7 8 0 2 : N S S I – 5428
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1 1LaboratoirumMateira,lJ urusanFisika ,FMIPA ,Universtia sRiau m a n a P 5 , 2 1 M K s a t n a r b e o S R H . l J -PekanbaruRiau 2Insttiuteo fMicroengineeirngandNanoelecrtonics r o g n a l e S , i g n a B 0 0 6 3 4 , a i s y a l a M n a a s g n a b e K y ti s r e v i n U -Malaysia 7 5 0 0 9 6 1 8 2 1 8 0 . p l e T * k u , o c . o o h a y @ o n o t _ n a w i :l i a m e a r t s b A c t Metal snanoparitcle s(plaitnum-PtN sand palladium-PdNs )have successfullybeen e h T . s r o t c e ll o c t n e r r u c l e e t s s s e l n i a t s d n a s e d o rt c e l e n o b r a c f o e c a f r u s e h t n o n w o r g . d o h t e M l a c i m e h C t e W g n i s u t u o d e ir r a c n e e b e v a h s N d P d n a s N t P f o s h t w o r g s n o it a z ir e t c a r a h C o fthe PTN sand PdN shave been performed by using FESEM X ( D R X d n a ) y p o c s o r c i M n o rt c e l E g n i n n a c S n o i s s i m E d l e i F ( -RayDfifraciton )fo r f o e c n a m r o f r e p e h t t s e t o t r e d r o n i , e li h w n a e M . s e i d u t s l a r u t c u rt s d n a l a c i g o l o h p r o m c e l E e c n a d e p m I , s ll e c r o ti c a p a c r e p u s rtochemica lSpecrtoscopy (EIS )ha sbeen e h t n o y l m r o fi n u w e r g s N d P d n a s N t P t a h t d e m ri f n o c s tl u s e r t n e m ir e p x e e h T . e n o d e h t t a h t d e m ri f n o c n r e tt a p D R X e h T . l e e t s s s e l n i a t s d n a s e d o rt c e l e n o b r a c f o e c a f r u s w t y b d e t n e s e r p e r e r e w s e t a rt s b u s e h t n o n w o r g s N t P oXRDpeak sa t2θ=40.247o d n a 46.815owtiht hei rcrystallographicplane so f(111 )and(200) .Meanwhlie,t wo t a s k a e p 2θ=40.225° da n 2θ=46.713°r epresentedPdN sgrownont hesubsrtates . f o s e c n a ti c a p a c c if i s e p s e h t d e tl u s e r s t n e m e r u s a e m S I E supercapactio rcell so f8.81 e h T . y l e v it c e p s e r , s N t P t u o h ti w d n a h ti w s e d o rt c e l e n o b r a c e h t r o f r g / F 2 . 0 2 d n a f o s e c n a ti c a p a c c if i s e p s e h t f o g n i v o r p m i n i d e tl u s e r s ll e c e h t n o s N d P f o n w o r g .r g / F 2 2 . 0 1 o t r g / F 1 8 . 8 m o r f s ll e c r o ti c a p a c r e p u s s d r o w y e K : Impedance Electrochemica l Spectroscopy , Meta l nanoparitcles, s r o ti c a p a c r e p u S ..
