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Indian Institute of Technology Roorkee

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Structural evolution magnetic properties of granular metallic alloys

January 9

2012
and nano-

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CONTENTS

1. 2. 3. 4. 5.

Introduction Literature Survey Literature Summary Problem Formulation Experimental Procedure and Characterization Tools

6. References

SUBMITTED TO: Dr. B.S.S. Daniel MMED

SUBMITTED BY: KARTIK LOHIYA (08118020) KULVINDER SINGH TUTEJA (08118021)

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1. INTRODUCTION
The experimental study and comprehension of the properties of metallic nanoparticles with a tunable size and composition is a challenge in solid state physics and chemistry due to the novel behaviours exhibited by the nanoscale systems (e.g., giant magneto resistance, magneto caloric effect enhancement and quantum tunnelling of the magnetization), quite different from the bulk materials [1, 2]. These new properties and the reduced dimension of these systems make them suitable for multiple application elds such as magnetic recording [3], catalysis [4] or biomedicine [5]. Due to their unique physical and chemical characteristics such as small scale and surface effects, nanomaterials are now widely produced and used in different elds. In the recent years, magnetic nanoparticles such as metals, alloys and multi-layers have attracted tremendous interest from researchers in many elds due to their promising applications in the area of ferro-uids, microwave absorbance, hyperthermia, catalysis, magnetic resonance imaging (MRI) and drug delivery system, magnetic recording and magnetic based sensors and excellent reviews are available on such topics. Nanocrystalline magnetic alloys such as NiCu, CoNi, FeCo and FeCoCu are promising candidates for hyperthermia and microwave applications because their magnetic transition temperatures and microwave absorbance characteristics vary with composition and grain size. In addition to the polyol reduction, many methods such as hydrogen and hydrothermal reduction, mechanical alloying, sonochemical method, thermal decomposition, solgel process, co-evaporation, microemulsion method, sequential ion implantation, electroless deposition, biomineralization and magnetic eld-assisted solvothermal process have been reported in the literature for the synthesis of CoNi alloy nanoparticles [6].

2.

LITERATURE SURVEY
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A brief outline of the various methods available for synthesis of metal alloy nanoparticles :
2.1 Ni -Fe alloy nanoparticles by hydrothermal process (size=150nm) [7] :

It consists of two steps:

A. Preparation of NiFe2O4 precursor particles: NiCl2 and FeCl3 are dissolved in ethylene glycol

(EG) with Ni2+:Fe3+ molar ratio of 1:2. Certain amount of sodium acetate and polyethylene glycol are then added to the solution with continuously stirring for 30 min. The mixed solution is transferred into an autoclave, sealed and held at 200 C for 18 hrs. The autoclave is then cooled naturally to room temperature and the products are collected for subsequent investigation.
B. Preparation of Ni-Fe alloy particles: The precursor NiFe2O4 particles are reduced in a

hydrogen atmosphere at 300 and 400 deg C for 1 hr., respectively. The reduced products are cooled in N2 atmosphere to room temperature naturally in the furnace.
2.1 Synthesis of NiCu nanoparticles by Pulsed Wire Discharge (size > 100nm) [8] :

Ni (pure: 99%) and Cu (pure: 99.9%) single wires are twisted together to form a stranded wire. The wire is located between the electrodes in a chamber filled with N2 gas at a pressure of 100 kPa. After charging, the capacitor is discharged through the wire by closing the gap switch. After discharge, the particles floating in the chamber are collected by evacuating the chamber through a filter.
2.2 Synthesis of NiAl nanoparticles by hydrogen plasmametal reaction (size = 20 to 40

nm) [9] : The NiAl ingots are prepared from aluminum (purity >99.9 wt.%) and nickel (purity >99.7 wt.%) by arc melting in an argon atmosphere. Arc-melted ingots are flipped over and remelted four times to get a homogeneous composition. Then NiAl nanoparticles are produced by arc melting in a 50% Ar (purity >99.99%) and 50% H2 (purity >99.99%) mixture of 0.1 MPa atmosphere. The flow rate of the circulation gas for collection of nanoparticles is 100 l/min. Identical master alloy buttons (NiAl ingot) weighing 50 g are used in this work. Arc current and voltage are selected as 180A and 25V, respectively. Before the nanoparticles are taken out from the arc-melting chamber, they are slowly passivated with a mixture of argon and air to prevent them from burning.
2.3 Synthesis of Ni-Fe alloy nanoparticles by hydrogen reduction of metal chlorides (size

