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Gold nanoparticle synthesis using the thermophilic bacterium Thermus scotoductus SA-01 and the purification and characterization of its unusual gold reducing protein 利用嗜热细菌Thermus scotoductus SA-01合成金纳米颗粒及其不同寻常的金还原蛋白的纯化和表征
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-08-06 DOI: 10.1007/s13404-014-0147-8
Mariana Erasmus, Errol Duncan Cason, Jacqueline van Marwijk, Elsabé Botes, Mariekie Gericke, Esta van Heerden

Nanoparticles are very important materials for implementing nanotechnology in diverse areas and are abundant in nature as living organisms operate at a nanoscale. As nanoparticles exhibit interesting size- and shape-dependent physical and chemical properties, the synthesis of uniform nanoparticles with controlled sizes and shapes is of great importance. Nanoparticles are the end products of a wide variety of physical, chemical and biological processes, some of which are novel and radically different and others of which are quite commonplace. The ability to produce nanoparticles with specific shapes and controlled sizes could result in interesting new applications that can potentially be utilized in areas such as optics, electronics and the biomedical field. In the present study, we have demonstrated the ability of the thermophilic bacterium Thermus scotoductus SA-01 to synthesize gold nanoparticles and determined the effect of the physico-chemical parameters on particle synthesis. Furthermore, a protein purified from this bacterium is shown to be capable of reducing HAuCl4 to form elemental nanoparticles in vitro. The protein was purified to homogeneity and identified through N-terminal sequencing as an ABC transporter, peptide-binding protein. It is speculated that this protein reduces Au(III) through an electron shuttle mechanism involving a cysteine disulphide bridge. Through manipulation of physico-chemical parameters, it was possible to vary nanoparticles in terms of number, shape and size. This is the first report of a transporter protein from a thermophile with the ability to produce nanoparticles in vitro thus expanding the limited knowledge around biological gold nanoparticle synthesis.

纳米粒子是在不同领域实现纳米技术的非常重要的材料,并且在自然界中丰富,因为生物体在纳米尺度上运作。由于纳米颗粒表现出有趣的大小和形状依赖的物理和化学性质,合成具有控制大小和形状的均匀纳米颗粒是非常重要的。纳米粒子是各种物理、化学和生物过程的最终产物,其中一些是新颖的、完全不同的,而另一些则相当普遍。生产具有特定形状和控制尺寸的纳米颗粒的能力可能会导致有趣的新应用,可以在光学,电子和生物医学领域等领域得到潜在的利用。在本研究中,我们证明了嗜热细菌Thermus scotoductus SA-01合成金纳米颗粒的能力,并确定了物理化学参数对颗粒合成的影响。此外,从这种细菌中纯化的蛋白质被证明能够在体外还原HAuCl4形成元素纳米颗粒。通过n端测序鉴定该蛋白为ABC转运蛋白、肽结合蛋白。推测该蛋白通过涉及半胱氨酸二硫桥的电子穿梭机制还原Au(III)。通过操纵物理化学参数,可以改变纳米颗粒的数量、形状和大小。这是第一个来自嗜热菌的转运蛋白具有在体外产生纳米颗粒的能力的报道,从而扩大了关于生物金纳米颗粒合成的有限知识。
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引用次数: 25
Phase diagram of Au–Al–Pd at 500 °C 500℃时Au-Al-Pd的相图
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-07-26 DOI: 10.1007/s13404-014-0146-9
Jyun Lin Li, Pei Jen Lo, Ming Chi Ho, Rick Yu, Ker-Chang Hsieh

The isothermal phase diagram of Au–Al–Pd at 500?°C was constructed using diffusion couples and equilibrated bulk alloys. Electron microprobe analyses were used to determine the phase compositions and phase relationships. Thirteen three-phase equilibria and two ternary phases (T1 and T2) were identified in this study. Phase T1 contained 37?at% Au, 26?at% Pd, and 37?at% Al. Phase T2 contained 44?at% Au, 24?at% Pd, and 32?at% Al. The Au solubility in the Al3Pd2, AlPd, and AlPd2 phases were 6, 15, and 34?at%, respectively. The Pd solubility in the AuAl2, Au2Al, Au8Al3, and Au4Al phases were 5, 10, 13, and 3?at%, respectively.

