research article preparation of soft magnetic fe-ni-pb-b alloy...

Hindawi Publishing CorporationThe Scientific World JournalVolume 2013 Article ID 946897 6 pageshttpdxdoiorg1011552013946897

Research ArticlePreparation of Soft Magnetic Fe-Ni-Pb-B Alloy Nanoparticles byRoom Temperature Solid-Solid Reaction

Guo-Qing Zhong and Qin Zhong

State Key Laboratory Cultivation Base for Nonmetal Composite and Functional Materials School of Material Science and EngineeringSouthwest University of Science and Technology Mianyang 621010 China

Correspondence should be addressed to Guo-Qing Zhong zgq316163com

Received 15 August 2013 Accepted 24 September 2013

Academic Editors F Benito-Lopez and S-P Ju

Copyright copy 2013 G-Q Zhong and Q Zhong This is an open access article distributed under the Creative Commons AttributionLicense which permits unrestricted use distribution and reproduction in any medium provided the original work is properlycited

TheFe-Ni-Pb-B alloy nanoparticleswas prepared by a solid-solid chemical reaction of ferric trichloride nickel chloride lead acetateand potassium borohydride powders at room temperature The research results of the ICP and thermal analysis indicate that theresultants are composed of iron nickel lead boron and PVP and the component of the alloy is connected with the mole ratioof potassium borohydride and the metal salts The TEM images show that the resultants are ultrafine and spherical particles andthe particle size is about a diameter of 25 nm The largest saturation magnetization value of the 2118 emu gminus1 is obtained in theFe-Ni-Pb-B alloy The mechanism of the preparation reaction for the Fe-Ni-Pb-B multicomponent alloys is discussed

1 Introduction

The various metals and alloys have been widely used inscience and technology Many amorphous alloys such as Fe-based amorphous alloys possess superior magnetic proper-ties compared to their crystalline counterparts because oftheir unique atomic structures [1] A great deal of effort hasbeen devoted to iron series alloy nanoparticles because ofthe novel optical catalytic electrical andmagnetic properties[2ndash8] Generally the preparation methods of the nanoalloyshave strict environment requirement or complicated experi-ment process because of the strong activity of the fresh metalnanoparticles [9ndash12] The metal-boron alloys nanoparticleswere generally prepared in solution by chemical reductionmethod But a variety of synthetic parameters such as theratio of the reactants pH of the solution and the order of thematerials added have significant effect on the morphologyof the obtained materials in the aqueous chemical reductionwhich has been researched in recent years [13ndash17] Roomtemperature solid-solid chemical reaction is a novel tech-nique for preparation of nanosized materials Recently wehave found that some amorphous alloys nanoparticles andthe copper bismuth or antimony nanocrystalline particlescan be prepared very easily by room temperature solid-solid

reaction [18ndash21]The reaction can be quickly accomplished atroom temperature which is a challenge to those traditionalmethods

Lead can form eutectic alloy [22 23] or hypomonotecticalloy [24ndash26] with another metal and is applied to thebattery or lubricating materials electrical contact materialssuperconducting materials and so on In recent years theprepared method and character of a series of lead alloys havebeen studied The preparation and characteristics of Fe-PbNi-Pb and a series of ternary alloys about lead have beenreported [27ndash29] Lead is a soft metal and it is insoluble iniron under equilibrium conditions Therefore the study onthe room temperature solid-solid chemical reaction prepara-tion of the lead-based multicomponent alloy nanomaterialswill be very interesting not only for studying incompatibil-ity alloy but also for exploration of the new preparationmethod of other multicomponent alloy nanoparticles In thiswork the Fe-Ni-Pb-B multicomponent alloy nanoparticlesare synthesized by room temperature solid-solid chemicalreaction the effect of the mole ratio of potassium borohy-dride and the metal salts on the component of the alloynanoparticles is discussed and the magnetic performance istested

