SPS制备SmCo7-xFex块状纳米晶磁体的研究

采用高能球磨法制得SmCo7-xFex非晶粉末,然后采用放电等离子技术将其烧结为块状纳米晶磁体,对磁体的微观结构和磁性能进行了观察和测试.结果表明,SmCo7-xFex球磨5 h后成为非晶粉末,经SPS烧结后得到1:7相.TEM观察表明,磁体晶粒尺寸在20～50 nm.另外,磁体具有较好的磁性能,当x=0.4时,矫顽力为992.8 kA/m,剩磁为0.634T,(BH)max为69.75KJ/m3.     

固化球磨纳米晶粉末制备块体超细晶Mg-3Al-Zn合金(英文)

采用粉末冶金技术制备块体超细晶Mg-3Al-Zn合金。首先采用球磨Mg、Al、Zn混合粉末来制备纳米晶粉末,所得的粉末的平均晶粒尺寸为45nm。随后将球磨好的粉末封入铝包套内,分别在室温和633K温度下,在真空烧结炉内进行真空热压。然后将烧结后的样品在423K下挤压以进行进一步的致密化处理。结果表明:致密后的冷压样品的晶粒尺寸为180nm,而热压坯的晶粒尺寸为600nm,冷压样品的屈服强度达464MPa;超细晶镁合金的强化机制主要是细晶强化,这主要是由于HCP结构的材料晶粒尺寸对材料的影响更为明显。固化后冷压样品的最终密度为(1.777±0.006)g/cm3,而热压样品的最终密度为(1.800±0.006)g/cm3。     

Investigation of the processes of refining of ceramic articles in a plasma flow

Results of investigations of the process of dissipation of polydisperse particles in low-temperature plasma flow with the formation of ultrafine, including nanosized, particles are presented. A special method is proposed that can be used for producing polydisperse powders, including ultrafine and nanosized powders, with spherical particles and the amorphous, crystalline, or amorphous, crystalline structure.     

An Investigation of Carbon Content and Consolidation Temperature on Microstructure and Properties of Hafnium Boride Ceramic

This paper discusses the use of Plasma Pressure Compaction to consolidate hafnium diboride powders. The effect of carbon addition on densification was studied. The influence of consolidation temperature on microstructure, density, and hardness of the bulk sample is presented. The interrelationship between microstructure and properties of the bulk sample are rationalized in light of the intrinsic influence of carbon content and the extrinsic influence of consolidation temperature.     

Structure, composition, and physicomechanical characteristics of HfB2 and Hf-B-N films

The paper deals with the study of the effect of the deposition conditions (the bias potential and substrate temperature) on the structure, composition, and physicomechanical characteristics of nanocrystalline films of hafnium diboride and boridonitride formed by the method of nonreactive (in Ar) and reactive (in Ar + N₂) HF magnetron sputtering, respectively. The optimal conditions for the deposition of the hafnium diboride coatings with growth texture in plane (00.1) and the best physicomechanical characteristics are deter-mined. It is shown that at a bias potential of ±50 V and a substrate temperature of ～500°C superstoichiometric highly textured films are formed with a nanohardness of 44 GPa and an elastic modulus of 396 ± 11 GPa. A relation between the composition, structure, and physicomechanical characteristics of the films is found. Reactive sputtering in (Ar + N₂) makes it possible to produce amorphous-crystalline films of the composite (HfB₂ + BN) that consists of grains of the HfB₂ nanocrystalline phase, the spaces between which are filled with the amorphous phase of graphite-like BN.     

放电等离子烧结-非晶晶化法合成Ti7oNb7.8Cu8.4Ni7.2Al6.6复合材料

采用机械合金化制备不含和含2%(体积分数)B4C的钛基非晶合金粉末,随后采用放电等离子烧结-非晶晶化法合成不含／含(TiB+TiC)的Ti7oNb7.8Cu8.4Ni7.2Al6.6超细晶／细晶钛基复合材料;运用X射线衍射分析(XRD)、差示扫描量热分析(DSC)、扫描电子显微镜(SEM)和万能材料试验机等对制备的钛基非晶粉末和超细晶／细晶钛基复合材料进行表征.结果表明高能球磨80h的钛基粉末中主要为非晶相,B4C颗粒的加入对钛基粉末的玻璃转变温度、晶化温度和晶化焓有显著的影响.另外,不含／含(TiB+TiC)的复合材料的显微硬度分别为5.47和5.33GPa;以50K/min升温到1223K并保温10min获得的Ti70Nb7.8Cu8.4Ni7.2Al6.6块体试样的断裂强度和断裂应变分别为2098MPa和11.5%.     

