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A novel green route for the fast combustion synthesis of silicon carbide nanofibers

Michał Soszyński ,  Błażej Laudy ,  Rafał Konopka ,  Piotr Baranowski 

Warsaw University, Department of Chemistry, Pasteura 1, Warsaw 02-093, Poland

Abstract

     It is well known that nanomaterials offer many unique and variety properties arousing great interest of researchers and give hope to the many potential applications. Silicon carbide also belongs to this type of material [1-4]. In particular, the 1-D dimensional form (nanofibers, nanowires, nanotubes) is most promising, mainly for a good electrical and mechanical properties [5-8]. There have been many attempts to produce a 1-D SiC, for example:
             - synthesis from the elements [9,10];
             - carbothermic reduction [11];
             - chemical vapor deposition [12];
             - arc, microwave or induction discharge [13];
             - NRW use as template for the growth [14];
             - laser ablation [15];
             - “hot filaments” method [16].

The above-mentioned methods and techniques of production of 1-D SiC are, however,  multi-step approaches while energy and time-consuming factors makes them at the same time unattractive in the process scale-up and industrial use. Thus, the combustion synthesis (CS), which is a new way to obtain silicon carbide nanofibres is economically justified and privileged.
     Combustion synthesis  is a well-known method [17] for the preparation of useful compounds of carbon, such as nano SiC, activated carbon, [18] and magnetic carbon encapsulated [19]. The high temperature and pressure of very fast redox reaction provide opportunities to process materials with a high melting point. Furthermore, these reactions are thermally autogenous and usually lead to the formation of nano-sized products. Basically, there is no restriction on the choice of appropriate reagents, it is important, however, to connect a strong oxidizer and reducer [20]. From the past experience it can be concluded that by careful selection of starting reactants the combustion leads to the desired product, but in most cases the mechanism of the process is still not clearly defined. In addition, the proposed synthesis method is autothermal, which means that after the initiation the reaction is carried out without energy needs. This makes such processes economically very attractive.
      The aim of this study is to demonstrate that SiC nanofibers can be one-pot produced in fast and single step synthesis using waste materials as substrates and to optimize the conditions in order to maximize the main product - nanofibers SiC.
 

Fig. 1. Fragments of discarded or waste silicon solar panels (A); the experimental setup after the process (Si from waste panels and waste PTFE powder, 1 MPa, air atmosphere) (B)

      Lowering the cost of synthesis of nanomaterials is extremely important for the further development of nanotechnology, which is often limited by the high price of their precursors. So far in the process of nanofibers SiC production we used pure commercial reagents, which are relatively expensive. Thus, the attempt to use cheap or waste reactants is obviously justified. While there have been many attempts to re-use silicon from discarded or waste silicon solar panels there are currently, however, no rational methods for their disposal. Obviously, in the near future this problem can become a major barrier to the development of photovoltaics [21]. We also carried out the exploratory experiments using domestic waste technical PTFE (Teflon) powder.
      To carry out successful syntheses we used silicon material resulting from grinding waste photovoltaic panels. The powder mixture is prepared from the stoichiometric amount of the reactants: 36% wt. Si and 64% wt. of PTFE. The synthesis was performed in an air atmosphere (initial pressure of 1 MPa) in the system presented in Fig. 1. [22]. The obtained products were almost identical to the ones obtained in previous tests with the commercial reactants. The have a ‘spongy’ morphology, demonstrating a significant content of fibrous structures. ‘The microscopic observation confirmed the presence of SiC nanofibers (SEM - Fig. 2.). Further investigation in search of the most favorable process conditions were carried out in CO and CO2 atmosphere. We analyzed the morphology and composition of the reaction products from all tests, including the diameter of nanofibers obtained. The performed CS was monitored opto-electronically to efficiently track the progress of the reaction and to evaluate the velocity of propagation of a combustion wave.   
  substaty_produkty_1.jpg

Fig.2. Silicon carbide nanofibers produced during combustion synthesis (starting reactants: silicon from waste solar panels and waste PTFE powder, 1 MPa, CO2 atmosphere), (A) raw products, (B) products after purification

      The performed studies indicate that silicon from the ground silicon solar panels efficiently reacts during the combustion synthesis with waste PTFE, and the reaction products contain SiC. Thus, a substantial reduction in the cost of the starting reactants is achieved. A scale-up of the CS will be a further step in minimizing the costs associated with the synthesis. The production of a larger amount of material will be extremely important for consideration of different applications. Thus, due to the low time-and energy-consumption, and simple design of the reactor the products can be produced in more than gram quantities.


The research has been supported by the NCN grant No. UMO-2011/03/B/ST5/03256 and UMO-2012/05/B/ST5/00709.

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Presentation: Poster at Nano PL 2014, Symposium A, by Michał Soszyński
See On-line Journal of Nano PL 2014

Submitted: 2014-09-29 11:25
Revised:   2014-09-29 13:56