2 The Scientific World Journal

2 Experimental

All chemicals used in the preparation experiment werein analytical grade which were purchased from ChengduKelong Chemical Reagent Factory in China Ferric trichlo-ride hexahydrate nickel chloride hexahydrate and leadacetate trihydratewereweighed and placed in an agatemortarand mixed up and the corresponding mole ratio of the threemetal salts was 100 100 0500 Then the white potassiumborohydride powder was added to the above mixture andthe mole ratio of the metal salts to potassium borohydridewas 100 125 Immediately the mixture became black andreleased a lot of colorless gas The released gas was testedwith moist pH paper and the result indicated that the gaswas faintly acid gas The reason was that the acetic acid andhydrogen chloride were released in the reaction process Themixture was grinded carefully about 3min and then 2 ofpolyvinylpyrrolidone (PVP) of the total mass of the metalsalts was added to the above agate mortar and the grindingwas kept on about 5minThe reactionwas conducted at roomtemperature Then the resultant was moved to a glass beakeras soon as possible and the resultant was rinsed repeatedlyby deionized water and collected by a centrifugation forremoval of the residual reactants until no chlorine ion inwashed water could be tested by the silver nitrate solutionAfterwards the resultant was washed thoroughly by ethanolto remove residual water in the resultant Finally the resultantwas dried in vacuum at 313 K for 5 h The resultant was fineblack particles and recorded as 1 The same method was usedto prepare resultants 2 and 3 in which the mole ratio ofthe metal salts to potassium borohydride was 100 200 and100 300 respectively

The composition of the resultants was determined bythe inductively coupled plasma-atomic mass spectrometerFirst the sample was solubilized by a certain amount ofconcentrated nitric acidThen the content of the iron nickellead and boron in the sample solution was measured by aThermo X-2 ICP-MS instrument The thermal properties ofthe resultant were examined by a TA Q500 thermogravimet-ric analyzer at a heating rate of 20Kminminus1 and the TG-DTA curves of the resultant were shown in Figure 1 Thepowder X-ray diffraction (XRD) patterns of the resultantswere recorded by a 119863max-II X-ray diffractometer Cu K

1205721

radiation (120582 = 0154056 nm) and Ni filter and scanning ratewas 8∘ (2120579)minminus1 at room temperature The powder X-raydiffraction data of the resultants were collected in the diffrac-tion angle ranges of 3∘ndash80∘ in Figure 2 The morphology andthe particle sizes of the resultant were studied by a TecnaiG20 (FEI) transmission electron microscopy at 300 kV ForTEM observation the samples were dispersed in ethanol byultrasonic treatment and dropped on carbon-copper gridsThe TEM images of the resultant were given in Figure 3 Thesoftmagnetic properties of the resultants were investigated bya BKT-4500Z vibrating sample magnetometer

3 Results and Discussion

The chemical composition and the percentage content ofthe resultants are listed in Table 1 The results of the ICP

300 400 500 600 700 800 900 100075

80

85

90

95

100

Mas

s (

)

minus0010

minus0005

0000

0005

0010

0015

0020

Hea

t flow

(Wg

)

5695 K9942 K

8637 K7002 K

minus1781

T (K)

Figure 1 TG-DTA curves of resultant 2

10 20 30 40 50 60 70 80

(a)

(b)

(c)

2120579 (deg)

Figure 2 Powder X-ray diffraction patterns of the Fe-Ni-Pb-B alloynanoparticles (a) resultant 1 (b) resultant 2 and (c) resultant 3

analysis indicate that the percentage content of iron nickellead and boron in the resultant 2 is 966 2645 4650and 031 respectively The total content of the metals andboron of resultant 2 is about 8292 As the PVP was addedthe total percentage content of the metals and boron is notequal to 100 Therefore the other elements (1708) inthe resultant most possibly come from the PVP and theconjecture is demonstrated in the result of TG-DSC analysisIn addition several compositions of the alloy nanoparticleshave been gained by adding a different ratio of KBH

