2016 International Conference on Advanced Manufacture Technology and Industrial Application (AMTIA 2016) ISBN:

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1 2016 International Conference on Advanced Manufacture Technology and Industrial Application (AMTIA 2016) ISBN: Preparation and Characterization of Ultra-Fine Silver Powder by Hydrogen Peroxide and Ascorbic Acid Reduction Xiao-he BAI, Peng ZHANG and Zhi-dan LIN * Department of Materials Science and Engineering, College of Science and Engineering, Jinan University, Guangzhou , PR China *Corresponding author Keywords: Ascorbic acid, Hydrogen peroxide, Morphologies, Coral clusters. Abstract. In this work, using chemical reduction method, we synthesized silver particles with different sizes and morphologies by simply changing the proportion of the associative reducing agents. More specifically, when the reducing agent is ascorbic acid, the morphologies of silver particles are quasi-spherical shapes, the diameter size of silver nanoparticles was in the range from 200 nm to 300 nm. When the reducing agent is hydrogen peroxide, the morphologies of silver particles are irregular bulks, the diameter size of silver nanoparticles was in the range from 1 um to 2 um. When the volume ratio of ascorbic acid (0.09M) and hydrogen peroxide (0.98M) is 1: 1, the morphologies of silver particles are unique, they are coral clusters reunited by long silver nanoplates. Introduction In recent years, as one of the most precious metal powder, Silver particles is widely used in the electronics industry because of its excellent electrical conductivity, thermal conductivity, and chemical stability[1-2]. The size and morphology of Ultra-fine silver particle directly affects the volume effect and surface effect and other characteristics, therefore, to prepare regular morphology, particle size uniformity, good dispersion of silver particles is particularly important. Preparation of silver particles include electrochemical method, chemical reduction method [3], spray decomposition method [4], laser method, hydrothermal method, microemulsion method, polyols, chemical vapor deposition method, etc.[5] But these preparation methods require precise apparatus and relatively harsh conditions, it is not suitable for mass production. Liquid phase reduction method [6-8] because of simple equipment, easy operation, low cost, and energy-saving advantages has became the main method for preparing silver particles. The reducing agents of liquid phase reduction method commonly include formaldehyde, hydrazine, glucose, sodium hypophosphite, ascorbic acid and hydrogen peroxide. During the manufacturing process, in order to prevent agglomeration of silver, it is normal to add to appropriate dispersing agents, such as gelatin, polyvinyl acetate (PVA), polyvinyl pyrrolidone (PVP), succinic acid (PAA), gum arabic, sodium citrate, and methyl cellulose, etc. Due to the steric hindrance of the macromolecule structure, the agglomeration of silver particles can not occur. The author uses liquid-phase chemical reduction method, silver ammonia solution as raw material, polyvinylpyrrolidone (PVP) as a dispersing agent and protective agent, ascorbic acid and hydrogen peroxide according to a certain proportion of complex as a reducing agent to prepare ultra-fine silver controllably. At the same time, the growth and dispersion of gold particles in the mechanism of the reaction system were studied and found that by varying the ratio of ascorbic acid and hydrogen peroxide can be prepared by a unique morphology of silver nanoparticles. Experimental Procedure Silver nitrate (pure p.a.) were provided by Tianjin Damao Chemical Reagent Factory, ascorbic acid and hydrogen peroxide were purchased from Aldrich and used as the reducing agents, Polyvinyl pyrrolidone (PVP) were provided by Tianjin Damao Chemical Reagent Factory and used as stabilizers, Deionized water was used for the preparation of mixture solution. Silver powder was obtained by reaction of silver nitrate with the mixture of hydrogen peroxide and

