TEMPLATE SYNTHESIS OF Cu AND Cu-Sn NANOPARTICLES USING CARBON FOAM AS A SUPPORT. Ivania MARKOVA-DENEVA, Tihomir PETROV, Ivan DENEV
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1 TEMPLATE SYNTHESIS OF Cu AND Cu-Sn NANOPARTICLES USING CARBON FOAM AS A SUPPORT Ivni MARKOVA-DENEVA, Tihomir PETROV, Ivn DENEV University of Chemicl Technology nd Metllurgy, 8, Kl. Ohridski lvd., Sofi, Bulgri, e-mil: vni@uctm.edu Astrct Cu nd intermetllic Cu-Sn nnoprticles hve een synthesized through orohydride reduction in wter solution of corresponding chloride slts y NBH 4 using templte technique with cron fom s support t room temperture nd tmospheric pressure. The Cu nnoprticles hve een otined in the cron fom pores using 1.5 M nd 2.0M CuCl 2.2H 2 O solutions, s well s the Cu-Sn nnoprticles hve een prepred using CuCl 2.2H 2 O nd SnCl 2.2H 2 O solutions with the sme concentrtion t mss rtio Cu:Sn=40:60. The morphology of the synthesized Cu nd Cu-Sn nnoprticles using cron fom s support hs een investigted y mens of SEM nlysis. The XRD nlysis crried out hs proved the existence of Cu, Sn nd Cu 10 Sn 3 phses. Thus prepred porous cron fom/cu or Cu-Sn nnoprticles nnocomposites re new electrode mterils for electrochemicl power sources. Keywords: Cu nnoprticles, intermetllic Cu-Sn nnoprticles, templte synthesis, cron fom 1. INTRODUCTION The synthesis using supports known s templte synthesis is pplied for otining of nnosized metllic prticles, wires, fiers, rods, tuules [1-7]. At this method in the pores of support (templte) metl is deposited through chemicl or electrochemicl reduction of corresponding metllic ion. Porous mterils like s SiO 2, moleculr sieves type MCM-41 etc. re used s supports. In our work cron fom (C-fom) hs een used for the first time s support to relize templte synthesis of Cu nd Cu-Sn nnoprticles, ecuse the C-fom is chrcterized y porous structure [2,5,6]. The C-fom is low mteril cost nd light weight. It is chrcterized y unique properties such s high mechnicl strength, high electricl conductivity, low therml conductivity, nd low therml expnsion coefficient. It cn e otined through pyrolysis nd therml tretment of chep precursors such s cols, different polymer mterils, tr-sed mesoporous pitches, olive stones, coffee precipitte, nd rice wste. The C-fom pplictions re vried due to its unique properties. Recently the C-fom hs n importnt ppliction s porous ttery nd fuel cell electrodes. Perspective mterils for electrodes in contemporry energy storge systems re porous nnocomposite mterils sed on C-fom nd intermetllic (Cu-Sn) nnoprticles. The unique properties of C- fom nd in the first ply its porous structure hve initited our ide to use C-fom s support for templte synthesis of Cu nd Cu-Sn nnoprticles through orohydride reduction method to e otined nnocomposite mterils with porous cron mtrix nd ctive deposited in its pores Cu nd Cu-Sn nnoprticles for electrodes in electrochemicl power sources. The purpose of this work is to otin porous C-fom/ctive Cu or Cu-Sn nnoprticles composite mterils y templte synthesis of metllic (Cu) nd intermetllic (Cu-Sn) nnoprticles using C-fom s support through chemicl reduction with NBH 4 (orohydride reduction) in wter solutions of chloride slts of Cu nd Sn 1
