纳米Zr-V-O粉末的XRD及TG-DSC研究

利用机械合金化制备纳米Zr-V粉末，对制备过程的材料进行物相分析和热分析试验。初始粉末Zr（150μm）和V（150μm）元素粉末（纯度99．15％）按原子比1：2或1：1进行混合后在氩气气氛中放入SimoloyerCMol—2球磨仓中，按几种不同的试验条件进行球磨。同时在997K和1047K下热处理40min和1h，并对热处理前后的粉末进行了物相和TG-DSC实验分析。     

机械合金化制备铝基非晶和纳米晶合金

综述了机械合金化制备纳米晶、非晶的研究进展,重点介绍了机械合金化制备铝基纳米 晶,非晶合金的研究现状。     

放电等离子烧结制备纳米Ni块体材料

采用自悬浮定向流法制备纳米Ni粉体,利用放电等离子烧结技术制备出了直径10 mm、厚2 mm,致密度为96.8 %,显微硬度为4.17 GPa的纳米块体材料。用X射线衍射仪、扫描电子显微镜和显微硬度计分析了烧结块体样品的相组成、晶粒尺寸、微观形貌和显微硬度。研究表明：随烧结温度的升高,块体样品的致密度和晶粒尺寸增大,当烧结温度为650 ℃时,致密度最高,晶粒尺寸为44.8 nm;显微硬度随烧结温度的增高先增大后减小,当烧结温度为550 ℃时,显微硬度最大为4.33 GPa;较高烧结温度下,断口微观形貌的纳米级韧窝出现,显示了韧性断裂的特征。     

采用真空热压技术制备纳米金属钨块体材料

 采用真空热压技术,在570 ℃和1 GPa的条件下成功制备具有单相α-W结构、平均晶粒尺寸为34 nm、尺寸为Φ10 mm×1 mm的难熔金属钨纳米块体材料,其密度为理论密度的88.8%,显微硬度为4.8 GPa。纳米金属钨的密度和显微硬度随热压温度、热压压强和热压时间增大而升高。     

纳米氧化锌粉体的制备及发光性质的研究

采用沉淀法制备纳米ZnO粉体，探讨了晶粒尺寸与反应浓度和热处理温度的关系，并对所得到的纳米ZnO粉体的发光性质进行了研究，对不同温度热处理的样品的发光性质做了比较。ZnO的可见发光机制的解释一直未有定论。一部分作者认为绿光是由氧空位引起的；另一部分认为是锌空位造成的。本文的实验结果揭示了可见发光的内部过程，肯定了双声子参与的发光过程，支持了绿色是由锌空位造成的这一观点。此外，用230nm以下波长激发样品时，可见发光的行为明显不同于用325nm以上的波长去激发同一样品时的发光情形。实验表明高能激发，样品能发白光，因此，用ZnO做白光二极管是可能实现的。     

Ag-ZnO纳米复合热电材料的制备及其性能研究

ZnO是一类具有潜力的热电材料, 但其较大声子热导率影响了热电性能的进一步提高. 纳米复合是降低热导率的有效途径. 本文以醋酸盐为前驱体, 溶胶-凝胶法制备了Ag-ZnO纳米复合热电材料. 扫描电镜照片显示ZnO颗粒呈现多孔结构, Ag纳米颗粒分布于ZnO的晶粒之间. Ag-ZnO纳米复合材料的电导率比未复合ZnO材料高出100倍以上, 而热导率是未复合ZnO材料的1/2. 同时, 随着Ag添加量的增加, 赛贝克系数的绝对值逐渐减小. 综合以上原因, 添加7.5%mol Ag的Ag-ZnO纳米复合材料在700 K时的热电优值达到0.062, 是未复合ZnO材料的约25倍. 在ZnO基体中添加导电金属颗粒有利于产生导电逾渗通道, 提高材料体系的电导率, 但同时导致赛贝克系数的绝对值减小. 总热导率的差异来源于声子热导率的差异. 位于ZnO晶界的纳米Ag颗粒, 有利于降低声子热导率. 关键词： 热电材料 ZnO 纳米复合 热导率     

纳米Mg-Ni合金的制备技术

纳米Mg-Ni贮氢材料具有成本低，活化容易、贮氢容量大，吸放氢动力学性能优异等特点，有很大的应用前景。本文用机械合金化法进行了纳米Mg-Ni合金的制备，且对制备的粉末进行了XRD，TEM，SEM等微观结构的分析。     

CeOx与ZnO纳米复合粉体的制备及其发光性能

通过溶胶-凝胶法制备CeOx／ZnO纳米复合粉体,并对其结构和光致发光特性进行了研究。发现500℃烧结出的复合粉体在502nm处的绿光发射同纯ZnO的相比有显著的增强;600℃烧结的样品在603nm出现新的发光峰。通过XRD和XPS分析认为荧光增强的主要原因同粉体中铈主要以Ce^3 形式存在有关,新的发光峰可能来源于ZnO／CeO2界面处形成的新的能级跃迁。     

