降低,较低温度(100 ℃)制备的催化剂具备较高的催化活性;当TiO₂质量分数处于67.3%～73.0%时,催化剂既具有较高的光催化降解活性也具有较好的磁分离回收性能;光催化剂TiO₂/Fe₃O₄（100 ℃,TiO₂质量分数70%）在循环使用5次后,在降解75 min时仍能达到对罗丹明B 99%的脱色率和90%的回收率。     

BST铁电厚膜的丝网印刷制备工艺研究

对丝网印刷制备BST铁电厚膜工艺中的粉体合成、浆料配置、烧结条件等进行了研究,采用X射线衍射、透射电镜和扫描电子显微镜及配套的能谱仪对制备的BST粉体与厚膜样品的微观结构、成分进行测试分析.结果表明,在氧化铝衬底上一次印刷湿膜,经1 230～1 260℃烧结0.5 h后可获得单相钙钛矿结构,平均晶粒尺寸可达0.5μm且...     

囊泡模板法制备纳米/微米级酚醛树脂中空球

以十六烷基三甲基溴化铵(CTAB)和十二烷基硫酸钠(SDS)分子自组装形成的囊泡为模板, 用氨水溶液提供缓冲环境, 甲阶酚醛树脂为前驱体, 控制表面活性剂配比, 反应温度和时间不变, 通过改变搅拌速率得到纳米/微米级酚醛树脂多层中空球, 并利用X射线衍射仪（XRD）、 透射电子显微镜（TEM）、 扫描电子显微镜（SEM）、 比表面积和孔隙分析仪、 热重分析仪（TGA）对所得微球进行表征. 结果表明： 酚醛树脂中空纳米球的粒径为50~60 nm, 球壳厚度约为10 nm; 酚醛树脂中空微米球分为单室和多室两种形貌, 单室中空球粒径为2~5 μm, 多室中空球粒径可达10 μm, 球壳厚度约为500 nm; 两种形貌的酚醛树脂中空球的球壳均为多层周期结构.     

Microstructures and mechanical properties of nanocrystalline NiTi intermetallics formed by mechanosynthesis

The formulation of nanocrystalline NiTi shape memory alloys has potential effects in mechanical stimulation and medical implantology. The present work elucidates the effect of milling time on the product's structural characteristics, chemical composition, and microhardness for NiTi synthesized by mechanical alloying for different milling durations. Increasing the milling duration led to the formation of a nanocrystalline NiTi intermetallic at a higher level. The formation of nanocrystalline materials was directed through cold fusion, fracturing, and the development of a steady state, which were influenced by the accumulation of strain energy. In the morphological study, uninterrupted cold diffusion and fracturing were visualized using transmission electron microscopy. Particle size analysis revealed that the mean particle size was reduced to~93 μm after 20 h of milling. The mechanical strength was enhanced by the formation of a nanocrystalline intermetallic phase at longer milling time, which was confirmed by the results of Vickers hardness analyses.     

ZnFe~Ⅲ类水滑石制备过程研究

以ZnSO4、FeSO4为原料,采用共沉淀和氧化的两步法合成了ZnFeⅢ二元类水滑石化合物,详细探讨了原料配比、pH及氧化处理条件等因素对合成产物物相的影响,借助XRD,FTIR,N2吸附等手段对合成物物化性能进行表征。研究结果表明:以Zn(NO3)2、Fe(NO3)3为原料,改变合成条件只能得到碱式碳酸锌或碱式硝酸锌;而以FeSO4、FeSO4为原料,采用共沉淀和氧化的两步法可得到晶相单一、结晶度良好的ZnFeⅢHTLcs。两步法制备ZnFeⅢ类水滑石的最适宜的条件为:n(Zn2+)/n(Fe2+)=2.0～3.0,pH=6.0～7.0,氧化温度为25℃,该条件下合成的ZnFeⅢHTLcs有较高的热稳定性,热分解温度为600℃;有较窄的粒径分布,中值粒径为1.24μm,平均粒径为1.28μm;吸附等温线类型为Ⅱ型,比表面积为23.08m2/g。