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l u p m u g n e p n a d n o b r a k a d o rt k e l e a r a t n a k a t n o k s a ti l a u K t a p a r ( i s a t s e r p n a k u t n e n e m t a g n a s ) r o t c e ll o c t n e r r u c ( s u r a ) i s n a d e p m i n a d p u d i h s u l k i s , y g r e n e superkapastio relek -a i m i k o rt [Wu ,F.C. ,e.ta.l ,2004] .Sejauh ini ,beberapa s u r e t a y a p u dliakukanuntukmeningkatkankualtia skontak n a g n e d : a y n a r a t n a i d , t u b e s r e t penambahanlapisan karbon [P .L .Taberna ,e ta.l ,2006] nd a lapisanema s[C -hiChang , u H e ta.l ,2004] pada curren tcollector. Penumbuhan na -l e k it r a p o n logam pada permukaan elekrtoda karbon dan r o t c e ll o c t n e r r u c diharapkan dapa tmeningkatkan prestasi r o ti s a p a k r e p u s elekrtokimia. Bahan logam yang dapa t n a k a n u g i d dianraranya adalah plaitnum dan palladium, a n e r a k mempunyais fia tkatail syangbaik. Plaitnumdanpalladium [Deraman ,e ta.l ,2002 ]dapa t n a h a b m a n e P . o n a n r u t k u rt s m a l a d n a k h u b m u ti d l e k it r a p o n a n logam plaitnum dan palladium pada bahan r o p a li d h a l e t g n a y i tr e p e s n a k u k a li d t a p a d h a l e t n o b r a k kan [Koga ,H. ,e tal ,2009 ;Longl iBo ,e ta.l ,2008] . Nanoparitke l logam (plaitnum dan palladium ) h u b m u ti d kan pada permukaan elekrtoda karbon dengan n a g n e d n a k li s a h i d n o b r a k a d o rt k e l E . h a s a b a i m i k e d o t e m n a k r o p a l i m a k h a l e t g n a y e d o t e m n a k a n u g g n e m u l e b e s mnya [Gang Chang , e t a.l , 2007] . Penguijan l e k it r a p o n a n n a h u b m u n e p p a d a h r e t logam dliakukan i u h a t e g n e m k u t n u X D E n a d M E S n a k a n u g n e m n a g n e d g n a y m o t a e s a t n e s r e p a tr e s s i n e j n a d r u t k u rt s o rt k i m n a k g n a d e S . n a k u k a li d a g u j D R X n a ij u g n e P . n a k li s a h i d t n e n e m k u t n u ukan nlia i kapastians i spesiifk se l e d o t e m n a k a n u g g n e m r o ti s a p a k r e p u s Elecrtochemica l n a d e p m I ceSp c se rtocopy( EIS.)I
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n a h u b m u n e p m a l a d n a k a n u g i d g n a y a m a t u n a h a B : h a l a d a m a g o l l e k it r a p o n a n K2PtCl4 ,K2PdCl6,ascorbi tacid , n a t u r a l LP %L 5 , tirsodiumsirta t0, 10 M , NaBH40,1 M , 0 B A T C ,1 M , NaOH0,1Mdanai rmurni .Sedangkanala t i s a s ir e t k a r a k n a d n a h u b m u n e p k u t n u i a k a p i d g n a y a m a t u , e c a n r u f , h t a b c i n o s a rt l U : h a l a d a m a g o l l e k it r a p o n a n , r u k u s a l e g , l a ti g i d n a g n a b m it Penguijan SEM dliakukan D R X n a ij u g n e p n a k g n a d e s , v p 5 5 a r p u s l e d o m t a l a n a g n e d X d e c n a v d A r e k u r B t a l a n a k a n u g g n e m n a k u k a li d -Ray 8 D l e d o m ) S X A ( n o it u l o S danSolartoni nterface1286. k u t n u n a k a n u g i d ) l a c i m e h c t e w ( h a s a b a i m i k e d o t e M n a d m u n it a l p ( m a g o l l e k it a p o n a n n a k h u b m u n e m ll a p adium) .Penumbuhan nanopaitke lplaitnum dliakukan n o b r a k a d o rt k e l e m a d n e r e m n a g n e d dan pengumpu laru s t i b r o c s a i s a rt n e s n o k n a g n e d n a h u b m u n e p n a t u r a l m a l a d 2 , 0 d i c a Mdanl arutanpenumbuhplaitnum(K2PtCl4 )1M . p s e s o r P enumbuhan dliakukan dua kal i (mulitgrowth ) n a k g n a d e S . m a j 4 + m a j 4 u t k a w n a g n e d Nanoparitke l n a