4

in theexperimental process Increasing the addition of potassiumborohydride fromTable 1 the percentage content of iron andnickel in the resultant is increased This indicates that themole ratio of potassium borohydride to the metal salts hasan obvious effect on the composition of the resultant

The TG-DTA curves of resultant 2 in air from roomtemperature to 1023K are shown in Figure 1 There is anobvious weight loss process in the TG curve below 650KBecause the resultant contains iron nickel lead boron andPVP so the lost component must come from the oxidationand decomposition of PVP The total percentage weight lossis 1781 and it fits right in with the data (1708) of the ICP

The Scientific World Journal 3

(a) (b)

Figure 3 Transmission electron micrographs of the Fe-Ni-Pb-B alloy nanoparticles

Table 1 The testing data of ICP of the resultants

Resultant n (metal salts) n (KBH4) Fe () Ni () Pb () B () Total ()1 100 125 945 2518 4257 019 77392 100 200 966 2645 4650 031 82923 100 300 1213 2856 4679 022 8770

determinationThe weight of the residue is constant at 650KThere are multiple weak exothermic peaks in the DTA curvefrom 650 to 1023K which are caused by the crystallizationof the resultant in heating process The results of the ICP andthermal analysis indicate that the resultant is not oxidized Infact the freshmetal alloy particles can be oxidized very easilyby the oxygen in the air [21] In this case the particles can becladded by PVP to insulate oxygen from air

By now there is no literature that reported the preparationof the high lead multicomponent amorphous alloys Weobserve that the sharp peaks and diffuse peak exist in theX-ray powder diffraction patterns in Figure 2 This indicatesthat the resultants are mainly consisted of nanoamorphousphase and a minute amount of nanocrystalline phase [2]The probable reason is that the reactions are very quicklycarried out at room temperature and the generated particlescannot accomplish the conversion from amorphous state tocrystalline state At the same time the self-diffusion of leadand the incompatibility alloy formed easily of lead and othermetals may be the main reason [30] Combined with theTEM images of resultant 2 two different crystal states havebeen found in Figure 3 In addition to a large amount ofspheroidal particles some linear products are scattered in theresultant This may explain the existence of sharp peaks anddiffuse peak in the XRD patterns A statistical analysis of theTEM images shows that the resultant is mainly formed fromultrafine and spherical nanoparticles and a small amount ofnanowires are interspersed among themThe average particlesize of the spherical nanoparticles is measured from the TEMimages and estimated to be of diameter 25 nm A layer of filmcan be observed in Figure 3 that is the PVP which is coated

on the surface of the nanoparticles and it is the probablereason that the fresh metal alloy nanoparticles have not beenoxidized easily

Figure 4(a) illustrates the hysteresis loops of resultants 12 and 3 respectively The data of saturation magnetizationcoercivity and remanent magnetization for resultants 1 2and 3 is listed in Table 2 It can be seen that the increase inthe metallic relative content in resultants causes significantenhancement of the saturation magnetic polarization (Ms)from 901 emu gminus1 for 1 to 2122 emu gminus1 for 3 namely it isincreased with reducing agent additionThe determined dataof the coercive force (Hc) for 1 2 and 3 is similar and isrespectively 6585 7785 and 5417Oe which are graphicallyillustrated in the corresponding Figure 4(b) The long andnarrow hysteresis loops indicate that the resultants have lowcoercive force and remanent magnetization Therefore theresultants have superior soft magnetic property

The preparation of multicomponent nanoalloys such asthe Fe-Ni-Pb-B alloy nanoparticles by a room temperaturesolid-solid chemical reaction has never been reported Asmuch as the chemism is cloudy the preparation method ofsolid-solid reaction at room temperature had been seldomstudied In this experiment the potassium borohydride isthermodynamically unstable and possesses rather reducingactivationThe iron nickel and lead can be reduced out fromtheir metal salts using the potassium borohydride as reduc-tant The standard electrode potentials of the correspondinghalf-reactions are as follows

