SnO_2@TiO_2核-壳纳米线的制备及其光催化性能

通过固-液-气(VLS)生长机制,利用化学气相沉积法(CVD)制备SnO_2纳米线。利用原子层沉积(ALD)以钛酸四异丙酯为前驱体在SnO_2纳米线表面沉积不同厚度的TiO_2壳层,形成SnO_2@TiO_2核-壳纳米线结构。通过中间Al_2O_3插层,分别制备出金红石和锐钛矿2种不同晶型的TiO_2,从而制备出2种不同复合结构的SnO_2@TiO_2核-壳纳米线。实验研究该复合结构中TiO_2的厚度与晶型对紫外光下光催化降解甲基橙溶液活性的影响。     

预退火处理对非晶Cu-Ti合金晶化过程动力学的影响SCIEI

对非晶Cu_(40)Ti_(60)合金引入一种预退火处理工艺,利用DSC研究了急冷态及预退火处理样品的晶化过程动力学,发现预退火处理使非晶合金的晶化温度、晶化激活能和Avrami指数值下降。由实验结果和理论分析得到了非晶Cu_(40)Ti_(60)合金的形核激活能和长大激活能。     

SnO2@TiO2核-壳纳米线的制备及其光催化性能研究

本文通过固-液-气(VLS)生长机制,利用化学气相沉积法(CVD)制备SnO₂纳米线。利用原子层沉积(ALD)以钛酸四异丙酯为前驱体在SnO₂纳米线表面沉积不同厚度的TiO₂壳层,形成SnO₂@TiO₂核-壳纳米线结构。通过中间Al₂O₃插层,分别制备出金红石和锐钛矿两种不同晶型的TiO₂,从而制备出两种不同复合结构的SnO₂@TiO₂核-壳纳米线。实验研究该复合结构中TiO₂的厚度与晶型对紫外光下光催化降解甲基橙溶液活性的影响。     

Fe基非晶及纳米晶合金的制备和电化学腐蚀行为

分别采用单辊甩带法和非晶晶化退火法制备出非晶及纳米晶合金Fe73.5Si13.5B9Nb3Cu1;利用DSC、XRD和TEM对该非晶合金的晶化行为进行了分析;并用电化学极化曲线的方法和电化学阻抗技术研究了该非晶合金经不同温度退火后在1mol/LHCl溶液里的电化学腐蚀行为。结果表明,该非晶合金的晶化过程出现2个阶段。当退火温度为500℃时,合金尚未晶化,仍保持非晶态;当温度达到550℃时,出现了晶化衍射峰,晶粒平均直径约13nm;当温度达到600℃时,晶粒平均直径约为15nm。经过退火得到的纳米晶合金的腐蚀电位大于未退火的非晶,且阳极电流密度变得更低,表明纳米晶状态时的耐腐蚀性能比非晶状态的更好。该非晶合金未退火、550℃退火和600℃退火时的EIS均由单一容抗弧构成,具有一时间常数;且随着退火温度升高,电化学反应电荷转移电阻在增大。     

退火工艺对Fe_(91.63)B_(1.27)Si_(7.09)非晶带材腐蚀性能的影响

采用真空电弧炉铜模铸造法制备出Fe_(91.63)B_(1.27)Si_(7.09)非晶带材,并用失重法对比研究了非晶带材在HCl、H_2SO_4溶液里的腐蚀行为;采用X射线衍射仪和光学显微镜对该非晶带材的相组成、晶化过程及试样的腐蚀形貌进行了研究,并综合分析了退火工艺对Fe_(91.63)B_(1.27)Si_(7.09)非晶带材耐腐蚀性能的影响。结果表明:Fe_(91.63)B_(1.27)Si_(7.09)非晶带材在20%H2SO_4溶液中的耐蚀性比45钢高300倍。非晶合金晶化程度随退火温度升高而提高,带材的腐蚀速率取决于退火温度。在500℃以下退火时,Fe_(91.63)B_(1.27)Si_(7.09)非晶带材腐蚀速率变化不大;在500℃以上退火时,Fe_3Si相和Si_4Cu_(15)相析出,腐蚀速率明显增大;当退火温度上升到700℃时,已由非晶态完全转变成晶态,腐蚀速率大幅度提高。     