2 ascorbic acid. Because of different proportions of mixture, Silver powder has different morphologies, different sizes and other different characteristics. Aqueous ammonia was employed to control ph value, the temperature was kept at 30 C for 10 min to carry out the reaction, the mass of PVP having molecular weights of is 5% by the mass of silver nitrate in the reaction. Direct observation of the silver powder end termination was made by scanning electron microscopy (SEM), to reveal the shape of the particle, their diameter and size distribution. The crystal structure was characterized by X-ray diffraction. Results and Discussion In this experiment, in order to improve the conversion rate of the product, the molar ratio between AgNO 3 and Vc improves to 2: Taking into account the resistance of Ag (NH 3 ) + n dissociating into Ag +, and some H 2 O 2 also automatically break down according to 2 H 2 O 2 = 2 H 2 O + O 2, H 2 O 2 / Ag (MR) should be greater than 5. Table 1 shows the method of Vc and H 2 O 2 complexed in this work. Table 1. Solution of hydrogen peroxide and ascorbic acid complex ratio table. Group The volume of material ( ml ) AgNO 3 ( 0.15M) H 2 O 2 ( 0.98M) Vc ( 0.09M) the volume ratio of Vc solution and H 2 O 2 solution a : 0 b : 1 c : 1 d : 3 e : 1 Particle Preparation and Characterization Preparation of metal nanoparticles by chemical synthesis is divided into three stages 1) nucleation, 2) evolving into seeds from the nucleus, 3) seeds grow into nanoparticles. [9-11] seeds are the larger particles than nucleus. Once seeds generated, the basic structure of the nanoparticles is determined. In our reaction system, the reducing agents were the compound solution of ascorbic acid and hydrogen peroxide, the reducibility of Vc is moderate, H 2 O 2 is weaker, so the mixture of them actually controlled the seeding structure by Kinetics. Because of different proportions of the mixture, leading to different reaction rate with precursor, producing different kinds of crystal structure and finally producing different morphologies. Figure 1. SEM images of silver particles formed when Vc and H 2 O 2 were mixed in different ratios as reducing agent (a: all of Vc. b: the volume ratio of Vc and H 2 O 2 was 3: 1).

3 When the reducing agent was all ascorbic acid, as shown in Figure 1 a, the morphologies of silver particles were spherical shapes, the diameter size of silver particles was in the range from 200 nm to 300 nm. When the volume ratio of Vc and H 2 O 2 was 3: 1, as shown in Figure 1 b, the morphologies of silver particles were quasi-spherical shapes, particles size between nm. We can get a conclusion that adding H 2 O 2 became the shapes of particles irregular and the range of particle size more wider. When the volume ratio of ascorbic acid and hydrogen peroxide is 1: 1, as shown in Figure 2 a, the morphologies of silver particles are unique, they are coral clusters reunited by long silver nanoplates. As shown in Figure 2 b, we can observe that the long silver nanoplates are not smooth, fully growing pimple-like bumps and shorter sheet in the above. The forming of nano-crystal structure is mainly controlled by thermodynamics and dynamics, it is the result of a combination of both[12]. In dynamics, because the mixed reducing agents control the silver atoms production rates, seeds and nucleis can be closely stacked by these atoms, accompanied by the occurrence of Stacking fault phenomenon to generat sheet seeds. In terms of thermodynamics, use PVP as stabilizers in this experiment. PVP selectively adsorbed on {100} planes of silver species to prompt silver atoms deposited on the other planes,[13] it is the reason why long silver nanoplates are not smooth fully growing pimple-like bumps and shorter sheet in the above. On the other hand, because the force of combining to {100} planes of silver speciesis is not strong owing to the molecular weight of PVP is 10,000, and the shorter molecular chains of PVP MW = can not be completely wrapped in silver surfaces, a lot of seeds and formed crystals gather together leading to long sheet of silver nanoparticles reunited. a b Figure 2. SEM images of silver particles formed when Vc and H 2 O 2 were mixed in the ratio of 1:1 as reducing agent. Figure 3. SEM images of silver particles formed when Vc and H 2 O 2 were mixed in different ratios as reducing agent (a: the volume ratio of Vc and H 2 O 2 was 1: 3. b: all of H 2 O 2 ).