H2

+ 2eminus 997888rarr 2Hminus 119864∘ = minus2251V

Fe3+ + 3eminus 997888rarr Fe 119864∘ = minus0037V


Table 2 The saturation magnetization coercivity and remanent magnetization of the resultants

Resultant Saturation magnetization (emu gminus1) Coercivity (Oe) Remanent magnetization (emu gminus1)1 901 6585 1302 1759 7785 2343 2122 5417 220

minus4000 minus3000 minus2000 minus1000 0 1000 2000 3000 4000

minus20

minus10

0

10

20

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(A)

(B)

(C)

(a)

minus1500 minus1000 minus500 0 500 1000 1500

minus3

minus2

minus1

0

1

2

3

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(b)

Figure 4 Complete magnetic hysteresis curve (a) and partial of this curve showing the coercive force (b) of the Fe-Ni-Pb-B alloynanoparticles (A) resultant 1 (B) resultant 2 and (C) resultant 3

Ni2+ + 2eminus 997888rarr Ni 119864∘ = minus0246V

Pb2+ + 2eminus 997888rarr Pb 119864∘ = minus0126V(1)

Although the above standard electrode potentials of thehalf-reactions are those in the aqueous solution the E∘values may be used as a reference to discuss the roomtemperature solid-solid reaction Obviously the Hminus anionsin the potassium borohydride can very easily reduce theFe3+ Ni2+ and Pb2+cations to their corresponding atomsBecause the electronegativity of iron (18) nickel (19) andlead (19) is less than that of boron (20) the iron nickellead and boron atoms can form the alloy In theory moreFe3+ ion should be reduced by KBH

4

than the Ni2+ and Pb2+ions in the experiment But in fact the content of iron inthe resultants is far less than the amount of iron added inthe experiment Where did the iron go We observed thatthe effluent of the washed the resultants was a pale greenclear liquid The pH of the effluent was measured usingpH paper and pH value of the effluent was about 6 Thisindicated that the effluent did not contain a great deal ofthe Fe3+ ion In order to further study the reason about thereduction of the iron content in the resultants we madethe qualitative experiment to determine the Fe2+ ion in the

effluent and the mix solution of the metal salts The Fe2+ion can form the blood-red complex with phenanthrolineBy the addition of phenanthroline the effluent could becomeimmediately blood-red but themix solution of themetal saltsdid not redden This illustrated the presence of ferrous ionin the effluent In order to demonstrate the validity of theconclusion we used the alkali to form the precipitate andobserved the gradual change on the color of the precipitateWhen the sodium hydroxide solution was added to theeffluent a large amount of white precipitate was formed inthe beginning and then the precipitate turned gradually intodark green After standing for some time the precipitateturned slowly to orange-red This fits well with the colorchange process in which the ferrous ion is precipitated underalkaline condition and then oxidized to iron ion by air Theabove testing results indicate that a part of iron ion in theexperiment is reduced to ferrous ion and is not reducedentirely to ironThe standard electrode potentials of restoringthe ferric ion to ferrous ion and restoring ferrous ion to ironin the corresponding half-reactions are listed as follows

Fe3+ + eminus 997888rarr Fe2+ 119864∘ = 0770V

Fe2+ + 2eminus 997888rarr Fe 119864∘ = minus0407V(2)


It is clear that the iron ion is more easily reduced to theferrous ion Therefore the iron ions in the experiment couldfirst be reduced to the ferrous ions and then the ferrousions were reduced to iron atoms However the reduction ofthe Fe2+ ion to Fe atom is more difficult than the reductionof the Ni2+ ion to Ni atom and the Pb2+ ion to Pb atom Inthis case many irons ions in the reaction are reduced to theferrous ions in a short time but not iron atoms This alsosupports the above composition analyses of the resultantsPerhaps this is why the mole ratio of n(Fe) n(Ni) n(Pb)in the resultants is much less than 100 100 0500 whichis the mole ratio of n(FeCl