退火对ZrCuNiAl非晶合金组织和硬度的影响

通过差示扫描量热法、X射线衍射、扫描电镜和显微硬度分析,研究了退火温度对Zr_(65)Cu_(17.5)Ni_(10)Al_(7.5)非晶合金组织结构和显微硬度的影响。随着升温速率的增加,玻璃转变温度T_g和晶化温度T_x逐渐升高。在623K(低于T_g)退火30min,试样保持非晶结构。在723K(高于T_g,低于T_x)以及823K和923K(高于T_x)退火30 min,发生晶化,结晶相为CuZr_2和NiZr_2。随着退火温度升高,结晶程度逐渐增加并达到饱和,纳米晶逐渐形核并长大,显微硬度先增大后减小。     

喷射沉积镧基非晶合金退火组织和成分分析

研究了喷射沉积La_(62)Al_(16)(Cu,Ni)_(22)大块非晶合金在不同退火工艺下的晶化过程和晶化组织转变。结果发现:573 K×30 min退火时,非晶合金可以完全晶化,并析出Al、AlNi、La和未知相。TEM显示Al和AlNi相的晶粒尺寸为纳米级,且晶化后的组织成分较为均匀,说明喷射沉积是制备镧基非晶合金的有效方法。     

非晶合金Fe_(80-x)Cu_xSi_5B_(15)和(Fe_(1-y)Co_y)_(82)Cu_(0.4)Si_(4.4)B_(13.2)的晶化行为

用X射线衍射、吸收和内转换电子发射Mossbauer谱技术,研究了Fe_(80-x)Cu_xSi_5B_(15)和(Fe_(1-y)Co_y)_(82)Cu_(0.4)Si_(4.4)B_(13.2)两系列非晶合金的晶化行为.单辊急冷法制备的非晶带,晶化首先从贴辊面开始,晶化产物为α-Fe相.在Fe_(80)Si_5B_(15)非晶合金中以少量Cu替代Fe可以提高晶化温度.我们的结果表明,过渡金属的含量超过80at.-%,如增加到82at.-%,晶化温度就明显降低.所研究两系列含Si的铁基非晶合金在400—450℃范围内退火2h,都出现α-Fe,Fe_3B和Fe_2B三种晶态相共存状态.退火温度再升高,亚稳相Fe_3B逐渐转变为Fe_2B和α-Fe.     

Ni-Fe-W-B非晶合金的晶化行为及其电化学腐蚀特性研究

采用单辊急冷法制备了57.5Ni-24.5Fe-14.5W-3.5B(质量分数,%)非晶薄带,并在不同温度下进行退火。用DSC和XRD分析了非晶薄带的晶化行为及析出相的演变过程;用电化学极化曲线及电化学阻抗法研究了试样在3.5%NaCl溶液中的电化学腐蚀行为;用SEM和EDS分析了试样腐蚀后的表面显微形貌及成分。结果表明:该非晶薄带的晶化过程分为3步,其晶化温度约为430,470和700℃;退火试样的耐腐蚀性整体优于非晶合金样,部分晶化试样的抗电化学腐蚀性能优于完全晶化试样;500℃退火试样表面形成致密钝化膜,抗腐蚀性能优异,而非晶薄带和720℃退火试样形成的钝化膜不稳定,易被点蚀和局部腐蚀。     

新型铁基(FeCo)73.5Cu1Nb3(SiB)22.5非晶合金晶化过程的X射线研究

用X射线衍射方法研究了(FeCo)73．5Cu1Nb3(SiB)22．5非晶合金在不同温度退火的晶化行为及晶格常数的变化。500℃退火时，在非晶基体中析出α-Fe(Si)(bcc)相，620℃退火时仍没有新相出现，680℃退火后的Fe3B、Fe23B6化合物中含有Si、Nb。α-Fe(Wi)相的晶格常数α0随退火温度的升高先减小后增大，在620℃时最小为α0=0．2836nm，在退火过程中，晶化相的结构不随外加磁场发生变化。热磁曲线表明：合金淬火非晶态时的Curie温度Tc=330℃；α-Fe(Si)(bee)相的晶化温度Tx=516℃，Curie温度Tc=640℃。     

