Microwave Induced Irradiation of Barium Ferrite Prepared by Sol-gel Auto-combustion

A. NURUDDIN1,2*, R. RIADY2 and SUYATMAN1

1 Engineering Physics Research Group, Faculty of Industrial Technology, Institut Teknologi Bandung, Ganesha 10, Bandung 401 !, Indonesia ! "aterials Engineering #tudy Progra$, Faculty of "echanical Engineering and %eronautics, Institut Teknologi Bandung, Ganesha 10, Bandung 401 !, Indonesia & 'orresponding author( e$ail address of corresponding author

Abstract: Effect of microwave irradiation on t e !ro!ertie" of #ari$m ferrite %&aM' wa" inve"ti(ated. &ari$m ferrite !owder wa" ")nt e"i*ed via "o+,(e+ a$to,com#$"tion ro$te, and "$#-ected to microwave radiation wit vario$" !ower and time e.!o"$re". T e !owder !ro!ertie" were e.amined #) /TIR, DTA0T1, 2RD, SEM, and 3SM. It wa" " own t at microwave irradiation en anced t e decom!o"ition and effective+) !re!ared !rimar) !rec$r"or" containin( "in(+e ! a"e #ari$m ferrite of a#o$t 24.5 6 wei( t. Microwave e.!o"$re a+one wa" in"$fficient to !rod$ce "in(+e ! a"e #ari$m ferrite and com!+ete+) remove "econdar) ! a"e #ari$m ferrite, f$rt er ca+cination at 744 o8 i" re9$ired to f$++) attain "in(+e ! a"e #ari$m ferrite wit avera(e !artic+e "i*e of 1:4 nm. Sat$ration % "s at 14;<e' and remanent %"r' ma(neti*ation, and coercivit) %)c' of t e !owder are 5=.> em$0(, >4.1 em$0(, and ?.== ;<e, re"!ective+). Re+ative+) +ow coercivit) i" d$e to in omo(eneit) of t e !owder". Key words: Bariu$ ferrite, "icro*a+e irradiation, #ol,gel auto,co$-ustion, "agnetic properties

1 I!"#$%&'"I$! &ari$m ferrite %&aM' i" a !ermanent ma(net wide+) $"ed for e+ectroma(netic %EM' wave0radar a#"or#er @1A. So+,(e+ a$to,com#$"tion !roce""e" ave #een wide+) $"ed to !re!are #ari$m ferrite !owder @2A. Microwave eatin( wa" ;nown to red$ce !roce""in( time wit o$t "acrificin( 9$a+it) of t e !rod$ct. E.!o"in( t e (e+ d$rin( a$to,com#$"tion !rod$ced "ma++er (rain t an t at treated #) oven eatin( @?A. T i" re!ort !re"ent" t e effect of microwave irradiation on t e cr)"ta++ine "tr$ct$re, !artic+e "i*e and ma(netic !ro!ertie" of #ari$m ferrite. ( )*P)#IM)!"A+ M)",$% T e "tartin( materia+" are !$re rea(ent of ferric nitrat %/e%N<?'?. 7B2<', #ari$m nitrat %&a%N<?'2' a" t e main !rec$r"or", and citric acid %8A' act" a" a c e+atin( a(ent and f$e+. T e mo+ar ratio of &a : /e : 8A i" 1 : 11.C : 2C re"!ective+). NB><B wa" $"ed to ad-$"t t e !B va+$e of ?.>. T e "o+$tion wa" t erma++) de )drated to dr)ne"" and !rior to microwave irradiation at vario$" !ower at time e.!o"$re". T e +oo"e !owder wa" eat treated at vario$" tem!erat$re" ca+cination to revea+ t e evo+$tion of cr)"ta++ine formation. /TIR, 2RD, SEM, and 3SM were em!+o)ed to c aracteri*e t e &aM !ro!ertie".

- #)S&+"S A!% %IS'&SSI$! /i(. 1 " ow" T10DTA c$rve of dr) (e+ eat treated from room tem!erat$re $! to 744o8 wit eatin( rate of 14o80min$te". It i" c+ear+) " own t at t ere i" an

/i(.1. T10DTA c$rve of dr) (e+ e.ot ermic reaction a" indicated #) i( !ea; eat f+ow and "i(nificant "am!+e wei( t +o"". Sam!+e wei( t +o"" of a#o$t 226 at tem!erat$re D ?24o8 i" !rimari+) attri#$ted

to t e eva!oration of )dro.)+ (ro$!. At t i" tem!erat$re ran(e" ferric nitrate and #ari$m nitrate are t erma++) decom!o"ed. In t e !re"ence of citric acid t e decom!o"ition of ferric nitrate can !rod$ce ma( emit % , /e2<?' @>A. A$to,com#$"tion occ$re" w en t e tem!erat$re i" increa"ed to a#o$t ?:>o8 w ere e.ot ermic reaction ta;e !+ace, corre"!ondin( to t e decom!o"ition of t e remainin( or(anic materia+ from citric acid. T i" reaction cea"e" at >44o8 accom!anied #) ?26 weight-loss. Further temperature increases to 900oC there is weight gain corresponding to reaction of all intermediate phase precursors to form barium ferrite.