500℃时Au-Al-Pd的等温相图用扩散偶和平衡体合金构建了°C。用电子探针分析确定了相组成和相关系。本研究确定了13个三相平衡和2个三元相(T1和T2)。第1期含有37?在% Au, 26?在% Pd和37?T2相含有44?在% Au, 24?在% Pd和32?Au在Al3Pd2、AlPd和AlPd2相中的溶解度分别为6、15和34?分别在%。钯在AuAl2、Au2Al、Au8Al3和Au4Al相中的溶解度分别为5、10、13和3?分别在%。
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引用次数: 1
Gold etching for microfabrication 微加工用金蚀刻
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-05-11 DOI: 10.1007/s13404-014-0143-z
T. A. Green

The etching of gold is a key enabling technology in the fabrication of many microdevices and is widely used in the electronic, optoelectronic and microelectromechanical systems (MEMS) industries. In this review, we examine some of the available methods for patterning gold thin films using dry and wet etching techniques. Dry methods which utilise reactive ion etching (RIE) have a number of important advantages over other methods, but the low volatility of gold etch products has made the development of suitable processes problematic. More recently, the adoption of high-density plasma reactors with optimised chlorine-based chemistries has allowed improved processes to be developed, and etching in hydrogen plasmas also shows promise. Wet etching methods for gold have also been critically reviewed. Traditionally, iodine- and cyanide-based etch processes have been used, but in the last decade, a number of alternative etchants have been studied. Of particular interest is the recent development of a range of novel non-aqueous-based gold etchants, and the suitability of these etchants for microfabrication is assessed.

金的蚀刻是制造许多微器件的关键使能技术,广泛应用于电子、光电和微机电系统(MEMS)行业。在这篇综述中,我们研究了一些可用的方法来图像化金薄膜使用干法和湿法蚀刻技术。利用反应离子蚀刻(RIE)的干燥方法比其他方法有许多重要的优点,但是金蚀刻产品的低挥发性使得开发合适的工艺成为问题。最近,高密度等离子体反应器的采用优化了氯基化学物质,使得改进的工艺得以发展,氢等离子体蚀刻也显示出前景。对金的湿法蚀刻方法也进行了评述。传统上,以碘和氰化物为基础的蚀刻工艺已经被使用,但在过去的十年中,一些替代蚀刻剂已经被研究。特别令人感兴趣的是最近开发的一系列新型非水基金蚀刻剂,并评估了这些蚀刻剂对微细加工的适用性。
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引用次数: 103
Room temperature evolution of gold nanodots deposited on silicon 硅上沉积金纳米点的室温演化
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-05-09 DOI: 10.1007/s13404-014-0142-0
C. Garozzo, A. Filetti, C. Bongiorno, A. La Magna, F. Simone, R. A. Puglisi

In this work, the morphological and structural evolution of gold nanodots deposited on Si substrates has been monitored for 2.4?×?103?h. Gold nanodots on Si are of great scientific interest because they can be used in numerous ways, for example as subwavelength antennas in plasmonics, as electrical contacts in nanometric devices, or as catalysts for the formation of quasi-1dimensional nanostructures. Their characteristics have been studied in a very large number of papers in literature, and among the several aspects, it is known that continuous Au films peculiarly interact with Si by interdiffusion even at room temperature. It would be expected that also small nanostructures could undergo to an interdiffusion and consequent modifications of their structure and shape after aging. Despite the cruciality of this topic, no literature papers have been found showing a detailed morphological and structural characterization of aged Au nanodots. Au nanoparticles have been deposited by sputtering on Si and stored in air at temperature between 20 and 23?°C and humidity of about 45?%, simulating the standard storage conditions of most of the fabrication labs. The morphological and structural characterizations have been performed by bright field transmission electron microscopy (TEM). A specific procedure has been used in order to avoid any modification of the material during the specimen preparation for the TEM analysis. A digital processing of the TEM images has allowed to get a large statistical analysis on the particles size distribution. Two different types of nanoparticles are found after the deposition: pure gold crystalline nanodots on the Si surface and gold amorphous nanoclusters interdiffused into the Si subsurface regions. While the nanodots preserve both morphology and structure all over the time, the amorphous agglomerates show an evolution during aging in morphology, structure, and chemical phase.