TiO2/SiOx core-shell nanowires generated by heating the multilayered substrates

By heating Au/TiN/Si substrates, we fabricated TiO₂/SiO_x core-shell nanowires. By changing the thickness of predeposited Au layers, we demonstrated that the thickness of the Au layer needs to be optimized to obtain nanowires. High-resolution transmission electron microscopy image, X-ray diffraction spectrum, and selected area electron diffraction pattern coincidentally revealed that the resultant core nanowires had a tetragonal rutile structure of TiO₂, and the shell was comprised of amorphous SiO_x. The dominant growth mechanism was a base-growth mode, in which Au played a catalytic role, resulting in morphological changes with variation of the Au layer thickness. The TiO₂/SiO_x core-shell nanowires exhibited a broad photoluminescence emission band, which comprised four peaks centered at 1.54, 2.34, 2.67, and 2.99 eV, respectively. We expected that the 1.54 eV- and 2.34 eV-centered peaks arised from the TiO₂ core, whereas the 2.67 eV- and 2.34 eV-peaks were ascribed to both the TiO₂ core and the SiO_x shell.     

Annealing-induced enhancement of ferromagnetism in SnO2-core/Cu-shell coaxial nanowires

In this study, we have coated tin oxide (SnO₂) nanowires with a Cu shell layer via the sputtering method and subsequently investigated the effects of thermal annealing. The annealing-induced changes in morphologies, microstructures, and compositions of the resulting core-shell nanowires were characterized by using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and energydispersive X-ray spectroscopy (EDX). The Cu shell layers were agglomerated to form clusters, which were mainly comprised of the Cu₂O phase. For the first time, a hysteresis loop indicating weak ferromagnetism was observed from the pure SnO₂ nanowires. Both the coercivity and the retentivity in the hysteresis loop were slightly increased by Cu-sputtering, indicating a very slight enhancement of ferromagnetism. Also, the ferromagnetic behavior was significantly enhanced by thermal annealing. We discuss the possible mechanisms of annealing-induced enhancement of ferromagnetism in the SiO₂/Cu core-shell nanowires, which include the generation of Cu₂O phase, Cu-doping into the SnO₂ lattice, and the generation of oxygen vacancies in SnO₂ core nanowires.     

Formation and thermal stability of amorphous Ni-Mo-P alloys

The experimental researches on the chemical deposition of Ni-Mo-P amorphous alloys were carried out by adding Na2 MoO4 into acidic solutions. The optimum technology conditions were obtained by orthogonal design experiments. The structures and the relationship between compositions and their thermal stability were studied by energy spectrum (EC), scanning electron micrograph and X-ray diffraction spectrum. Compared with Ni-P amorphous alloys, the Ni-Mo-P amorphous alloys have high crystallization temperature and thermal stability, and the hardness reaches its peak when the annealing temperature is 500 ℃. With the increase of the heat treatment temperature, the surface morphology of the alloys changes.     

磁控溅射和退火制备ZnO/SiO2复合薄膜

采用射频磁控溅射和退火处理的方法在单晶硅衬底上制备了ZnO/SiO2复合薄膜,利用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)和接触角测量等测试手段研究溅射气压、溅射功率、氧氩比和退火温度等对复合薄膜成分组成、组织结构及润湿性能的影响。研究表明,复合薄膜中主要有ZnO、SiO2、Zn2SiO4 3种物相,且分别以六方纤锌矿结构、无定形态和硅锌矿型等形式存在。随着溅射和退火工艺的改变,复合薄膜的接触角在41°～146°间变化,组织形态由颗粒状向纳米竹叶状变化。溅射气压0.5 Pa,溅射功率120 W,氧氩比(O2∶Ar)为0∶30,退火温度为700℃的条件下获得具有六方纤锌矿结构的ZnO纳米组织,该组织呈现出竹叶状,在薄膜表面交错排列形成了无序多空隙的微观形貌,使复合薄膜具有超疏水性,接触角为146°。     

Generation of Zn2SiO4 Nanocrystallites in a Shell of ZnO/SiOx Core-Shell Nanowires to Change Photoluminescence Properties

This study addresses the annealing effects of ZnO/SiO_x core-shell nanowire optical properties, in terms of Zn₂SiO₄ crystallite generation. At 700 °C, the integrated PL intensity of deep-level emission was increased by annealing. With regard to UV emission, free exciton (FX) peak intensity was reduced and the ratio of FX to non-FX peak intensities increased as annealing temperature was increased. These annealing induced changes, including the enhancement of deep-level emission and suppression of FX emission, are mainly related to the generation of Zn₂SiO₄ crystallites. Transmission electron microscopy revealed that Zn₂SiO₄ crystallites were formed inside the SiO_x shell layer.     