/i(. 2 " ow" t e 2RD !attern" of "am!+e" $!on microwave e.!o"$re" at different !ower" for 2C min$te". T e &aM !ad of =14 (ram wa" !+aced $nderneat t e "am!+e d$rin( microwave irradiation. It " ow" t at t e microwave !ower of ?:C watt i" "$fficient to decom!o"e t e c e+ated meta+ nitrate" to form intermediate ! a"e of ,/e2<?, &a8<? and &a/e2<>. Bowever, for "am!+e" irradiated at i( er !ower t e diffraction !attern remain" t e "ame. T ere "eem" t at t e microwave ener() i" in"$fficient to eat $! t e "am!+e to !rovide !rec$r"or" reaction to form &a/e12<17. In t i" condition, t ere i" no #ari$m ferrite i" !rod$ced. /i(. ? " ow" t at t e 2RD !attern of t e "am!+e e.!o"ed to microwave wit different wei( t of &aM !ad". Red$cin( t e wei( t of &aM !ad en ance" 2RD !ea; inten"it), w ic mean" more microwave eat i" a#"or#ed #) t e "am!+e t an t at #) &aM !ad. /$rt er ana+)"i" " ow" t at &aM !ad can #e $ti+i*ed to fine t$ne microwave eat into t e "am!+e w ic a""i"t" !rec$r"or reaction" to form "in(+e ! a"e #ari$m ferrite, a" " own in /i(. > #e+ow.

30 2#

BaFe12O19 c%ntent (& 'ei"(t)

20 1# 10 # 0

/i(.2. 2RD !attern" of microwave irradiated "am!+e" at !ower of %a' ?:C watt, %#' C?7 watt, and %c' =44 watt, wit &aM !ad of =14 (r.

(d)
O
X

O F
A HA A F AF

F F FA

F : - Fe2O3 A : BaFe12O19 H : - Fe2O3 O : BaFe2O4 X : BaCO3

100

200

300

400

#00

600

$00

Ba) *ad 'ei"(t ("+a,)

Intensity (a !)

/i(.>. Sin(+e ! a"e #ari$m ferrite content in t e "am!+e.

F F
A

(c)
O

O F
X H A A A F

F FAA F

(b) (a)

OF O
X X

F
H A A A AF

F FA A F AF F

O F AHA

AF

20

40

60

80

2 (de" )

/i(.?. 2RD !attern" of microwave irradiated "am!+e" at !ower of C?7 watt wit &aM !ad wei( t of %a' =14 (r., %#' >C= (r., %c' 21C (r., and %d' 7= (r.

Sin(+e ! a"e #ari$m ferrite of a#o$t 24.5 6 wei( t can #e !rod$ced #) !+acin( 7= (ram &aM !ad $nderneat t e "am!+e. T e concentration tend" to decrea"e a" t e &aM !ad wei( t wa" added. No "in(+e ! a"e #ari$m ferrite wa" !rod$ced for =14 (ram &aM !ad. Noted a++ "am!+e" were e.!o"ed to C?7 watt microwave !ower for 2C min$te". In t e c$rrent condition", owever, "in(+e ! a"e #ari$m ferrite co$+d not #e f$++) !rod$ced #) mere+) e.!o"in( t e microwave to "am!+e. In"tead, microwave irradiation i" effective mean" for !rod$cin( intermediate ! a"e !rec$r"or" %&a8<?, /e2<?, &a/e2<>'.

(b)
-+ans,ittance (a ! ) CO3
2-

BaFe2O4 Fe-O

(a)

CO3 O-H COO COO

3000 2500 2000
-

2-

4000

3500

1500
-1

1000

500

.a/en!,be+ (c, )

/i(.C. /TIR !attern" of %a' dr) (e+, and %#' microwave irradiated "am!+e. /i(.C " ow" /TIR !attern of dr) (e+ and microwave irradiated "am!+e for 2C min$te" wit !ower of C?7 watt and &aM !ad of >C= (ram. In dr) (e+, t e #road #and" at ?444,?C44 cm,1 are d$e to <,B "tretc in( from citric acid. Since t ere i" no #and at a#o$t 15C4 cm ,1 w ic i" a"cri#ed to B,<,B #endin( vi#ration, it indicate" t at "am!+e i" f$++) dr). Two #and" centered at 154> cm ,1 and 1>44 cm,1 corre"!ond to 8<<, anti,")mmetrica+ "tretc in( and 8<<, ")mmetrica+ "tretc in( mode", re"!ective+) @CA. T e"e +i(and" c e+ate t e meta+ ion" to form com!+e. coordination @5A. T e !ea; at 14C4 cm ,1 remain" $na""i(ned. T e #and at 57= cm,1 i" o#"erved for 8<?2,, and t e #road #and a!!ear" #etween >C4 and 544 cm,1 i" c aracteri"tic of /e,<B "tretc in(.