3

sdot6H2

O) n(NiCl2

sdot6H2

O) n[Pb(CH

3

COO)2

sdot3H2

O] in the reaction raw materialsThe mole ratios of n(Fe) n(Ni) n(Pb) in the resultants1 2 and 3 are 0394 100 0479 0384 100 0498 and0446 100 0464 respectively Hence the percentagecontent of iron in resultants becomes bigger throughincreasing potassium borohydride addition It is feasible thatthe Fe-Ni-Pb-B alloy nanoparticles are prepared by roomtemperature solid-solid chemical reaction

4 Conclusions

In summary the Fe-Ni-Pb-Bmulticomponent alloy nanopar-ticles can be prepared very easily by a simple solid-solidchemical reaction method at room temperature The advan-tages of this synthetic method are simple and convenientoperation high yield energy saving and being environmen-tal friendly it is in accordance with the requirements ofgreen chemistry The characterization results indicate thatthe resultants are mainly consisted of nanoamorphous phaseand a minute amount of nanocrystalline phase and theaverage diameter is about 25 nm The resultants are all softmagnetic behavior The mole ratio of potassium borohydrideand the metal salts has an obvious effect on the resultants incomposition crystal structure and magnetism

Acknowledgments

This work was supported by the Open Funds of StateKey Laboratory Cultivation Base for Nonmetal CompositeFunctional Materials in China (10zxfk32) and the InnovationFound for Postgraduates of Southwest University of Scienceand Technology (11ycjj04)

References

[1] M Wen M F Zhong K J E Wu et al ldquoSoft magnetic CondashFendashBndashP and CondashFendashVndashBndashP amorphous alloy nano-particlesprepared by aqueous chemical reductionrdquo Journal of Alloys andCompounds vol 417 no 1-2 pp 245ndash249 2006

[2] J K L Lai Y Z Shao C H Shek G M Lin and T LanldquoInvestigation on bulk NdndashFendashAl amorphousnano-crystallinealloyrdquo Journal ofMagnetism andMagneticMaterials vol 241 no1 pp 73ndash80 2002

[3] D S Lee T K Jung M S Kim W Y Kim and H YamagataldquoDevelopment of nano-structured AlndashSindashFe based bulk alloysfrom atomized powdersrdquo Materials Science and Engineering Avol 449ndash451 pp 761ndash764 2007

[4] M Khajepour and S Sharafi ldquoCharacterization of nanostruc-tured FendashCondashSi powder alloyrdquo Powder Technology vol 232 pp124ndash133 2012

[5] Y J Suh H D Jang H ChangW B Kim andH C Kim ldquoSize-controlled synthesis of FendashNi alloy nanoparticles by hydrogenreduction of metal chloridesrdquo Powder Technology vol 161 no3 pp 196ndash201 2006

[6] ZWei Z R Li Z Jiang et al ldquoIn-situ XAFS study on structuresand devitrifications of NindashB nano-amorphous alloysrdquo Journal ofAlloys and Compounds vol 460 no 1-2 pp 553ndash558 2008

[7] D S Lu W S Li X Jiang C L Tan and R H Zeng ldquoMagneticfield assisted chemical reduction preparation of CondashB alloys asanodematerials for alkaline secondary batteryrdquo Journal of Alloysand Compounds vol 485 no 1-2 pp 621ndash626 2009

[8] Y Ge G Ying Z Bangwei W Lingling O Yifang and LShuzhi ldquoPreparation and thermal properties of amorphousFendashWndashB alloy nano-powdersrdquo Journal of Materials ProcessingTechnology vol 74 no 1ndash3 pp 10ndash13 1998