=56 to 82 nm) [10] :

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Two quartz boats loaded with solid phases of FeCl2 and NiCl2 are placed separately. Ar gas containing metal chloride vapors flows through the inner tube while hydrogen (H2) and additional Ar gases through the outer. Ni-Fe nanoparticles that have been synthesized in the reaction zone are collected by a Teflon membrane filter. These nanoparticles are allowed to react with small amount of oxygen existing in Ar gas for about 12 hrs. since Ni-Fe nanoparticles are easily oxidized in ambient air to form thin oxide layer to prevent further oxidation.
2.4 Synthesis of polymer encapsulated Ni-Cu magnetic nanoparticles for hyperthermia

applications [11] : A. Physical method (size = 300 to 400 nm) Nickel powder (325 mesh, 99%) and copper powder (500 mesh, 99%) mixture are heated at 1465 deg C (100 deg C above the melting temperature of Ni-Cu alloy) for three hours under nitrogen atmosphere. The bulk solid alloy is mechanically abraded to produce a powder texture and further ball milled for 37 days in acetone. B. Chemical method (size = 50 to 80 nm) 0.2M metallic precursor (mixture of metal salts viz. nickel acetate tetrahydrate and copper acetate monohydrate) in ethylene glycol is mixed with 1M sodium hydroxide and heated at 195 deg C. Water and volatile products of the reaction are distilled off while the polyol is refluxed. After a few hours, the metal alloy particles are quantitatively precipitated from the solution and this portion is recovered by centrifugation, washed with ethanol and dried in air at 50 deg C. The encapsulation by polymers is then carried out.

2.1 Synthesis of Ni-Cu alloy powder directly from metal salts solution [12] :

An aqueous solution of 0.07M Cu(NO3)2. 3H2O and 0.03M Ni(NO3)2.6H2O is prepared as a stock solution. The precursor solution for self sustaining combustion and ultrasonic mist combustion is prepared by adding twice the stoichiometric amount of glycine as a fuel to the above stock solution while, for ultrasonic mist pyrolysis, the stock solution is used as prepared. The self-sustaining combustion process is performed by heating the stock solution on a hot plate in open air. As soon as the water became fully vaporized, spontaneous combustion starts by the burning of the metal salts and fuel. The mist of precursor solution is generated at room temperature. The droplets are passed through a reactor held at 800 deg C. The synthesized powder is collected after cooling the furnace to room temperature. In

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order to reduce the metal oxides and suppress the oxidation of the metal elements, this process is performed in a reducing gas mixture of Ar + 4% H2.
2.2 The preparation of Ni- Cr alloy nanoparticles on supports (size = 2 to 30 nm) [13] :

Nitrates (in Ni:Cr ratios of 2:1, 1:1 and 1:2) are dissolved in the minimum amount of ethylene glycol and loaded onto a support. Silica (SiO2, BDH precipitate, acid washed) or baddeleyite (ZrO2, 99.8% purity) are used as the supporting medium. A strong reaction occurs with carbopack supports on reduction, resulting in greatly increased graphitization of the support. A 50% molar metal loading is prepared with typically 0.50 gm of support used. The sample is dried in an oven at 100 deg C for 24 hrs. and then reduced at 600 deg C for 6 hrs. with hydrogen.
2.3 Preparation of Ni-Pt nanoparticles [14]

A. Preparation of Ni-Pt-1 (size = 12.5 to 50 nm) To a well-stirred suspension of Vulcan Carbon XC 72 (0.1 g) in 30 ml of water, 10 ml each of 5 mM solutions of K2PtCl4 and NiCl2.6H2O are added followed by 0.2 g of poly(N-vinyl2-pyrrolidone) (mol. wt. 10000). The resulting mixture is placed in a constant temperature water bath at 60 deg C. Hydrazine (40 L) and 400 L of 1 M NaOH are added in succession to the reaction mixture. The reaction mixture is stirred for about two hours before the carbon supported Ni-Pt-1 nanoparticles are filtered off, washed copiously with water and dried in a vacuum oven at 120 deg C. B. Preparation of Ni-Pt-2 (size = 13 to 25 nm) Same procedures as those of Ni-Pt-1 with the exception that the reduction reaction takes place at room temperature for 12 hrs. Ni-Pt-3 is synthesized using the same amounts of reactants as in the preparation of Ni-Pt-1, but the reaction mixture is exposed to microwave irradiation. The reaction vessel is placed in a CEM microwave reactor and subjected to a 100W radiation for 10 minutes. The reaction mixture is stirred during the microwave heating. The reaction mixture is then allowed to cool to room temperature and the suspension is filtered to recover the solid product, which is subsequently washed with water and dried in a vacuum oven.
2.1 Synthesis of metastable Ni-Ag alloys by

a novel laser-liquid-solid

interaction

technique (size= 100 nm) [15] :