在这项工作中,我们监测了沉积在Si衬底上的金纳米点在2.4 × 103小时内的形态和结构演变。硅上的金纳米点具有很大的科学意义,因为它们可以有多种用途,例如用作等离子体中的亚波长天线,用作纳米器件中的电触点,或用作准一维纳米结构形成的催化剂。文献中对它们的特性进行了大量的研究,在这几个方面中,已知连续的Au薄膜即使在室温下也与Si具有特殊的相互扩散作用。预计小纳米结构在时效后也会发生相互扩散,从而导致其结构和形状的改变。尽管这一课题至关重要,但还没有文献论文显示老化金纳米点的详细形态和结构表征。金纳米颗粒通过溅射沉积在硅上,并在20 - 23℃的温度下储存在空气中。°C,湿度约45?%,模拟大多数制造实验室的标准存储条件。通过亮场透射电镜(TEM)对其进行了形态和结构表征。为了避免在TEM分析的样品制备过程中对材料进行任何修改,使用了特定的程序。对透射电镜图像进行数字处理,可以对颗粒尺寸分布进行大量的统计分析。沉积后发现两种不同类型的纳米颗粒:在Si表面的纯金晶体纳米点和在Si亚表面区域相互扩散的金非晶纳米团簇。随着时间的推移,纳米点的形貌和结构都保持不变,而非晶团块在老化过程中形貌、结构和化学相都发生了变化。
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引用次数: 4
Probing the surface oxidation of chemically synthesised gold nanospheres and nanorods 探测化学合成金纳米球和纳米棒的表面氧化
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-05-03 DOI: 10.1007/s13404-014-0141-1
Blake J. Plowman, Nathan Thompson, Anthony P. O’Mullane

In this study, the electrochemical behaviour of commercially available gold spheres and rods stabilised by carboxylic acid and cetyl trimethyl ammonium bromide (CTAB) moieties, respectively, are investigated. The cyclic voltammetric behaviour in acidic electrolyte is distinctly different with the nanorods exhibiting unusual oxidative behaviour due to an electrodissolution process. The nanospheres exhibited responses typical of a highly defective surface which significantly impacted on electrocatalytic activity. A repetitive potential cycling cleaning procedure was also investigated which did not improve the activity of the nanorods and resulted in deactivating the gold spheres due to decreasing the level of surface defects.

在这项研究中,研究了市售金球和金棒的电化学行为,分别由羧酸和十六烷基三甲基溴化铵(CTAB)稳定。酸性电解液中的循环伏安行为与纳米棒由于电溶解过程而表现出异常的氧化行为明显不同。纳米球表现出典型的高缺陷表面反应,显著影响电催化活性。我们还研究了一种重复的电位循环清洗程序,该程序并没有提高纳米棒的活性,而是由于降低了表面缺陷的水平而导致金球失活。
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引用次数: 7
Effect of gold addition on the microstructure, mechanical properties and corrosion behavior of Ti alloys 添加金对钛合金组织、力学性能和腐蚀行为的影响
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-04-16 DOI: 10.1007/s13404-014-0138-9
Yong-Ryeol Lee, Mi-Kyung Han, Min-Kang Kim, Won-Jin Moon, Ho-Jun Song, Yeong-Joon Park

We performed a systematic investigation of the Ti–xAu (x?=?5, 10, 15, 20, and 40?wt%) alloys to assess the effect of addition of element Au on the microstructure, mechanical properties, and corrosion behavior of commercially pure titanium (cp-Ti). The phase and microstructure were characterized using X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results indicated that the Ti–xAu alloys containing up to 15?wt% Au showed a hexagonal close-packed α-Ti structure, whereas the Ti–xAu alloys containing more than 20?wt% Au were mainly composed of the α-Ti phase and Ti3Au intermetallic phase. We also investigated the effect of alloying element Au on the mechanical properties (including Vickers hardness and modulus) and corrosion behavior of Ti–xAu binary alloys. The addition of gold to Ti improved its hardness. Electrochemical results showed that the Ti–xAu alloys exhibited improved corrosion resistance than cp-Ti.

我们对Ti-xAu (x?=?)5、10、15、20和40?wt%)合金,以评估添加元素Au对商业纯钛(cp-Ti)的显微组织、机械性能和腐蚀行为的影响。采用x射线衍射(XRD)、光学显微镜、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对其物相和微观结构进行了表征。结果表明,Ti-xAu合金中含有15?wt% Au表现为六方密排α-Ti结构,而Ti-xAu合金含20?wt% Au主要由α-Ti相和Ti3Au金属间相组成。我们还研究了合金元素Au对Ti-xAu二元合金力学性能(包括维氏硬度和模量)和腐蚀行为的影响。在钛中加入金提高了它的硬度。电化学结果表明,Ti-xAu合金的耐蚀性优于cp-Ti。
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引用次数: 20
Evolution and investigation of copper and gold ball bonds in extended reliability stressing 扩展可靠性应力下铜和金球键的演化与研究
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2014-03-29 DOI: 10.1007/s13404-014-0135-z
C. L. Gan, F. C. Classe, B. L. Chan, U. Hashim