[9] M R Rezvani and A Shokuhfar ldquoSynthesis and characteri-zation of nano structured CundashAlndashMn shape memory alloy bymechanical alloyingrdquoMaterials Science and Engineering A vol532 pp 282ndash286 2012

[10] F R Ai A H Yao W H Huang D P Wang and X ZhangldquoSynthesis of PVP-protected NiPd nanoalloys by modifiedpolyol process and their magnetic propertiesrdquo Physica E vol42 no 5 pp 1281ndash1286 2010

[11] S Gurmen A Guven B Ebin S Stopic and B FriedrichldquoSynthesis of nano-crystalline spherical cobalt-iron (CondashFe)alloy particles by ultrasonic spray pyrolysis and hydrogenreductionrdquo Journal of Alloys and Compounds vol 481 no 1-2pp 600ndash604 2009

[12] Z G Fan and C Y Li ldquoPreparation of NiB alloy from spentNiAl catalysts by induction furnacerdquo Journal of Alloys andCompounds vol 436 no 1-2 pp 178ndash180 2007

[13] M L Yuan J H Tao L Yu et al ldquoSynthesis andmagnetic prop-erties of FendashNi alloy nanoparticles obtained by hydrothermalreactionrdquo Advanced Materials Research vol 239ndash242 pp 748ndash753 2011

[14] C M Chen and J M Jehng ldquoAmination application over nano-MgndashNi hydrogen storage alloy catalystsrdquo Applied Catalysis Avol 267 no 1-2 pp 103ndash110 2004

[15] A Yedra L F Barquın J C G Sal and Q A PankhurstldquoNanoscale alloys prepared by sodium borohydride reductionof aqueous FendashCu and CondashCu solutionsrdquo Journal of Magnetismand Magnetic Materials vol 254-255 pp 14ndash16 2003

[16] V G de Resende E de Grave G M da Costa and J JanssensldquoInfluence of the borohydride concentration on the compo-sition of the amorphous FendashB alloy produced by chemicalreduction of synthetic nano-sized iron oxide particlesmdashpart IIgoethiterdquo Journal of Alloys and Compounds vol 440 no 1-2 pp248ndash253 2007

[17] M Aonuma H Ogawa and Y Tamai ldquoProcess for productionof ferromagnetic powderrdquo USP 4063000A 1977

[18] G Q Zhong H L Zhou and Y Q Jia ldquoA simple method forpreparation of copper nanocrystalline particlesrdquo Nanoscienceand Nanotechnology Letters vol 5 no 7 pp 809ndash812 2013

[19] G Q Zhong H L Zhou J R Zhang and Y Q Jia ldquoA simplemethod for preparation of Bi and Sb metal nanocrystallineparticlesrdquoMaterials Letters vol 59 no 18 pp 2252ndash2256 2005

[20] G Q Zhong H L Zhou and Y Q Jia ldquoPreparation ofamorphous NindashB alloys nanoparticles by room temperature


solid-solid reactionrdquo Journal of Alloys and Compounds vol 465no 1-2 pp L1ndashL3 2008

[21] M L Liu H L Zhou Y R Chen and Y Q Jia ldquoRoom tem-perature solid-solid reaction preparation of iron-boron alloynanoparticles andMossbauer spectrardquoMaterials Chemistry andPhysics vol 89 no 2-3 pp 289ndash294 2005

[22] B Saatci N Maraslı and M Gunduz ldquoThermal conductivitiesof solid and liquid phases in PbndashCd and SnndashZn binary eutecticalloysrdquoThermochimica Acta vol 454 no 2 pp 128ndash134 2007

[23] E A El-Danaf K A Khalil andM S Soliman ldquoEffect of equal-channel angular pressing on superplastic behavior of eutecticPbndashSn alloyrdquoMaterials and Design vol 34 pp 235ndash241 2012

[24] H Xie G C Yang P Q La et al ldquoMicrostructure andwear performance of Nindash20wt Pb hypomonotectic alloysrdquoMaterials Characterization vol 52 no 2 pp 153ndash158 2004

