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Paramagnetic Behaviour of Silver Nanoparticles Generated By Paramagnetic behaviour of silver nanoparticles generated by decomposition of silver oxalate Hoa Le Trong, Kateryna Kiryukhina, Michel Gougeon, Valérie Baco-Carles, Frédéric Courtade, Sophie Dareys, Philippe Tailhades To cite this version: Hoa Le Trong, Kateryna Kiryukhina, Michel Gougeon, Valérie Baco-Carles, Frédéric Courtade, et al.. Paramagnetic behaviour of silver nanoparticles generated by decomposition of silver oxalate. Solid State Sciences, Elsevier, 2017, vol. 69, pp. 44-49. 10.1016/j.solidstatesciences.2017.05.009. hal-01750400 HAL Id: hal-01750400 https://hal.archives-ouvertes.fr/hal-01750400 Submitted on 29 Mar 2018 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Open Archive TOULOUSE Archive Ouverte (OATAO) OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible. This is an author-deposited version published in : http://oatao.univ-toulouse.fr/ Eprints ID : 19787 To link to this article : DOI:10.1016/j.solidstatesciences.2017.05.009 URL : http://dx.doi.org/10.1016/j.solidstatesciences.2017.05.009 To cite this version : Le Trong, Hoa and Kiryukhina, Kateryna and Gougeon, Michel and Baco-Carles, Valérie and Courtade, Frédéric and Dareys, Sophie and Tailhades, Philippe Paramagnetic behaviour of silver nanoparticles generated by decomposition of silver oxalate. (2017) Solid State Sciences, vol. 69. pp. 44-49. ISSN 1293-2558 Any correspondence concerning this service should be sent to the repository administrator: [email protected] Paramagnetic behaviour of silver nanoparticles generated by decomposition of silver oxalate Hoa Le Trong a, b, c, Kateryna Kiryukhina a, d, Michel Gougeon a, b, Valerie Baco-Carles a, b, * Fred eric Courtade d, Sophie Dareys d, Philippe Tailhades a, b, a Universite de Toulouse, UPS, INPT, Institut Carnot Chimie Balard Cirimat, 118, route de Narbonne, F-31062 Toulouse Cedex 9, France b CNRS, Institut Carnot Chimie Balard Cirimat, F-31062 Toulouse, France c Ho Chi Minh City University of Science, Vietnam National University Ho Chi Minh City, 227 Nguyen Van Cu Q 5, 750000 Ho Chi Minh City, Viet Nam d Centre National d’Etudes Spatiales, CNES, 18 Avenue Edouard Belin, 31 401 Toulouse Cedex 09, France a b s t r a c t Silver oxalate Ag2C2O4, was already proposed for soldering applications, due to the formation when it is decomposed by a heat treatment, of highly sinterable silver nanoparticles. When slowly decomposed at low temperature (125 C), the oxalate leads however to silver nanoparticles isolated from each other. As soon as these nanoparticles are formed, the magnetic susceptibility at room temperature increases from À3.14 10À7 emu.OeÀ1.gÀ1 (silver oxalate) up to À1.92 10À7 emu.OeÀ1.gÀ1 (metallic silver). At the end of the oxalate decomposition, the conventional diamagnetic behaviour of bulk silver, is observed from room temperature to 80 K. A diamagnetic-paramagnetic transition is however revealed below 80 K Keywords: Silver oxalate leading at 2 K, to silver nanoparticles with a positive magnetic susceptibility. This original behaviour, Silver nanoparticles compared to the one of bulk silver, can be ascribed to the nanometric size of the metallic particles. Paramagnetic silver Oxalate decomposition Nanocrystalline metal Soldering 1. Introduction however observed at room temperature [13,14] and theoretical studies have predicted ferromagnetism for clusters of bare noble 1.1. Magnetic properties of noble metals nanoparticles metals [15 e17]. In this work, paramagnetic properties are experi- mentally observed for the first time, in bare nanoparticles of silver Bulk copper, silver or gold, display diamagnetic properties. resulting from the controlled thermal decomposition of silver Nanoparticles of such metals capped by surfactants or embedded in oxalate. inorganic matrices, can however be paramagnetic or ferromagnetic [1e3]. Gold nanoparticles can exhibit paramagnetism. That was, for instance, observed when they are dispersed in poly-N-vinyl-2- 1.2. Metals nanoparticles for low temperature soldering pyrrolidone [4]. Gold nanoparticles functionalized by various li- gands can also be ferromagnetic [5e8]. X-ray magnetic dichroïsm From a technological point of view, metallic nanoparticles pre- (XMCD) [9], muon spin relaxation [10] and 197Au Mossbauer€ sent a growing interest for low temperature soldering applications. spectroscopy [2] have proved the direct contribution of gold to Indeed, gallium nitride based electronic chips are increasingly used ferromagnetism. XMCD has also demonstrated the ferromagnetic in power electronic systems. For space applications, their high contribution of copper and silver in thiol-capped nanoparticles [2]. power density makes the thermal management critical and re- Their saturation magnetization could be related to the strength of