<,B and 8<<, #and" di"a!!ear, in"tead t e #and at 1>?C cm,1, =5: cm,1 and 51= cm,1 a!!ear corre"!ondin( to 8<?2,, &a/e2<> and ,/e2<?, re"!ective+). T e #and" at C=: and >2: cm,1 are a"cri#ed to /e,< @=,14A. /i(. 5 " ow" 2RD !attern" of microwave irradiated "am!+e" ca+cined at different tem!erat$re". 8a+cination t e "am!+e at 544o8 a" no "i(nificant effect on t e diffraction !attern. E en t e tem!erat$re ca+cination" i" increa"ed to :44o8 "in(+e ! a"e #ari$m ferrite i" form wit t e remainin( &a/e2<>. T i" intermediate ! a"e #ari$m ferrite com!+ete+) di"a!!eared w en t e "am!+e i" ca+cined at 744o8. /or com!ari"on, t e "ame re"$+t wa" o#tained for t e dr) (e+ direct+) ca+cined wit conventiona+ oven at 744o8 for ? o$r". Sc errer ca+c$+ation of t e 2RD +ine #roadenin( for t e i( e"t !ea; inten"it) !rovided avera(e cr)"ta++ite "i*e of >2 nm. T e"e "am!+e" were "$#-ected to f$rt er c aracteri*ation" to revea+ t e "$rface mor! o+o() and ma(netic !ro!ertie".

/i(.=. SEM ima(e" of "am!+e ca+cined at 744o8.

a a a a a a a a a a F F a a a a a

(c)
Intensity (a ! )

a a a a

F : - Fe2O3 a : BaFe12O19 H : - Fe2O3 % : BaFe2O4 0 : BaCO3 a a

a a a

(b) a a a (a)
a 0

%FH F a a a a

20

40

60

80

2 (de"+ee)

/i(.5. 2RD !attern" of microwave irradiated "am!+e" and ca+cinated at %a' 544o8, %#' :44o8, and %c' 744o8 for 1 r. After microwave e.!o"$re at C?7 watt for 2C min$te",

/i(.?. 3SM (ra! of &aM ca+cined at %a' :44o8, %#' 744o8. /i(. = " ow" t e SEM micro(ra! of #ari$m ferrite !owder ca+cined at 744o8. T e mor! o+o() of !artic+e" i" !+ate,+i;e " a!e. T e !artic+e orientation i" random wit

rat er #road !artic+e "i*e di"tri#$tion. T e avera(e !artic+e "i*e wa" mea"$red a" a#o$t 1:4 nm, w ic i" +ar(er t an t e avera(e cr)"ta++ite "i*e. T i" "$((e"t" t at eac (rain a((re(ate a#o$t five cr)"ta++ite". /i(. : " ow" t e 3SM ma(neti*ation )"tere"i" +oo! of t e !owder ca+cined at :44 and 744 o8 mea"$red at room tem!erat$re. T e " a!e of #ot c$rve" are 9$iet "imi+ar, #$t i( er ca+cination" tem!erat$re !rod$ce" +ar(er ma(neti*ation and coercivit). T e "at$ration %"s at 14;<e', remanent %"r' ma(neti*ation, and coercivit) %)c' of t e !owder ca+cined at 744o8 are 5=.> em$0(, >4.1 em$0(, and ?.== ;<e, re"!ective+). /or coma!ri"on, t e t eoretica+ ma(neti*ation va+$e ca+c$+ated for "in(+e cr)"ta+" of #ari$m ferrite i" =2 em$0( @11A. Re+ative+) +ow coercivit) i" d$e to in omo(eneit) of t e !owder". . '$!'+&SI$!S Microwave irradiation" ave #een effective+) $"ed for !rod$cin( #ari$m ferrite !owder. Dr) (e+ meta+,nitrate" can #e i(nited and a$to,com#$"ted #) moderate microwave !ower for re+ative+) " ort time com!arin( to t e conventiona+ !roce"". T e (e+ f$++) decom!o"ed into main !rec$r"or" for !re!arin( #ari$m ferrite. Bowever, microwave irradiation a+one co$+d not com!+ete+) tran"form t e !rec$r"or" to !rod$ce "in(+e ! a"e #ari$m ferrite. /a"t eat treatment a" !rod$ced !+ate+ate,+i;e " a!e and "ma++er (rain "i*e of #ari$m ferrite wit in omo(eneo$" di"tri#$tion. T i" !ro!ertie" !rod$ce re+ative+) i( "at$ration ma(neti*ation #$t red$ce t e coercivit). Ac/nowledgments T i" wor; i" financia++) "$!!orted #) IT& FF,Re"earc 1rant. #)F)#)!')S
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