[25] A P Silva A Garcia and J E Spinelli ldquoMicrostructure mor-phologies during the transient solidification of hypomonotecticandmonotecticAlndashPb alloysrdquo Journal of Alloys andCompoundsvol 509 no 41 pp 10098ndash10104 2011

[26] H B Cui J J Guo Y Q Su et al ldquoEffect of Cr addition onmicrostructure and wear resistance of hypomonotectic CundashPballoyrdquoMaterials Science and Engineering A vol 448 no 1-2 pp49ndash55 2007

[27] H Xie J Sun G C Yang Y Z Chen andZ L Lu ldquoLiquid phaseseparation and its thermodynamic description in undercooledNindashPb hypermonotectic meltsrdquoMaterials Science and Engineer-ing A vol 457 no 1-2 pp 33ndash37 2007

[28] J P Monchoux and E Rabkin ldquoMicrostucture evolution andinterfacial properties in the FendashPb systemrdquoActaMaterialia vol50 no 12 pp 3161ndash3176 2002

[29] J H Hsu and Y H Huang ldquoTunnelingmagnetoresistance effectin FendashPbndashO and FendashPbO granular films a comparisonrdquo Journalof Magnetism and Magnetic Materials vol 203 no 1ndash3 pp 94ndash96 1999

[30] F Fang M Zhu H Q Deng X L Shu and W Y Hu ldquoSelf-diffusion of Al and Pb atoms in AlndashPb immiscible alloy systemrdquoMaterials Science and Engineering B vol 108 no 3 pp 253ndash2572004

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CoatingsJournal of

Advances in

Materials Science and EngineeringHindawi Publishing Corporationhttpwwwhindawicom Volume 2014

Smart Materials Research



MetallurgyJournal of


BioMed Research International

MaterialsJournal of


Nano

materials


Journal ofNanomaterials


2 Experimental

All chemicals used in the preparation experiment werein analytical grade which were purchased from ChengduKelong Chemical Reagent Factory in China Ferric trichlo-ride hexahydrate nickel chloride hexahydrate and leadacetate trihydratewereweighed and placed in an agatemortarand mixed up and the corresponding mole ratio of the threemetal salts was 100 100 0500 Then the white potassiumborohydride powder was added to the above mixture andthe mole ratio of the metal salts to potassium borohydridewas 100 125 Immediately the mixture became black andreleased a lot of colorless gas The released gas was testedwith moist pH paper and the result indicated that the gaswas faintly acid gas The reason was that the acetic acid andhydrogen chloride were released in the reaction process Themixture was grinded carefully about 3min and then 2 ofpolyvinylpyrrolidone (PVP) of the total mass of the metalsalts was added to the above agate mortar and the grindingwas kept on about 5minThe reactionwas conducted at roomtemperature Then the resultant was moved to a glass beakeras soon as possible and the resultant was rinsed repeatedlyby deionized water and collected by a centrifugation forremoval of the residual reactants until no chlorine ion inwashed water could be tested by the silver nitrate solutionAfterwards the resultant was washed thoroughly by ethanolto remove residual water in the resultant Finally the resultantwas dried in vacuum at 313 K for 5 h The resultant was fineblack particles and recorded as 1 The same method was usedto prepare resultants 2 and 3 in which the mole ratio ofthe metal salts to potassium borohydride was 100 200 and100 300 respectively

The composition of the resultants was determined bythe inductively coupled plasma-atomic mass spectrometerFirst the sample was solubilized by a certain amount ofconcentrated nitric acidThen the content of the iron nickellead and boron in the sample solution was measured by aThermo X-2 ICP-MS instrument The thermal properties ofthe resultant were examined by a TA Q500 thermogravimet-ric analyzer at a heating rate of 20Kminminus1 and the TG-DTA curves of the resultant were shown in Figure 1 Thepowder X-ray diffraction (XRD) patterns of the resultantswere recorded by a 119863max-II X-ray diffractometer Cu K