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A solution is prepared by dissolving nitrate or acetate precursors of silver and nickel in ethylene glycol, diethylene glycol and 2-ethoxyethanol. A cooling coil is used to maintain the solution temperature at 25 deg C. The reactor is constantly purged with nitrogen to prevent oxidation of the powders. The precursor solution is irradiated either by a continuous wave CO2 laser (10640 nm) or a pulse YAG laser (1064 nm) with powers ranging from 150300W, and the interaction time varying from 13 minutes. The particles are separated using a centrifuge for 15 minutes, washed with distilled water for another 15 minutes, then dispersed in ethanol using an ultrasonic bath, and allowed to settle overnight.
2.2 Synthesis of nanocrystalline CoNi alloys by precursor approach [6] :

CoNi alloy particles were synthesized by polyol reduction of Cox Ni1-x(OH)2 . In a

typical

synthesis, the mixed cobalt nickel hydroxide was prepared by co-precipitation as follows. In a 250 ml beaker, nickel chloride hexahydrate and cobalt chloride hexahydrate in appropriate molar ratios were dissolved in 60 ml de-ionized water. To this, 60 ml aqueous solution of sodium hydroxide (6 mmol) was added dropwise at room temperature for about 35 min. During the precipitation, green precipitates were formed in all the cases. The precipitates were ltered, washed with de-ionized water many times followed with ethanol and then dried at room temperature in air. The dried hydroxide powders were ground using a ceramic mortar and pestle. The yield of precursors varied from about 0.2 to 0.4 g. The polyol reduction of the mixed hydroxides was carried out as follows. About 0.25 g of the precursors (mixed metal hydroxides) was heated at 115o C for 4 h to remove the physically adsorbed water molecules. Then, the precursor powders were reuxed at 180 o C for 614 h in about 20 ml ethylene glycolNaOH (1 g) system to yield the nanocrystalline alloys. The powders turned black within 24 h, in all the cases, indicating the reduction process. The alloy powders were ltered, washed with acetone many times and then dried at room temperature in air. More details on the precursors and the alloy powders, obtained after the polyol reduction.

2.3 Freshly prepared cobalt (II) and nickel (II) hydroxides subjected to reduction in

ethylene glycol to obtain CoNi powder [16] : Ni-Co powders were obtained by the co-reduction of either commercial (Aldrich Chem. Co. Inc.) or freshly prepared Co (IX) and Ni (II) hydroxides in 1,2-ethanediol (ethylene
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glycol, EG) (b.p. 196-198C) at the refluxing temperature. Ni (II) hydroxide was obtained in quantitative yield by precipitation from a Ni (II) nitrate hexahydrate (Aldrich Chem. Co. Inc.) aqueous solution by adding an aqueous NaOH solution under controlled pH (around 10) and temperature (60C). Nickel hydroxide was obtained as a light-green gel, which was allowed to age for several days. It was then separated from the mother liquid by centrifugation, washed first with water and then with acetone, dried at room temperature, and finally ball-milled for 30 min. Cobalt (II) hydroxide was obtained in quantitative yield by precipitation from a Co (II ) nitrate hexahy- drate (Aldrich Chem. Co. Inc. ) aqueous solution by adding a NaOH solution under controlled pH (around 10) and temperature (25C). The product was immediately separated from the mother liquid by centrifugation, washed with different portions of water, then ethanol was used to remove the water and diethyl ether to eliminate the ethanol. Co- balt hydroxide was then dried in vacuum and stored in Nz in order to prevent its oxidation by exposure to air. Metallic powders were prepared from the suspen- sion obtained by adding 9.6 mmol of Ni (OH ) 2 and 3 mmol of Co(OH), (Ni/Co atomic ratio 76/24) to 20 ml of EG by refluxing under magnetic stirring. The precipitate was separated from the reaction medium by centrifugation, washed with several portions of acetone, and dried at room temperature.