2 (CuCl 2.2H 2 O, SnCl 2.2H 2 O) with different concentrtions nd different mss rtio Cu:Sn t room temperture nd tmospheric pressure to e used s electrodes in electrochemicl power storge systems. 2. EXPERIMENTAL 2.1 Templte synthesis of Cu nd Cu-Sn nnoprticles in the pores of C-fom from CuCl 2.2H 2 O nd mixture of CuCl 2.2H 2 O nd SnCl 2.2H 2 O t mss rtio Cu:Sn = 40:60 A templte synthesis of Cu nd Cu-Sn nnoprticle is relized using modified commercil C-fom. In this cse the nnoprticles hve een deposited in the C-fom pores. The Cu-Sn nnoprticles hve een prepred using mss rtio Cu:Sn=40:60. The synthesis hs een crried out in rector ensuring regime of consecutively introducing of the oth solution of reducing gent (NBH 4 ) nd support (C-fom), pplying during the synthesis mechnicl stirring y mgnetic stirrer. The support used is commercil C-fom product, which is previously wetted with the copper solutions or mixture of copper nd tin slts. Solutions of CuCl 2.2H 2 O nd SnCl 2.2H 2 O with different concentrtions (from 0.5M to 2.0M) hve een used. At first 2М CuCl 2.2H 2 O nd 2М SnCl 2.2H 2 O solutions hve een prepred. The lower concentrtion solutions (1.5М, 1.0М и 0.5М) hve een otined through diluting of the 2M CuCl 2.2H 2 O nd 2M SnCl 2.2H 2 O solutions. 4.4М NBH 4 in 14М NOH hs een pplied s reducing gent. 2.2 Investigted techniques used The synthesized porous nnocomposite mterils sed on modified commercil C-fom s mtrix nd Cu nd Cu- Sn nnoprticles s ctive components were investigted y mens of electron microscopy (SEM/TEM) nlyses including specific surfce re diffrction (SAED) nd lso y XRD nlysis. SEM nlysis of the synthesized nnosmples ws crried out on scnning electron microscope JEOL JSM 5300 t ccelerting voltge 20 kv. X-ry diffrction ptterns of cron fom were collected within the 2θ rnge from 10 o to 95 o with constnt step 0.03 o nd counting time 1 s/step on Philips PW 1050 diffrctometer using CuKα rdition. 3. RESULTS AND DISCUSSION 3.1 SEM investigtions of the synthesized nnosized products Figure 1 presents SEM imges of Cu nnoprticles synthesized y templte technique using C-fom s support from 0.5М CuCl 2.2H 2 O solution, while in Fig. 2 re shown SEM imges of Cu nnoprticles, synthesized from 1.0М CuCl 2.2H 2 O solution. Fig. 1. SEM imges of Cu nnoprticles deposited using C-fom s support from 0.5M CuCl 2.2H 2 O t different mgnifictions: - x 200, x 2
3 Fig. 2. SEM imges of Cu nnoprticles deposited using C-fom s support from 1.0M CuCl 2.2H 2 O t different mgnifictions: - x 200, x In Fig. 3 re given SEM imges of Cu nnoprticles synthesized in the C-fom pores from1.5м CuCl 2.2H 2 O solution. Figure 4 presents SEM imges of Cu-Sn nnoprticles otined using C-fom s support from mixture of 1.0М CuCl 2.2H 2 O nd 1.0М SnCl 2.2H 2 O solutions t mss rtio Cu: Sn=40:60. From the SEM microgrphs, shown in Figs 1 to 3, cn e seen tht t the lower concentrtion of the initil copper solution (0.5М CuCl 2.2H 2 O) the synthesized in the C-fom pores Cu nnoprticles re ggregted. At the higher concentrtion (1.5М CuCl 2.2H 2 O) prticles with little dispersion nd out equl size hve een otined. Fig. 3. SEM imges of Cu nnoprticles deposited using C-fom s support from 1.5M CuCl2.2H2O t different mgnifictions: - x 200, x Fig. 4. SEM imges of Cu-Sn nnoprticles deposited from mixture of 1.0M CuCl 2.2H 2 O nd 1.0M SnCl 2.2H 2 O using C-fom s support t different mgnifictions: - x 100, x 3