机械合金化W-Ni-Fe纳米复合粉的制备及结构研究

W,Ni,Fe粉末按照91.16W6．56Ni2.26Fe和95W5Ni的成分配比进行了机械合金化(MA)．通过调整球磨转速、球磨时间等工艺参数研究了其对粉末结构的影响,并对机械合金化粉末的物相、合金化特性、晶粒尺寸、点阵畸变及粉末形貌和颗粒度作了测定和分析讨论.机械合金化使晶粒细化并产生孪晶和位错．有利于原子扩散形成过饱和固溶体和非晶；高的球磨能有利于形成非晶相、晶粒细化和点阵畸变，350r／min球磨20h后晶粒尺寸可达25nm；输入的球磨能不同．粉末粒度的变化路径不同，但都会经历长大，变小和稳定三个不同阶段.     

超微LaMnO3的合成与导电性研究

采用柠檬酸盐热解法合成了ＬａＭｎＯ３超微粉末。经Ｘ射线衍射分析表明，所合成的ＬａＭｎｏ３为单相，属于六方晶系。实验发现，ＬａＭｎｏ３的平均粒径随焙烧温度的增加而明显地增大。首次研究了超微ＬａＭｎＯ３的电阻率随粒径的变化，发现ＬａＭｎＯ３的室温电阻率随粒径的增加而减小，导电活化能随粒径的减小而变小。     

粒径可控高振实密度球银的制备工艺研究

以硝酸银为原料,对苯二酚(C6H4(OH)2)为还原剂,链烷醇胺A为分散剂,用液相化学还原法制备高振实密度超细银粉。用激光粒度分布仪测试银粉的粒度分布与平均粒径,用扫描电子显微镜(SEM)和透射电子显微镜(TEM)分析银粉的形貌、粒径和团聚状态,用多晶X射线衍射(XRD)仪检测粉体的晶相。结果表明：通过调节硝酸银的浓度、硝酸银与还原剂的配比以及分散剂的用量等,可以实现对所制备球银粒径的控制;制备的超细银粉为面心立方晶体结构,呈规则球形,振实密度可达4.0 g/cm3。     

Fabrication of cast carbon steel with ultrafine TiC particles

The carbon steels dispersed with ultrafine TiC particles were fabricated by conventional casting method. The casting process is more economical than other available routes for metal matrix composite production, and the large sized components to be fabricated in short processing time. However, it is extremely difficult to obtain uniform dispersion of ultrafine ceramic particles in liquid metals due to the poor wettability and the specific gravity difference between the ceramic particle and metal matrix. In order to solve these problems, the mechanical milling (MM) and surface-active processes were introduced. As a result, Cu coated ultrafine TiC powders made by MM process using high energy ball milling machine were mixed with Sn powders as a surfactant to get better wettability by lowering the surface tension of carbon steel melt. The microstructural investigations by OM show that ultrafine TiC particles are distributed uniformly in carbon steel matrix. The grain sizes of the cast matrix with ultrafine TiC particles are much smaller than those without ultrafine TiC particles. This is probably due to the fact that TiC particles act as nucleation sites during solidification. The wear resistance of cast carbon steel composites added with MMed TiC/Cu-Sn powders is improved due to grain size refinement.     

高能球磨法制备纳米晶Ni粉的研究

采用高能球磨法制备出了纳米晶镍粉,并利用X射线衍射仪（XRD）、扫描电镜（SEM）、透射电镜（TEM）等分析检测手段,研究了该纳米晶镍粉末的结构、形貌和相的变化。结果表明,镍粉末平均粒度和晶粒度随球磨时间增加不断减小,而应变随球磨时间增加不断增大;当高能球磨54h后,球磨产物为FCC结构的鳞片状多晶体,晶粒度为17nm左右,应变为0.48%,颗粒尺寸为150～200nm;球磨时间增加至98h,产物中出现非晶相,但仍以多晶为主,晶粒尺寸为7nm,应变为1.24%,粉末团聚严重。     