This paper discusses the microstructure evolution of copper (Cu) and gold (Au) ball bonds after various extended reliability stresses such as biased highly accelerated temperature and humidity test (HAST), unbiased highly accelerated temperature and humidity test (UHAST), temperature cycling (TC), and high temperature storage life (HTSL) in BGA package. Objective of this study is to study the microstructure evolution and changes after long hours and long cycles of component reliability stressing and its predicted failure mechanisms and to determine the long-term reliability comparison with combination of bonding wires in HAST, UHAST, and TC. Secondary electron microscopy (SEM) and energy dispersive X-ray (EDX) have been carried out to understand the respective microstructure of failed samples in HAST, UHAST, TC, and HTSL long-term reliability failures. Respective failure mechanisms of copper and gold ball bonds carrion under HAST and UHAST, ball bond lifting in TC and HTSL have been analyzed and proposed. The evolution of surface morphology, including copper and gold ball bond micro cracking, gold ball bond Kirkendall microvoiding and intermetallic compound (IMC) formation, was studied in FBGA package with copper and gold ball bonds during various reliability stresses. Biased HAST, UHAST, TC, and HTSL mechanisms were proposed to explain the observed morphological changes and the resulting ball bond wear out modes after extended reliability stresses. Weibull reliability analyses have been established to compare the performance of copper and gold ball bonds under humid and dry environmental tests.

本文讨论了BGA封装中铜(Cu)和金(Au)球键在经过偏置高加速温湿度测试(HAST)、无偏置高加速温湿度测试(UHAST)、温度循环(TC)和高温储存寿命(HTSL)等多种扩展可靠性应力后的微观结构演变。本研究的目的是研究构件在长时间、长周期的可靠性应力作用下的微观结构演变和变化及其预测的失效机制,并确定在HAST、UHAST和TC中结合焊线的长期可靠性比较。利用二次电子显微镜(SEM)和能量色散x射线(EDX)分析了HAST、UHAST、TC和HTSL长期可靠性故障中失效样品的微观结构。分析并提出了铜和金球键在高低温和高低温条件下的腐蚀破坏机制,以及高温和高温条件下的球键提升机制。研究了含铜和金球键的FBGA封装在不同可靠性应力下表面形貌的演变,包括铜和金球键的微裂纹、金球键的Kirkendall微空洞和金属间化合物(IMC)的形成。提出了偏置的HAST、UHAST、TC和HTSL机制来解释在延长可靠性应力后观察到的形态变化和由此产生的球键磨损模式。建立了威布尔可靠性分析来比较铜和金球键在潮湿和干燥环境下的性能。
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引用次数: 21
Highlights from recent literature 近期文献亮点
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2013-12-14 DOI: 10.1007/s13404-013-0132-7
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引用次数: 0
Soldering of non-wettable Al electrode using Au-based solder 用金基焊料焊接不湿性铝电极
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2013-12-12 DOI: 10.1007/s13404-013-0130-9
Fengqun Lang, Hiroshi Nakagawa, Hiroshi Yamaguchi

In manufacturing three-dimensional SiC power modules, the Al electrode of SiC power devices should be soldered to the substrate. However, the Al electrode is difficult to be bonded by a solder due to the naturally formed aluminum oxide on it. In this paper, we describe an effective approach for soldering the non-wettable Al electrode by fabricating a Au-stud bump in the Al electrode together with a Au-20?wt% Sn or Au-12?wt% Ge solder. The soldering initiated at the Au bump and spreaded on the Al electrode. The soldering featured as reactive wetting, realized by the reaction of liquid Au in the Au-base solder and the Al electrode. The activation energy of the Au-20?wt% Sn soldering the Al electrode was Q?=?159?kJ/mol. A continuous Au4Al layer formed at the Au-20?wt% Sn bond interface. The shear strength exceeded 60?MPa, ~1 order magnitude higher than the required shear strength. For the bond with Au-12?wt% Ge solder on the Al electrode with a Au bump, the liquid Au-12?wt% Ge solder reacted with the solid Al electrode and formed a Au-Ge-Al solid solution after solidification. The shear strength of the Au-12?wt% Ge solder on the Al electrode with a Au bump was beyond 50?MPa. Little electrical characteristics of the SiC-SBD changed after the Al electrode was bonded to a circuit substrate using this technology.