去合金化制备纳米多孔铜

 以Mn-Cu合金为前驱体合金,在0.1 mol/L HCl 溶液中自由腐蚀去合金化成功制备出纳米多孔铜,采用扫描电镜和X射线能谱仪对去合金腐蚀前后样品的形貌和成分进行了分析,结果表明,Mn-Cu合金在0.1 mol/L HCl 溶液中发生锰的选择性溶解,制备出的纳米多孔铜呈3维网络状均匀结构,平均系带尺寸53 nm,平均孔径尺寸为140 nm。     

去合金化制备纳米多孔铜

以Mn-Cu合金为前驱体合金,在0.1 mol/L HCl 溶液中自由腐蚀去合金化成功制备出纳米多孔铜,采用扫描电镜和X射线能谱仪对去合金腐蚀前后样品的形貌和成分进行了分析,结果表明,Mn-Cu合金在0.1 mol/L HCl 溶液中发生锰的选择性溶解,制备出的纳米多孔铜呈3维网络状均匀结构,平均系带尺寸53 nm,平均孔径尺寸为140 nm。     

Characterization of nanocrystalline FeSiCr powders prepared by ball milling

FeSi₁₀Cr₁₀ powder was mechanically alloyed by high energy planetary ball milling, starting from elemental powders. The microstructural and magnetic properties of the milled powders were characterized by scanning electron microscopy, X-ray diffraction, ⁵⁷Fe Mössbauer spectrometry and a vibratory sample magnetometer.After 3 h of milling, the formation of two bcc solid solutions α-Fe₁ (Si, Cr) and α-Fe₂ (Si, Cr) is observed. Their grain sizes decrease with increase in milling time attaining, at 15 h of milling, 23 and 11 nm, respectively. Mössbauer spectra of the milled powder show the presence of two components. One is a ferromagnetic type with a broad sextuplet. Its distribution of hyperfine field is characterized by high and low hyperfine field’s peaks and a mean value of 26.5 T. The other is a single paramagnetic peak. Its low concentration increases to ∼4% at 15 h of milling. These results can be explained by different atomic environments affected by Si or/and Cr elements, as well as the increased disordered grain boundaries.Magnetic measurements of the milled FeSi₁₀Cr₁₀ alloy powder exhibit a soft ferromagnetic character with a decrease of both magnetization at saturation (Ms) and coercive force (Hc) with milling time attaining values of Ms=151 emu/g and Hc=2500 A/m at 30 h of milling time.     

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采用射频(RF)等离子体对颗粒形状不规则的钨粉球化,研究了加料速率和钨粉分散方式对球化率的影响。通过用电子扫描显微镜(SEM)观测得到的被球化粉末的百分比评估了球化效率。通过对球化处理的钨粉的X射线衍射谱(XRD)的检测,验证了在球化过程中无氧化发生和其它杂质介入。当钨粉以极短暂时间(约几毫秒)快速穿越等离子体炬时,钨粉颗粒因受热而熔化成液滴,快速冷却后,形成致密的球形固态颗粒。     

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向钨中添加稀土氧化物能显著细化晶粒和提高钨合金的高温稳定性,且具有弥散强化效应,在抑制晶粒长大、控制再结晶晶粒的形状以及提高材料的力学性能方面效果显著。从制备稀土氧化物弥散强化钨基复合材料(ODS-W)粒子方法出发,阐述了几种ODS-W制备工艺的研究现状并对其发展趋势进行展望。     

射频等离子体制备球形钨粉研究

采用射频(RF)等离子体对颗粒形状不规则的钨粉球化,研究了加料速率和钨粉分散方式对球化率的影响。通过用电子扫描显微镜(SEM)观测得到的被球化粉末的百分比评估了球化效率。通过对球化处理的钨粉的X射线衍射谱(XRD)的检测,验证了在球化过程中无氧化发生和其它杂质介入。当钨粉以极短暂时间(约几毫秒)快速穿越等离子体炬时,钨粉颗粒因受热而熔化成液滴,快速冷却后,形成致密的球形固态颗粒。     

Influence of environment and grain size on magnetic properties of nanocrystalline Mn–Zn ferrite

Nanocrystalline Mn_1−xZn_xFe₂O₄ (0.2?x?0.9) was prepared by mechanical alloying of the concerned oxide precursors and subsequent annealing in air and Ar atmosphere, respectively. Milling and annealing in air produces Zn-ferrites (ZnFe₂O₄) instead of Mn–Zn ferrites as MnO converts to higher oxides at higher oxygen partial pressure and fails to dissolve in the spinel phase. This is confirmed by careful quantitative X-ray diffraction analysis using Rietvelt profile matching and also by the non-saturating paramagnetic nature of the magnetization response with very low saturation level of these spinels milled and annealed in air. On the other hand, single-phase Mn–Zn ferrite results from the identical precursor oxide blend when milling and annealing are carried out under controlled (Ar) atmosphere. The average grain size of the as-milled and annealed powders, measured by Rietvelt refinement, varies between 6–8 and 14–18 nm, respectively. Further investigations performed with Mn_0.6Zn_0.4Fe₂O₄ reveal that a careful selection of annealing parameters may lead to an early superparamagnetic relaxation. Therefore, the blocking temperature can be significantly reduced through proper heat treatment schedule to ensure superparamagnetism and negligible hysteresis at low temperature.     