quires thermal investigations. Usually, they are mounted to a metal-ligand binding [11] even if that is still open to debate [12]. thermal substrate by soldering and wiring bonding steps. The sol- Ferromagnetism of uncapped gold or silver nanoparticles was dering process has to be carried out at moderate temperatures (<300 C) and low contact pressures, to avoid irreversible damages or accelerated ageing effects on electronic devices. One of the * Corresponding author. Universite de Toulouse, UPS, INPT, Institut Carnot Chimie Balard Cirimat, 118, route de Narbonne, F-31062 Toulouse Cedex 9, France. thermal challenge is consequently to replace solder (as AuSn alloy) E-mail address: [email protected] (P. Tailhades). with a new material with intrinsic higher thermal conductivity and http://dx.doi.org/10.1016/j.solidstatesciences.2017.05.009 which can be applied at moderate temperature. One way is to take solder, above 300 C [24]. A very slow decomposition carried out in benefit of the strong lowering of melting temperature alloys when between 100 and 130 C for several hours, allows also a complete the particle size of such metals is strongly reduced below 10 nm decomposition. In that instance, isolated nanoparticles of silver are [18e20]. Because the sintering generally occurs at an absolute obtained by this way. temperature close to 80% of the melting point, this decrease makes low-temperature sintering easier. 2. Materials and methods The starting oxalate powder was prepared as follow. A 1.3. Specificities of silver oxalate concentrated solution of silver nitrate (2 mol lÀ1) was reacted with oxalic acid solution (0.5 mol lÀ1) to produce a precipitate of oxalate. The silver oxalate (Ag2C2O4) is an interesting compound for such The silver nitrate (purity > 99.9%) was initially dissolved in a mounting applications, because its decomposition, already mixture of deionised water (10% vol.) and analytical grade ethylene fi described by taking into account the structural speci cities [21,22], glycol (90% vol.). Oxalic acid was dissolved in a mixture of absolute leads to silver nanoparticles according to the simple following ethyl alcohol (95% vol.) and deionised water (5% vol.). After pre- reaction: cipitation, the oxalate was separated from the liquors by centrifu- gation and washed by deionised water. This operation was repeated Ag C O /2Ag þ 2CO 2 2 4 2 five times. The oxalate was then dried at 50 C. The resulting nanoparticles have the required high sintering The silver oxalate and metallic silver were characterised by X- propensity in the range 200e300 C and the metallic silver formed ray diffraction with a Siemens D 5000 diffractometer equipped at the end of the soldering process has a high intrinsic thermal with a Brucker sol-X detector. The X-ray wavelength was that of the conductivity [23]. Moreover, the silver oxalate is easily decomposed copper Ka ray (Ka1 ¼ 0.15405 nm and Ka2 ¼ 0.15443 nm). The as illustrated by Fig. 1, which shows the spherical nanoparticles of chemical composition of the metallic powder was analysed by silver generated by a scanning electron microscope, at the end of Inductively Coupled Plasma e Mass Spectroscopy (ICP-MS). The several scans. The silver nanoparticles are arranged according to a samples were also investigated by two scanning electron micro- regular lattice, which corresponds to the periodicity of the electron scopes (SEM), a SEM ZEISS Ultra 55 and a field emission gun SEM beam modulation. This periodicity is close to 76 nm for the images JEOL JSM 6700 F equipped with an Energy-dispersive X-ray spec- (b), (c) and (d) in Fig.1. Silver oxalate also decomposes in air, in inert troscopy (EDS) system of Princeton Gamma Tech. or reducing atmosphere, by heating it above 100 C or by applying The magnetic properties were measured with a vibrating sam- mechanical stresses. Additionally, because the decomposition of ple magnetometer (VSM Quantum Design Versalab) and a SQUID silver oxalate is highly exothermic, a proper heating procedure magnetometer MPMSXL 7 from Quantum design. The decomposi- provides void mitigation in the solder joint. This joint having a high tion of the silver oxalate was carried out inside the VSM, which is thermal conductivity, is obtained without heating the chip to equipped with a system of heating up to 400 K. For such Fig. 1. Silver oxalate particles observed by scanning microscopy. (a): The lower part of the sample in image (a) was originally scanned for 30 min by a 300 pA and 3 kV electron beam. The scanned region was then enlarged and an image was recorded after a few additional scans lasting less than 1 min. The image obtained clearly shows two regions. At the bottom there is a texturing induced by the pulsed energy of the electron beam, which is responsible of the partial decomposition of the oxalate.
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