2.4

CoNi particles useful for microwave applications with sub-micron size range have been synthesized by the polyol process [17] : Monometallic Co and polymetallic CoNi or FeCoNi, monodispersed powders were obtained by precipitation in liquid polyols from cobalt hydroxide and polymetallic mixed hydroxides. The details of the preparation have been previously reported elsewhere. For cobalt and cobalt nickel powders, reduction of the metallic precursor by the polyol itself is followed by the nucleation and growth of the metal particles from the solution. Homogeneous nucleation leads to particles in the micrometer-size range. By modifying the nucleation step, using seed particles acting as nuclei heterogeneous nucleation, it is possible to obtain submicrometer-sized particles and to control accurately their average diameter by varying the number of foreign nuclei. For iron-based particles, the metal is generated in solution by disproportionation of the ferrous hydroxide, a lower yield of the disproportionation with respect to those of reduction of Co and Ni hydroxide limiting the Fe content in FeCoNi powders to 25%. In this case, homogeneous nucleation leads directly to submicrometer-sized particles.
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2.5

CoNi alloy nanoparticles have been synthesized by the polyol reduction of metallic salts [18] : Preparation of Co80Ni20 powder: Fine Co80Ni20 particles have been synthesized by the polyol process. Cobalt (II) and nickel (II) tetra hydrated acetates were dissolved in 1, 2propanediol in the presence of 0.25 mol dm3 sodium hydroxide. The concentration of this metallic precursor was typically 0.1moldm3 and the Co/Ni molar ratio was equal to four in all reactions. In order to obtain particlessmallerthan1m,anucleating agent (salts of Ag or Pt) has to be added to the initial solution. By increasing the concentration of the nucleating agent with respect to the metallic precursor, the particle diameter can be varied from around 500 to 10nm. The solutions were stirred and heated up to the boiling temperature (195C) for a few hours. Finally, the resulting powders were recovered by centrifugation and washed several times with ethanol.

2.6 CoNi anisotropic particles have been prepared by the polyol reduction of metal

acetates [19] : Cobalt particles were prepared in two steps. First, cobalt acetate tetra hydrate and the desired amount of sodium acetate trihydrate or sodium hydroxide were dissolved in 100 ml and 60 ml of 1,2-propanediol, respectively. In some cases, a small amount of de-ionized water was added. The mixture of the two solutions was heated in a three-necked ask to 150C for 1 h, with mechanical stirring. During this rst step, a solid phase precipitates, the nature of which depends on the experimental parameters (see next section). After 1 h, the suspension was cooled to room temperature. In the second step, 40 ml of a solution of ruthenium trichloride, RuCl3, in 1,2-propanediol was added. The Ru concentration was kept constant (2 6 102 3 mol l 2 1) with a molar [Ru]/[Co] ratio of 2.5. The mixture was heated to reux for 2 h. The reux temperature was in the range 160175C, depending on the composition of the solution and, particularly, on the amount of water. After cooling to room temperature, a black powder and, in most cases, a metallic mirror on the ask walls were observed. The metal powder was recovered by centrifugation, washed with ethanol and dried in air at 50C. For Co80Ni20 particles, the same procedure was followed, with a starting mixture of cobalt and nickel acetates in an 80:20 molar ratio. The cobalt concentration in the total volume (200 ml) was kept constant (0.08 mol l 2 1) in all experiments. Sodium acetate and sodium hydroxide were varied in the concentration ranges 00.5 and 00.2 mol respectively. Two parameters were varied: (i) the base ratio, dened
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as either the molar [acetate]/[Co] or [hydroxide]/[Co] ratio; (ii) the hydrolysis ratio, dened as the molar [H2O]/[Co] ratio.

1. LITERATURE SUMMARY
Various methods for production of nano particles have been mentioned above for various two phase systems. These mainly include chemical processes such as polyol reduction method (from metal salts, acetates), hydroxides reduction etc. Also pulsed wire discharge method has been used for Ni-Cu system. These so produced nano particles are very useful for different purposes as mentioned above. But these process are equipment intensive (they require laser, autoclave etc.) as well as costly. Also, there is less control on the particle size. So our endeavour was to synthesise metal nanoparticles by a simpler method and see for the change in the magnetic properties due to alloying it with another metal. Also effective size control is the most important parameter for different applications. So considering our system (Co-Ni), the two are immiscible in bulk phase so no useful alloy can be produced, which is the case with most of the alloy system but at nano level due to increased surface area the reaction tendencies for particles increases and alloys at such level are possible. Now the size of these nanoparticles can be controlled over the process i.e. by controlling time and temperature. At low temperatures, more time will be required for alloy to be formed. But we will have effective control on the process and particle size.