g n e d n a k h u b m u ti d m u i d a ll a p 2t ahap :pembenihandan n a g n e d n a k u k a li d n a h i n e b m e P . n a h u b m u n e p merendam % 5 L L P n a t u r a l a d a p t a rt s b u s dan selanjutnya sampe l a d n e ri d m dalam larutan pembeniha n yang merupakan 0 n a r u p m a c ,5 m lK2PdCl60,01 M; 0,5 mlt irsodiumsirta t 0, 10 M; 02 m lai rmurn idan 0,5 m lNaBH4 0,1 M . , ri h k a r e T sampe ldriendam selama 5 jam pada larutan h u b m u n e p ,yatiu campuran 20 m lCTAB 0,1 M; 0,5 lm K2PdCl6 0, 01M ;larutan0,5m lNaOH0,1M danl arutan d i c a d i b r o c s a . M E S e d o t e m n a g n e d n a k u k a li d l e p m a s i s a s ir e t k a r a K r o ti s a p a k r e p u s l e s i s a t s e r p i j u n a g n a d e s , D R X n a d X D E . S I E e d o t e m n a g n e d n a k u k a li d Untukmenentukansrtuktu r i h u b m u ti d h a l e t e s k u t n e b r e t g n a y n o b r a k a d o rt k e l e l e k it r a p o n a n logam ,pelru dliakukan uj iSEM dan XRD . n a ij u g n e P in i dliakukan untuk meninjau morfolog i a d o rt k e l e n a a k u m r e p karbon dan distirbus ipenumbuhan m u n it a l p l e k it r a p o n a n d an palladium yang dihaslikan . , v p 5 5 a r p u s l e d o m t a l a n a g n e d n a k u k a li d M E S n a ij u g n e P t a l a n a k a n u g g n e m n a k u k a li d D R X n a ij u g n e p n a k g n a d e s X d e c n a v d A r e k u r B -RaySoluiton(AXS) mode lD8 .Uj i e s a t n e s o r p i u h a t e g n e m k u t n u n a k u k a li d a g u j X D E m u n it a l p danpalladiumyangt umbuh. i s a t s e r P kapasiit fsampe ldiinvesitgas idengan metode n a r u k u g n e p E IS dalam se lsuperkapastior yang dibua t n a k a n u g g n e m curren tcollecto rstainles ssteel ,separato r H n a t u r a l t il o rt k e l e n a d n o lf e t n i c n i c 2SO4. Elekrtodakejra a r u k u n a g n e d t a u b i d n ,massadant eba lmasing-masing 80 – 90 mg dan0.4-0.5 mm .Elekrtoil tdisalurkandalamse l u g g n u ti d h a l e t e S . i s k e j n i a r a c n a g n e d r o ti s a p a k r e p u s ti n e m 0 3 a m a l e s ,kemudianpengukurandliakukan.
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d a p m u n it a l p l e k it r a p o n a n n a h u b m u n e p l i s a H apermukaan i s a rt n e s n o k n a g n e d n a k p a i s i d g n a y n o b r a k a d o rt k e l e K i s a rt n e s n o k n a d M 2 , 0 d i c a d i b r o c s a 2PtCl4 M1 nd a n a k li p m a ti d m a j 4 + m a j 4 m u m it p o n a h u b m u n e p u t k a w a d a p Gamba r1 .Sedangkan nanoparitke lpalladium pada i s a rt n e s n o k n a g n e d n o b r a k a d o rt k e l e ascorbidacid0,4 M ; 0 B A T C ,1 M dan K2PdCl6 0,01 M idperilhatkan pada . 2 r a b m a G Gamba r1 dan 2 memperilhatkan bahwa nanoparitke l m u n it a l p danpalladiumyangt umbuhberbentuk bula tdan l a p m u g r e b -gumpal .Nanoparitke ltersebut tumbuh merata g n a y l e k it r a p n a r u k u n a g n e d n a a k u m r e p n a i g a b h u r u l e s e k a m a s d anmerata( unfiorm.) Ukuranr ata-ratananoparitke l m u n it a l p dan palladium yang tumbuh adalah betrurut -6 , 4 2 r a ti k e s t u r u t -26,8nm(untukplaitnum )dan1 -6.724.6 m n (untukpalladium). In imenunjukkandenstia sparitke l .r a s e b g n a y ) a ( ( b) 1 r a b m a G . Nanoparitke lplaitnumpadaelekrtodakarbon 0 0 0 . 0 0 1 ) b ( n a d i l a k 0 0 0 . 0 1 n a r a s e b r e p ) a ( il a k 2 r a b m a G . Nanoparitke l palladium pada elekrtoda ) b ( n a d i l a k 0 0 0 . 0 1 n a r a s e b r e p ) a ( n o b r a k 0 0 0 . 