4 In Fig. 5 re shown SEM imges of Cu-Sn nnoprticles synthesized using C-fom s support from mixture of 2.0М CuCl 2.2H 2 O nd 2.0М SnCl 2.2H 2 O solutions t the sme mss rtio Cu: Sn=40:60. c Fig.5. SEM imges of Cu-Sn nnoprticles deposited from mixture of 2.0M CuCl 2.2H 2 O nd 2.0M SnCl 2.2H 2 O using C-fom s support t different mgnifictions: - x 100, x 200, c x The SEM microgrphs of the Cu-Sn nnoprticles, presented in Figs. 4 nd 5, hve shown tht with incresing of the concentrtion of the initil slts the quntity of the synthesized Cu-Sn nnoprticles lso increses. At the highest concentrtion (2M solutions) it is oserved uniformly filling of the C-fom pores with prticles. Cu-Sn nnoprticles re deposited not only inside the pore, ut lso on the surfce of the grins forming the pores. 3.2 XRD investigtions of the synthesized nnosized Figure 6 presents XRD ptterns of Cu nnoprticles, synthesized respectively from 1.5М CuCl 2.2H 2 O nd 2М CuCl 2.2H 2 O solutions t mss rtio Cu:Sn=40:60. XRD ptterns prove the formtion of Cu phse (2θ = 56 о, 65 о и 98 о ). It is lso oserved Cu(OH) 2 phse (2θ = 20 о, 30 о, 43 о, 45 о, 48 о, 69 о ). In Fig.7 re given XRD ptterns of Cu-Sn nnoprticles synthesized respectively from mixture of 1.5М CuCl 2.2H 2 O nd 1.5М SnCl 2.2H 2 O solution nd mixture of 2М CuCl 2.2H 2 O nd 2М SnCl 2.2H 2 O solution t mss rtio Cu: Sn=40:60. Fig. 6. XRD ptterns of Cu nnoprticles synthesized from 1.5М CuCl 2.2H 2 O nd 2.0М CuCl 2.2H 2 O solutions XRD nlysis of the Cu-Sn nnoprticles otined from the oth solutions of, CuCl 2.2H 2 O nd SnCl 2.2H 2 O (1,5М и 2.0М), proves the formtion of three phses: Cu 10 Sn 3, Cu и Sn. 4
5 Fig. 8. XRD ptterns of Cu-Sn nnoprticles synthesized from mixture of 1.5М CuCl 2.2H 2 O nd 1.5М SnCl 2.2H 2 O nd mixture of 2М CuCl 2.2H 2 O nd М SnCl 2.2H 2 O t mss rtio Cu:Sn=40:60 4. CONCLUSION Porous C-fom/Cu or Cu-Sn nnoprticles composites hve een otined y templte synthesis of Cu nd Cu-Sn nnprticles through wet orohydride reduction method in wter solution of the corresponding slts with NBH 4 in the pores of modified commercil C-fom. The Cu nnoprticles synthesized from CuCl 2.2H 2 O solutions with different concentrtions re crystlline y structure nd hve low dispersion. The Cu-Sn nnoprticles prepred from mixture of the sme solutions t mss rtio Cu:Sn = 40:60 hve een deposited in the C-fom pores nd lso on the surfce of the grins forming the pores. The XRD nlysis hs proved the existence of Cu, Sn nd Cu 10 Sn 3 phses, which predetermine n ppliction of these synthesized porous composite mterils for electrodes in Li-ion tteries. ACKNOWLEDGMENTS LITERATURE The uthors cknowledge the Ministry of Eduction, Youtgh nd Science Fund Scientific investigtions for the finncil support under the Conrtct DDVU 02/98. [1] WOLFENSTINE, J., CAMPOS, S., Effect of Fe on the cycle life of Cu 6Sn 5 nodes, Mterils Letters, 2002, 57, [2] PARKPOOM L., Preprtion of polyenzoxzine fom nd its trnsformtion to cron fom, Mterils Science nd Engineering A, 2009, 527, [3] KLEMPNER, D, SENDIJAREVIC, V., Hndook of polymeric foms nd fom technology.cincinntti: Hnser Grdner Pulictions, [4] SALAVATI-NIASARI, M., BAZARGANIPOUR, M., DAVAR, F., Nno-sized Cu 6Sn 5 lloy prepred y co-precipitte reductive route, Polyhedron, 2010, 29, [5] JUAN, Li, Preprtion of cron foms with supercriticl toluene; J Porous Mter., 2010, 17, [6] ZHANG, S.P., LUI, M.X., GAN, Li.H., WU F.R., XU, Z. J., HAO, Z., CHAN, L.W., Synthesis of cron foms with high compressive strength from rylcetylene, New cron mterils, 2010, 25, 1, [7] WOLFENSTINE, J., CAMPOS, S., FOSTER, D., READ, J., BEHL, W.K., Nno-scle Cu 6Sn 5 nodes, J. of Porous Sources Short communiction, 2002, 109,
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