2. FORMULATION OF THE PROBLEM

The aim of our project was to analyse the feasibility of forming an alloy between two metals at the nano scale by hydrogen reduction process. If the possibility of alloy is there, then it becomes important to analyse the properties of the alloy prepared by hydrogen reduction method and that by other chemical processes. The alloy was prepared starting from corresponding precursors followed by thermal decomposition-reduction process of the precursors. There can be various parameters affecting the composition and the final
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properties of alloy. To save nickel nanoparticles from oxidation is a big challenge in itself. All these aspects have been analysed to a sufficient extent by the literature studies and experiments. 4.1 Preliminary Experiments The alloy formation is conrmed from the shift of XRD peak positions (Fig. 1) with respect to those of the constituent pure phases. When an alloy is formed of two elements with similar crystal structure (isomorphous system), the lattice parameter is different from those of pure metals and the shift is a measure of the amount of the elements present. As the XRD peak positions are representative of the crystal structure and lattice parameters, a quantitative analysis can be carried out. Also two peaks will be observed if the alloy doesnt form but a single peak indicates that alloy has been formed with a crystal structure between that of the two pure metals. During XRD analysis, there could be an error introduced due to misorientation of the sample placed in the specified holder. Sometimes the machine is not perfectly calibrated, which also introduce spurious shifting of the diffraction peaks. So when an alloy is formed, the lattice parameter is different from the pure metal, which in turn causes a shift in XRD peaks. Without proper calibration it will be impossible to detect the shift solely due to change in lattice parameter. So, to eliminate instrumental error we carried out internal calibration using pure aluminium as a reference. Now, when XRD is carried out, the error is the same for both the sample and the standard sample.

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Fig :1 XRD patterns of cobaltnickel alloys (RP2RP4), which were physically mixed with electrolytic grade Cu powder for internal calibration.

3.

EXPERIMENTAL PROCEDURE AND CHARACTERIZATION TOOLS

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5.1

Reagents

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All the chemicals were used without further purication. Nickel chloride hexahydrate (NiCl2. 6HO, 97% pure) was procured from Fisher Scientics, cobalt chloride hexahydrate (CoClO,97% pure) from Loba Chemicals, sodium hydroxide pellets (NaOH, 98% pure) from Qualigens and ethylene glycol (98% pure) from Rankems .Millipores water was used for the preparation of aqueous solutions. 5.2 5.2.1 Reduction of Precursors Reduction apparatus For reduction of precursors to metals or alloy we used hydrogen gas as the reducing agent. The temperature was maintained as 35o deg C and time = 4 hrs for all the reduction experiments. We used a tubular furnace for heating and an arrangement was made so as to allow passage of hydrogen gas. 5.2.2 Filling of Hydrogen Cylinder The filling of the hydrogen cylinder was done by hydrogen generator. The principle of hydrogen generation involved electrolysis of water. The apparatus was designed to fill a maximum of 90 psi of hydrogen. The generator had two pressure indicators, viz. actual pressure and set pressure. Actual pressure is the pressure of hydrogen gas in the cylinder whereas the set pressure is the pressure at which generator fills hydrogen into the cylinder. It is obvious the set pressure has to be higher than the actual pressure. The set pressure has to be maintained 2 psi above actual pressure. For every 20 mins, the set pressure has to be increased by 1 psi. So, in one hour 3 psi of gas is filled. So to fill 90 psi, 30 hrs were required.

5.3 5.3.1

Characterization techniques used: Powder X-ray Diffraction (XRD) The instrument for the powder XRD studies is Bruker AXS D8-Advance X-ray Diffractometer. Cu-K (=1.5406 ) radiation is used as X-ray source and scan speed 5/min and 5 to 75. The applied voltage and current for the measurements are 40kV and
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30 mA respectively. The mean crystallite size was calculated from the XRD pattern using Debye-Scherrer equation: Debye-Scherrer equation is, D= (0.9 )/(Cos) Where = X-ray wavelength (1.5406 ) = Full wavelength at Half maximum (FWHM in radians) = Braggs angle D= Mean crystallite size () 5.3.3 Field Emission Scanning Electron Microscope (FE-SEM) To observe the morphology and particle size, FE-SEM analyses will be done. The instrument used will be QUANTA 200 FEG marketed by FEI Netherlands. In this instrument, high voltage (20 kV) beam was produced by using a Field Emission Gun (FEG). The detector used for identifying back scattered electron beam was a Secondary Electron Detector (SED). EDAX images were used for semi quantitative analysis. The detector used for EDAX was Si-Li detector (X-ray detector).