烧结(Nd,Tb)-Fe-B磁体的元素扩散、反磁化和矫顽力

采用双合金法将两种粉末混合制备烧结永磁体可提高磁体磁性能;但在烧结过程中两种粉末之间存在元素扩散,元素扩散对磁性能的影响程度需要进一步研究。本文将Nd13Fe81B6和TbHx粉末混合制备烧结磁体,Nd13Fe81B6磁体矫顽力为4.5 kOe。当TbHx混合量为3 wt.%,烧结磁体的矫顽力增加至20.0 kOe。通过热激活研究认为,磁畴壁的形核是反磁化需要经过的过程。由于热力学的原因Tb元素更容易扩散进入Nd2Fe14B主相而不是富集在晶间富稀土相。Tb元素进入主相替代Nd可形成具有更高各向异性场的(Nd,Tb)-Fe-B表层,在反磁化过程中晶粒表层磁畴壁的形核场会增加,因此矫顽力增加程度显著。但是,TbHx混合量超过5 wt.%,矫顽力增加幅度降低。对于TbHx混合量7 wt.%的磁体,元素分布显示在主相晶粒内部贫Tb区域明显增少,证实在烧结过程中更多Tb原子从晶粒表层扩散入晶粒内部,这样晶粒表层反磁化形核场的提高程度会减弱,因而磁体矫顽力增加幅度降低。本研究说明要提高双合金Nd-Fe-B磁体磁性能需进一步控制元素扩散并优化磁体的元素分布。     

放电等离子烧结-热变形各向异性Nd-Fe-B磁体的微观组织及磁性能

采用放电等离子烧结及后续热变形技术制备各向异性Nd-Fe-B磁体,研究烧结温度对放电等离子烧结Nd-Fe-B磁体微观组织和磁性能的影响。随着烧结温度在650~900°C范围内的升高,烧结态Nd-Fe-B磁体的剩磁、内禀矫顽力及最大磁能积呈现先升后降的趋势。在800°C下烧结所获得磁体的磁性能最佳。随后,对800°C烧结后具有最佳磁性能的磁体采用放电等离子烧结技术进行后续热变形处理。与初始吸氢-歧化-脱氢-再复合粉末和烧结态磁体相比,热变形磁体拥有更显著的各向异性和更好的磁性能。当热变形温度为800°C且压缩比为50%时,热变形磁体中的Nd2Fe14B晶粒呈扁平片状且不发生异常长大;磁体沿热压方向具有最佳的磁性能：Br、Hcj和（BH）max分别为1.16 T、449 k A/m和178 k J/m3。     

The influence of powder characteristics on mechanical properties of Al2O3–TiC–Co ceramic materials prepared by Co‐coated Al2O3/TiC powders

Ultrafine Al₂O₃–TiC–Co (ATC) ceramic is prepared in order to improve the bending strength and fracture toughness of ceramic materials. The ultrafine Co‐coated Al₂O₃ and TiC powders have been synthesized by electroless plating at room temperature, and the composite powders were sintered by hot‐pressing to compact ATC samples. The average bending strength, average hardness and average fracture toughness values of ATC ceramic with different particle sizes and Co contents were investigated. The toughening mechanism of the ultrafine ATC ceramic was studied by transmission electron microscopy (TEM) and ceramic performance testing methods. The results show that the relative density, bending strength and fracture toughness values increase remarkably with the increase of Co content. The ultrafine grain of original powders is beneficial to improve the relative density, strength and toughness values of ATC ceramic. The Co phase hinders the growth of ATC ceramic grains during sintering. The Co phase forms a three‐dimensional mesh skeleton structure during sintering, improving the fracture toughness and strength of the composite ceramic.     

Preparation of ultrafine tungsten powders by in-situ hydrogen reduction of nano-needle violet tungsten oxide

Ultrafine tungsten powders with a grain size below 0.5 μm are key raw materials for fabricating ultrafine cemented carbides. Conventional hydrogen reduction technique has been utilized to prepare the ultrafine tungsten powders. In the present work, highly pure nano-needles of violet tungsten oxide (WO_2.72) were reduced by dry hydrogen. Nucleation and growth of the metallic tungsten in the early stage of hydrogen reduction have been studied by XRD, FESEM and HRTEM. Mechanism of formation of nano-size tungsten powders is proposed and a concept of in-situ hydrogen of the nano-needle WO_2.72 is presented. Empirical relations between an average diameter of nano-needle WO_2.72 and an average particle size of the resultant tungsten powders in both stage of nucleation and industrial conduction have been established. These empirical relations could be a reasonable guidance for suitably choosing the raw materials of nano-needle WO_2.72 to prepare ultrafine tungsten powders. It has been determined that the BET special surface areas of the in-situ hydrogen-reduced tungsten powders with the average particle size of 0.2 μm and 0.3 μm, which were produced from the raw nano-needle WO_2.72 powders with the average diameter of 60 nm and 80 nm, are 6.03 m²/g and 4.65 m²/g, and the oxygen contents are 0.35% and 0.29%, respectively.     