在制造三维SiC功率模块时,需要将SiC功率器件的Al电极焊接到衬底上。然而,由于铝电极上自然形成的氧化铝,它很难被焊料粘合。在本文中,我们描述了一种有效的焊接不可湿性铝电极的方法,即在铝电极上制造一个au螺柱凸起和一个Au-20?wt% Sn或Au-12?wt% Ge焊料。焊接在Au凸起处开始并扩展到Al电极上。该焊具有反应润湿的特点,是通过液态Au在Au基焊料和Al电极中的反应来实现的。Au-20的活化能?焊接Al电极的wt% Sn为Q = 159 kJ/mol。在Au-20?wt% Sn键界面。抗剪强度超过60?MPa,比要求的抗剪强度高~1个数量级。Au-12的键呢?在带有Au凸起的Al电极上焊料wt% Ge,液态Au-12?wt% Ge焊料与固体Al电极发生反应,凝固后形成Au-Ge-Al固溶体。Au-12的抗剪强度?有Au凸起的Al电极上的wt% Ge焊料大于50mpa。使用该技术将铝电极粘合到电路衬底后,SiC-SBD的电特性几乎没有变化。
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引用次数: 4
Nanostructured and nanopatterned gold surfaces: application to the surface-enhanced Raman spectroscopy 纳米结构和纳米图案金表面:在表面增强拉曼光谱中的应用
IF 2.2 4区 工程技术 Q2 Chemistry Pub Date : 2013-12-11 DOI: 10.1007/s13404-013-0127-4
A. Bouvrée, A. D’Orlando, T. Makiabadi, S. Martin, G. Louarn, J. Y. Mevellec, B. Humbert

Surface-enhanced Raman spectroscopy (SERS) has enormous potential for a range of applications where high sensitivity needs to be combined with good discrimination between molecular targets. However, the SERS technique has trouble finding its industrial development, as was the case with the surface plasmon resonance technology. The main reason is the difficulty to produce stable, reproducible, and highly efficient substrates for quantitative measurements. In this paper, we report a method to obtain two-dimensional regular nanopatterns of gold nanoparticles (AuNPs). The resulting patterns were evaluated by SERS. Our bottom-up strategy was divided into two steps: (a) nanopatterning of the substrate by e-beam lithography and (b) electrostatic adsorption of AuNPs on functionalized substrates. This approach enabled us to highlight the optimal conditions to obtain monolayer, rows, or ring of AuNPs, with homogeneous distribution and high density (800 AuNPs/μm2). The nanostructure distributions on the substrates were displayed by scanning electron microscopy and atomic force microscopy images. Optical properties of our nanostructures were characterized by visible extinction spectra and by the measured enhancements of Raman scattering. Finally, we tried to demonstrate experimentally that, to observe a significant enhancement of SERS, the gold diffusers must be extremely closer. If electron beam lithography is a very attractive technique to perform reproducible SERS substrates, the realization of pattern needs a very high resolution, with distances between nanostructures probably of less than 20?nm.

表面增强拉曼光谱(SERS)在需要高灵敏度和良好的分子靶标区分相结合的应用中具有巨大的潜力。然而,SERS技术很难找到它的工业发展,就像表面等离子体共振技术一样。主要原因是难以生产稳定、可重复和高效的底物用于定量测量。在本文中,我们报道了一种获得金纳米颗粒(AuNPs)二维规则纳米图案的方法。产生的模式通过SERS评估。我们的自下而上策略分为两个步骤:(a)通过电子束光刻对衬底进行纳米图案化,(b)在功能化衬底上静电吸附AuNPs。这种方法使我们能够突出获得单层,行或环状AuNPs的最佳条件,具有均匀的分布和高密度(800 AuNPs/μm2)。通过扫描电子显微镜和原子力显微镜图像显示了衬底上的纳米结构分布。我们的纳米结构的光学特性通过可见消光光谱和测量的拉曼散射增强来表征。最后,我们试图通过实验证明,为了观察到SERS的显著增强,金扩散器必须非常接近。如果电子束光刻是一种非常有吸引力的技术来执行可重复的SERS衬底,那么图案的实现需要非常高的分辨率,纳米结构之间的距离可能小于20nm。
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引用次数: 16
期刊
Gold Bulletin
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