4. REFERENCES
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Magnetism and Magnetic Materials, Amsterdam (1992), p. 199. (23). diffraction peak broadening, Physics Revised.Letter, (1988) 60 661.

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[3] [4] [5] [6] S. Sun, E.E. Fullerton, D. Weller and C.B. Murray, Magnetic nanoparticles: J.S. Bradley and G Schmid, Cluster and Colloids (1994) (New Yor k: VCH) ch 6 A.E. Merbach and E. Toth, Chemistry of Contrast Agents in Medical Magnetic S. Panday, B.S.S. Daniel and P. Jeevanandam, Synthesis of nanocrystalline CoNi synthesis, ordering and properties (2001) IEEE Transmission Magnetism 37.

Resonance Imaging (2001) (New York: Wiley) ch 10. alloys by precursor approach and studies on their magnetic properties, Journal of Magnetism and Magnetic Materials 323 (2011) 2271-2280. [7] L. Zhen, Y. X. Gong, J. T. Jiang, and W. Z. Shao, Synthesis of a-cobalt hydroxides with different intercalated anions and effects of intercalated anions on their morphology, basal plane spacing, and capacitive property, Journal of Applied Physics (2008), 104(3), 034312/1-034312/5. [8] K. Suwa, T. Nakayama, T. Suzuki, H. Suematsu, W. Jiang and K. Nihara, Heterogeneous nucleation and growth of metal nanoparticles in polyols, Japanese Journal of Applied Physics (2008), 47(1, Pt. 2), 775-779. [9] [10] Z. Wang , A.L. Fan , W.H. Tian , Y.T. Wang and X.G. Li, Materials Letters (2006), Y. J. Suh, H. D. Jang, H. Chang, W. B. Kim and H. C. Kim, Synthesis and 60(17-18), 2227-2231. characterization of polymer encapsulated CuNi magnetic nanoparticles for hyperthermia applications, Powder Technology (2006), 161(3), 196-201. [11] J. Chatterjee, M. Bettge, Y. Haik and C. J. Chen, Synthesis and characterization of polymer encapsulated CuNi magnetic nanoparticles for hyperthermia applications, Journal of Magnetism and Magnetic Materials (2005), 293(1), 303-309. [12] C.H. Jung, H.G. Lee, C.J. Kim and S.B. Bhaduri, Synthesis and characterization of iron-based alloy nanoparticles for magnetorheological uids, Journal of Nanoparticles Research (2003), 5(3-4), 383-388.

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R.D. Tilley and D. A. Jefferson, Designed synthesis of cobalt and its alloys by T. C. Deivaraj, W. Chen and J.Y. Lee, Studies on catalytic behaviour of CoNiB in

polyol process, Journal of Materials Chemistry (2002), 12(12), 3809-3813. hydrogen production by hydrolysis of NaBH, Journal of Materials Chemistry (2000), 14(11), 38948-3956. [15] D. Poondi and J. Singh, Oriented magnetic nanowires with high coercivity, Journal of Materials Science, Volume 35, 2000 , pp. 2467-2476(10).
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[16] A. Bianco, G. Gusmano, R. Montanari, G. Montesperelli and E. Traversa, Preparation of NiCo metal powders by co-reduction of Ni (II) and Co (II) hydroxides for magnetoresistive sensors, Material Letter 19 (1994) 263268. [17] G. Viau, F. Ravel, O. Acher, F. Fievet-Vincent and F. Fievet, Preparation and microwave characterization of spherical and monodisperse Co20Ni80 particles, Journal of Applied Physics, 76 (1994) 65706572. [18] 272. [19] N. Chakroune, G. Viau, C. Ricolleau, F. Fievet-Vincent and F. Fievet, Cobalt-based anisotropic particles prepared by the polyol process, Journal of Materials Chemistry, 13 (2003) 312318. C. Luna, M. del Puerto Morales, C.J. Serna and M. Vazquez, Multidomain to singledomain transition for uniform Co80Ni20 nanoparticles, Nanotechnology 14 (2003) 268

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