纳米晶(FeCo)78Nb6B15Cu1合金晶化过程及其磁特性研究

采用熔体快淬法制备(FeCo)78Nb6B15Cu1非晶薄带,通过DSC测试薄带的晶化特性,并据此在400,500,700和750℃进行1h退火处理。用XRD和SEM分析薄带在不同退火温度下的晶化行为,并用VSM测试薄带与粉体的静态磁参数。结果表明:对于固定成分的Hitperm合金,选择合适的退火温度,可控制晶粒大小和晶相比例。由于晶粒表面无序磁矩含量的变化,导致材料比饱和磁化强度发生变化,同时更小的纳米晶粒对降低矫顽力有利。由于淬态引入的微量结晶,薄带存在表面晶化现象,这在一定程度上会恶化材料的静态磁特性。     

退火温度对银包铜丝材界面和力学性能的影响

采用固液浇注和拉拔制备了银包铜复合细丝,研究了不同退火温度对界面及力学性能的影响、反复弯曲载荷条件下材料结合性能与材料硬度及界面区域微观组织的变化规律。利用光学显微镜、扫描电镜和X射线能量色散谱,研究了界面区域的微观形貌、元素分布与界面结合性能的关系。结果表明:两侧沿界面扩散区域其宽度随退火温度升高而增加。在400~500℃,保温60 min真空热处理,界面具有良好的结合性能。     

Cu互连中Ta-Si-N/Zr阻挡层热稳定性的研究

用射频反应磁控溅射的方法在Si(100)衬底和Cu膜间制备Ta-Si-N(10 nm)/Zr(20 nm)双层结构的扩散阻挡层.Cu/Ta-Si-N/Zr/Si样品在高纯氮气的保护下从600至800℃退火1 h.通过四探针电阻测试仪(FPP)、SEM、XRD和AES研究Cu/Ta-Si-N/Zr/Si系统在退火过程中的热稳定性.结果表明:沉积到Zr膜上的Ta-Si-N表面平坦,为典型的非晶态结构;Cu/Ta-Si-N/Zr/Si样品650℃以上退火后Zr原子扩散到Si中形成的ZrSi2能有效地降低Ta-Si-N与Si之间的接触电阻;Ta-Si-N/Zr阻挡层750℃退火后仍能有效地阻止Cu的扩散.     

热处理温度对非晶晶化法制备ZrO2-Mullite纳米复相陶瓷结构与力学性能的影响

采用非晶原位晶化法从Si-Al-Zr-O(SAZ)系非晶中制备ZrO2-mullite纳米复相陶瓷.用XRD、IR和SEM技术对前驱体非晶以及晶化后试样进行表征,并着重研究热处理温度对ZrO2-mullite纳米复相陶瓷结构与力学性能的影响.结果表明,前驱体SAZ非晶经960℃热处理开始析出t-ZrO2晶体,1000℃时莫来石晶相形成.试样经低温950～1000℃和高温1100～1250℃梯度热处理后,t-ZrO2、mullite成为主晶相,同时生成c-SiO2.其中低温阶段的核化温度对陶瓷试样的显微结构和断裂韧性产生重大影响.当核化温度由950升至1000℃时,纳米颗粒明显增大,断裂韧性急剧下降;而高温阶段的晶化温度对力学性能影响相对较小.随着晶化温度的升高,试样的断裂韧性和抗弯强度均先略有增加随后下降.试样经950℃核化、1150℃晶化后取得最佳力学性能:断裂韧性5.13 MPa·m1/2和抗弯强度521 MPa.     

Solution-based synthesis of ZnO nanoparticle/CdS nanowire heterostructure

The heterostructure of ZnO nanoparticle (NP)/CdS nanowire (NW) was successfully fabricated by a two-step chemical solution method. The first, CdS nanowires were synthesized by a simple solvothermal route. The second, ZnO nanoparticles were grown on the surface of CdS nanowires in a chemical solution of Zn(CH₃COO)₂·2H₂O and anhydrous ethanol at 200 °C. The heterostructure of synthesized ZnO NP/CdS NW was characterized by transmission electron microscopy (TEM). The effects of reaction conditions, such as different reaction time of CdS nanowires synthesized and deposition reaction time were investigated. Moreover, the formation mechanism of the ZnO NP/CdS NW heterostructure has been phenomenologically discussed.