1205721

radiation (120582 = 0154056 nm) and Ni filter and scanning ratewas 8∘ (2120579)minminus1 at room temperature The powder X-raydiffraction data of the resultants were collected in the diffrac-tion angle ranges of 3∘ndash80∘ in Figure 2 The morphology andthe particle sizes of the resultant were studied by a TecnaiG20 (FEI) transmission electron microscopy at 300 kV ForTEM observation the samples were dispersed in ethanol byultrasonic treatment and dropped on carbon-copper gridsThe TEM images of the resultant were given in Figure 3 Thesoftmagnetic properties of the resultants were investigated bya BKT-4500Z vibrating sample magnetometer

3 Results and Discussion

The chemical composition and the percentage content ofthe resultants are listed in Table 1 The results of the ICP

300 400 500 600 700 800 900 100075

80

85

90

95

100

Mas

s (

)

minus0010

minus0005

0000

0005

0010

0015

0020

Hea

t flow

(Wg

)

5695 K9942 K

8637 K7002 K

minus1781

T (K)

Figure 1 TG-DTA curves of resultant 2

10 20 30 40 50 60 70 80

(a)

(b)

(c)

2120579 (deg)

Figure 2 Powder X-ray diffraction patterns of the Fe-Ni-Pb-B alloynanoparticles (a) resultant 1 (b) resultant 2 and (c) resultant 3

analysis indicate that the percentage content of iron nickellead and boron in the resultant 2 is 966 2645 4650and 031 respectively The total content of the metals andboron of resultant 2 is about 8292 As the PVP was addedthe total percentage content of the metals and boron is notequal to 100 Therefore the other elements (1708) inthe resultant most possibly come from the PVP and theconjecture is demonstrated in the result of TG-DSC analysisIn addition several compositions of the alloy nanoparticleshave been gained by adding a different ratio of KBH

4

in theexperimental process Increasing the addition of potassiumborohydride fromTable 1 the percentage content of iron andnickel in the resultant is increased This indicates that themole ratio of potassium borohydride to the metal salts hasan obvious effect on the composition of the resultant

The TG-DTA curves of resultant 2 in air from roomtemperature to 1023K are shown in Figure 1 There is anobvious weight loss process in the TG curve below 650KBecause the resultant contains iron nickel lead boron andPVP so the lost component must come from the oxidationand decomposition of PVP The total percentage weight lossis 1781 and it fits right in with the data (1708) of the ICP


(a) (b)









H2







minus20

minus10

0

10

20

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(A)

(B)

(C)

(a)


minus3

minus2

minus1

0

1

2

3

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(b)





4







3

sdot6H2

O) n(NiCl2

sdot6H2

O) n[Pb(CH

3

COO)2

sdot3H2


4 Conclusions


Acknowledgments


References








































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




(a) (b)









H2







minus20

minus10

0

10

20

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(A)

(B)

(C)

(a)


minus3

minus2

minus1

0

1

2

3

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(b)





4







3

sdot6H2

O) n(NiCl2

sdot6H2

O) n[Pb(CH

3

COO)2

sdot3H2


4 Conclusions


Acknowledgments


References








































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials







minus20

minus10

0

10

20

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(A)

(B)

(C)

(a)


minus3

minus2

minus1

0

1

2

3

Mag

netiz

atio

n (e

mu

g)

Magnetic field (Oe)

(b)





4







3

sdot6H2

O) n(NiCl2

sdot6H2

O) n[Pb(CH

3

COO)2

sdot3H2


4 Conclusions


Acknowledgments


References








































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials





3

sdot6H2

O) n(NiCl2

sdot6H2

O) n[Pb(CH

3

COO)2

sdot3H2


4 Conclusions


Acknowledgments


References








































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials






















CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials



research article preparation of soft magnetic fe-ni-pb-b alloy...

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