Evolution of structure, microstructure and hyperfine properties of nanocrystalline Fe50Co50 powders prepared by mechanical alloying

Nanostructured Fe₅₀Co₅₀ powders were prepared by mechanical alloying of Fe and Co elements in a vario-planetary high-energy ball mill. The structural properties, morphology changes and local iron environment variations were investigated as a function of milling time (in the 0-200 h range) by means of X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray analysis and ⁵⁷Fe Mössbauer spectroscopy. The complete formation of bcc Fe₅₀Co₅₀ solid solution is observed after 100 h milling. As the milling time increases from 0 to 200 h, the lattice parameter decreases from 0.28655 nm for pure Fe to 0.28523 nm, the grain size decreases from 150 to 14 nm, while the meal level of strain increases from 0.0069% to 1.36%. The powder particle morphology at different stages of formation was observed by SEM. The parameters derived from the Mössbauer spectra confirm the beginning of the formation of Fe₅₀Co₅₀ phase at 43 h of milling. After 200 h of milling the average hyperfine magnetic field of 35 T suggests that a disordered bcc Fe-Co solid solution is formed.     

Investigating the magnetic properties of soft magnetic composites based on mechanically alloyed nanocrystalline Fe-5 wt% Ni powders

In this work, the soft magnetic composites (SMCs) of the nanocrystalline Fe-5 wt% Ni powders coated with phenolic resin were studied. The nanocrystalline powders with an average diameter of 10 nm were obtained by mechanical alloying up to 96 h milling in a high-energy planetary ball mill. The microstructure and magnetic properties of the milled powders were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy and a vibrating sample magnetometer. The results of X-ray diffraction showed that the bcc Fe(Ni) solid solution is formed after 24 h milling. Magnetic measurements indicated that the 96 h milled powders with a steady-state grain size of 10 nm have the highest saturation magnetization and the lowest coercivity. The SMCs based on nanocrystalline powders showed higher electrical resistivity and magnetic permeability up to 1 MHz, as compared with the pure iron-based composites. Besides, the nanocrystalline-based SMCs exhibited higher relaxation frequency and a significantly lower loss factor up to 1 MHz.     

ICF物理实验用纳米Cu块体靶材的制备研究

 采用自悬浮定向流法制备了金属纳米粉体并采用真空手套箱专利技术和冷压法在高压（1.5 GPa）作用下保压40 min后，成功制备出了相对密度达97％和显微硬度达1.85 GPa的金属Cu纳米晶材料。经XRD分析，其晶粒大小为20 nm。正电子湮没(PAS)实验结果表明，其空隙大小和数量与采用惰性气体冷凝法原位压制(IGC)的样品相比，空位簇数量较多，微空隙的大小和数量基本相当。激光惯性约束聚变（ICF）模拟实验表明：采用该方法制备的纳米Cu块体材料靶的激光转换效率比常规Cu材料靶高5倍。     

Decay processes of photoluminescence in a nanocrystalline SiC thin film

Nanocrystalline (nc)-SiC film has been deposited by helicon wave plasma enhanced chemical vapor deposition technique and intense blue-white light emission is obtained. Microstructure analyses show that the 3C–SiC particles are embed in amorphous SiC matrix, and the average size of the nc-SiC is 3.96 nm. The photon energy of the main photoluminescence (PL) band is higher than the band gap of bulk SiC, which indicates that the optical emission mainly occurs in quantum states of 3C–SiC nanocrystals. In addition, the band tail states of amorphous SiC also contribute to the optical emission. Three decay processes are obtained from time-resolved PL spectra by deconvolution treatment, and the decay components correspond to the quantum confinement effect (QCE), surface states of nc-SiC particles, and band tail of amorphous SiC, respectively. The fractional integrated PL intensity of QCE related decay process decreases dramatically in the lower PL photon energy, indicating that the QCE mainly contributes to the short wavelength optical emission.     

Photoacoustic study of nanocrystalline silicon produced by mechanical grinding

Mechanical grinding (MG) was used to produce nanocrystalline silicon and its thermal and transport properties were investigated by photoacoustic absorption spectroscopy (PAS). The experimental results suggest that in as-milled nanocrystalline silicon for 10 h the heat transfer through the crystalline and interfacial components is similar, and after annealed at 470 °C the heat transfer is controlled by crystalline component.