4 When the volume ratio of ascorbic acid and hydrogen peroxide is 1: 3, as shown in Figure 3 a, the morphologies of silver were not single, including spherical shapes, silver nanowires, and hexagonal block, the particle size has reached micron levels. When the reducing agent was all hydrogen peroxide, as shown in Figure 3 b, silver nanowires disappeared, almost are the irregular bulks, and the particle size became larger. From Figure 4, Silver powder prepared in 38.12, 44.30, and at the obvious diffraction peak corresponding to silver (111), ( 200), (220) and (311) planes, This shows that powders are elemental silver. And diffraction peaks are quite sharp, indicating a high degree of crystallinity of the silver powder. Figure 4. XRD patterns of silver nanoparticles synthesized with different volume ratios of Hydrogen peroxide solution and ascorbic acid solution. Summary In this work, using chemical reduction method, PVP as a dispersing agent, under alkaline conditions, we synthesized silver particles with different sizes and morphologies by simply changing the proportion of the associative reducing agents. Through experiments, we found that when the reducing agent is ascorbic acid, the morphologies of silver particles are quasi-spherical shapes, the diameter size of silver nanoparticles was in the range from 200 nm to 300 nm. When the reducing agent is hydrogen peroxide, the morphologies of silver particles are irregular bulks, the diameter size of silver nanoparticles was in the range from 1 um to 2 um. When the volume ratio of ascorbic acid (0.09M) and hydrogen peroxide (0.98M) is 1: 1, the morphologies of silver particles are unique, they are coral clusters reunited by long silver nanoplates. Acknowledgement This research was financially supported by Science and Technology Project of Guangdong Province (grant No. 2014B ).The project is The development of micro and nano silver paste and printable paste used in high-resolution display device.

5 References [1] Ahmed M O E, Leong W K. Colloidal silver nanoparticles stabilized by a water-soluble triosmium cluster[j]. Journal of organometallic chemistry, 2006, 691(5): [2] Zhao D, Ma L, Yang J, et al. Resent situation and development trends of silver powder and electronic paste[j]. Electronic Components and Materials, 2005, 24(6): 54. [3] Liu W, Lu J, Xu H, et al. Silver nanoparticles: Synthesis, properties, and therapeutic[j]. Drug Discovery Today, 2015,20 (5): [4] Liu Z, Liu Z, Li Q, et al. Morphology control of micro-sized spherical silver powder prepared by spray pyrolysis[j]. Chinese Journal of Nonferrous Metals, 2007, 17(1): 149. [5] Cinelli M, Coles S R, Nadagouda M N, et al. A green chemistry-based classification model for the synthesis of silver nanoparticles[j]. Green Chemistry, 2015, 17(5): [6] Liu Z, Qi X L, Wang H. Synthesis and characterization of spherical and mono-disperse micro-silver powder used for silicon solar cell electronic paste[j]. Advanced Powder Technology, 2012, 23(2): [7] Gu S, Wang W, Wang H, et al. Effect of aqueous ammonia addition on the morphology and size of silver particles reduced by ascorbic acid[j]. Powder technology, 2013, 233: [8] Li C C, Chang S J, Su F J, et al. Effects of capping agents on the dispersion of silver nanoparticles[j]. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2013, 419: [9] Wiley B, Sun Y, Chen J, et al. Shape-controlled synthesis of silver and gold nanostructures[j]. Mrs Bulletin, 2005, 30(05): [10] Lofton C, Sigmund W. Mechanisms controlling crystal habits of gold and silver colloids[j]. Advanced Functional Materials, 2005, 15(7): [11] Baletto F, Mottet C, Ferrando R. Microscopic mechanisms of the growth of metastable silver icosahedra[j]. Physical Review B, 2001, 63(15): [12] Xia Y, Xiong Y, Lim B, et al. Shape Controlled Synthesis of Metal Nanocrystals: Simple Chemistry Meets Complex Physics?[J]. Angewandte Chemie International Edition, 2009, 48(1): [13] Wiley B, Sun Y, Mayers B, et al. Shape controlled synthesis of metal nanostructures: the case of silver[j]. Chemistry A European Journal, 2005, 11(2):

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