WC-Co复合粉末的原位合成及于硬质合金涂层制备中的应用

目的为解决超细/纳米WC-Co热喷涂时易于脱碳等瓶颈问题,制备具有高的硬度、断裂韧性、耐磨性和表面质量等优异综合性能的超细及纳米结构硬质合金涂层,并推广其在工业领域中的应用。方法以原位合成技术批量制备的超细/纳米WC-Co复合粉末为原料,利用团聚造粒技术制备得到具有高球形度和致密性,并保持原有超细/纳米结构的喷涂喂料粉末,利用超音速火焰喷涂工艺制备低脱碳、高致密的超细结构WC基涂层。结果降低喂料粉末孔隙度可有效减少涂层中W2C等脱碳相的含量,在优化工艺下制备的超细结构WC基涂层的硬度达到1450HV0.3以上,韧性相对于常规微米结构涂层提高40%以上,在两种载荷和磨料条件下均表现出更高的耐磨性。结论利用原位反应技术批量合成的超细/纳米WC-Co复合粉制备的硬质合金涂层具有优良的综合性能,可应用于对涂层的硬度、耐磨性、强韧性配合和表面质量有较高要求的工况。     

制备工艺对NaFeB磁体力学性能的影响

采用速凝法在铸带炉中制备NdFeB铸带,再经烧结制得NdFeB磁体。研究了制备工艺对磁体力学性能的影响。并将其结果与采用感应炉制得的铸锭经相同烧结工艺得到的磁体的力学性能进行了比较。实验结果得出：铸带速度2．6m/s时磁体的抗弯强度约为231MPa,当铸带速度增大到4．0m/s,抗弯强度显著提高了50％;当氢含量从0．15％减少到0．047％,抗弯强度提高了1倍,达到270MPa,冲击功也从2．78kJ／m^2增加到7．58kJ／m^2,这是因为在烧结过程中氢原子穿过晶粒和晶界扩散,其扩散通道导致的微裂纹强烈影响磁体的抗弯强度;磁粉粒度从4．0um减少到2．9um时,磁体晶粒减小,组织致密,抗弯强度从213MPa增大到331MPa。铸锭法制备的烧结磁体的综合力学性能均比铸带法磁体的性能差得较多。     

Extrusion Upsetting Multiple Processing in Sandglass Die

The mechanical Properties of some alloys canbe improved When ultrafine microstrUcttires areobtained. Some materials appear some unusualproperties [l, 2] when grain sizes reach aboutnanoscale. Theoretic analysis and experimentalresults on superplasticity show that the ultrafinegrain (submicron or nanoscale grains, subgrainsor nanophase etc.) materials are possible to exhibit superplaSticity under much lower temperatllTe, or their superplastic strain rate can be enhanced to great extent [3--5]…     

纳米材料在硬质合金中的应用

WC晶粒不断细化是硬质合金发展的一个重要特征。从硬质合金的纳米原料、纳米硬质合金、纳米材料助长或增强超粗晶硬质合金以及硬质合金的纳米涂层材料等4个方面论述了纳米材料在硬质合金中的应用,着重报道了中国在这些方面的优势。纳米粒径原料的制备是首要难题,1997年发明的“紫钨原位还原”技术利用传统工艺制备纳米、超细碳化钨粉末,碳化钨粉的粒径可小于20 nm。纳米硬质合金技术利用低压热等静压或热等静压,克服了烧结过程中 WC异常长大的难题,制备100～200 nm纳米硬质合金,抗弯强度在5000 MPa以上,使用性能优于亚微或超细晶硬质合金,已用于生产。利用“纳米颗粒溶解法”制备的超粗晶硬质合金晶粒度可达12μm;而含有纳米Co2 W4 C增强相的超粗晶硬质合金产品,使用寿命比普通合金产品提高了2～3倍。涂层材料纳米化,是硬质合金工具的一个发展方向,在耐磨性、硬度和抗裂纹扩展方面有明显优势,加工工件表面质量更好,工具使用寿命更长。     

Effect of diffusion annealing on the hysteretic properties of sintered Nd-Fe-B magnets

Effect of diffusion annealing on the formation of dysprosium-saturated grain boundaries in sintered Nd-Fe-B magnets has been studied. As a source of diffusion, we used powders of metallic dysprosium, DyCu, DyGa, and Dy₃Co alloys and DyH _x hydride. Plates ∼1 mm thick made of sintered magnets were molded into powders with a particle size from 3 to 500 μm and subsequently annealed in a vacuum at 750–850°C for 0.5–10 h. After annealing, the microstructure and the elemental composition of grains and grain boundaries were studied by scanning electron microscopy. Under optimum annealing conditions, Dy atoms were shown to diffuse preferentially through grain boundaries of the magnets. The coercive force H _c of Nd-Fe-B plates, which were annealed in contact with the DyGa, Dy₃Co and DyH _x powders and subsequently annealed at 550°C, increases by 4–6 Oe; no substantial decrease in the remanence takes place. The increase in the coercive force depends of the powder particle size and temperature and time of diffusion annealing.