0 0 1 ilk a a y n t u j n a l e S hasi luj iEDXuntuknanoparitke lplaitnum m u i d a ll a p n a d diperilhatkanpadaGamba r3danGamba r4 , t u r u tr e b -turut .Prosentaseseitapelemenyangt erdapa tpada X D E i j u l i s a h i r a d l e p m a s diperilhatkanpada Tabe l1dan . 2 l e b a T . 1 l e b a T Prosentaseelemenpadas ampelplaitnum n e m e l E Weight% Atoms% C 15.78 66.39 O 4 .07 12.85 t P 80.15 20.76 l a t o T 1 00 1 00 2 l e b a T .Prosentaseelemenpadas ampe lpalladium n e m e l E Weight% Atoms% r C 18.12 19.37 e F 72.66 72.33 i N 8 .22 7 .78 d P 1 .00 0 .52 l a t o T 1 003 2 1 i r a D Gamba r3 dan4s etraTabe l1dan2terilha tbahwa l e k it r a p o n a n a w h a b i u h a t e k i d X D E m u rt k e p s n a k r a s a d r e b m u n it a l p dan palladium memang tumbuh d ipermukaan r o t c e ll o c t n e r r u c n a d n o b r a k stainles ssteel .Prosentase h u b m u t g n a y m u n it a l p l e k it r a p o n a n t a r e b sebesar80,15% ) m u i d a ll a p ( % 0 0 , 1 n a d ) m u n it a l p ( sedangkan prosentase % 6 7 , 0 2 a y n m o t a t a r e b (plaitnum )dan0,52%( palladium). . 3 r a b m a G EDXnanoparitke lplaitnumpada karbon 4 r a b m a G . EDX nanoparitke l palladium pada stain -s s e l .steel u l i s a H j - iXRayDfifracitondiperilhatkanpadaGamba r g n a y , ) m u i d a ll a p ( 6 r a b m a G n a d ) m u n it a l p ( 5 s a l e j n a g n e d n a k t a h il r e p m e m penambahan puncak pada e k it r a p o n a n n a h a b m a n e p n a g n e d n o b r a k a d o rt k e l e l a d a p m u n it a l p sudu t2θ = 40.163° dan 2θ = 46,761° a d a p m u i d a ll a p l e k it r a p o n a n n a h a b m a n e p n a d ) 5 r a b m a G ( 5 2 2 . 0 4 = θ 2 t u d u s ° dan 2θ = 46.713 ° (Gamba r 6). m o t a n a ri d a h e k t a b i k a a g u d i d i n i k a c n u p n a h a b m a n e P m u n it a l p danpalladium. . 5 r a b m a G Dfiraktogram XRD dar isampe lyang telah i d m u n it a l p l e k it r a p o n a n n a k h u b m u ti d . a y n s a t a s n a ij u g n e P e l superkapastio r elekrtokimia dengan n e m ggunakanperalatanElec crt h io e cm alI nterfaceSolarton . 0 8 2 1 Nyquis tplo thasi lpengukuran tersebu tuntuk sel r o ti s a p a k r e p u s dengan elekrtoda karbon yang telah r a b m a G a d a p n a k k u j n u ti d m u n it a l p l e k it r a p o n a n i h u b m u ti d . 8 r a b m a G a d a p n a k k u j n u ti d m u i d a ll a p k u t n u n a k g n a d e s , 7 t o l p t s i u q y N terdri i dar i itga bagian , yatiu bahagian rt s n a k k u j n u n e m g n a y n a r a k g n il h a g n e t e s uktu r yang s u r u l s ir a G . a d o rt k e l e i r o p r e b yangmembentuksudu t45 º i s u f fi d a y n i d a jr e t n a k k u j n u n e m id dalam karbon pellet , g n a d e s gair s tegak luru s pada frekuens i rendah a fi s n a k u j n u n e m tkapasiit fdar ielekrtod a. r a b m a G 6. Dfiraktogram XRD dar i sampe l yang g n u d n a g n e m nanoparitke lpalladium ) a ( ) b ( 7 r a b m a G .Nyquis tplo tse lsuperkapastio rdengannano -a d a p m u n it a l p l e k it r a p frekuensi( a )10.000- n a r a s e b r e p ) b ( z H 1 , 0 (a )pada frekuens i 0 0 0 . 0 1 - 3.000Hz t a p a d n a i d u m e k a k a m , s a t a i d t o l p t s i u q y N i r a D r o ti s a p a k r e p u s l e s i r a d k if i s e p s i s n a ti s a p a k i a li n n a k u t n e ti d t e l e p a d o rt k e l e n a k a n u g g n e m g n a y t u b e s r e t a i m i k o rt k e l e o n a n i h u b m u ti d h a l e t g n a y n o b r a k paritke lplaitnum dan i s n a ti s a p a k i a li n n a k t a h il r e p m e m 3 l e b a T . m u i d a ll a p n a k r a s a d r e b n a g n u ti h r e p l i s a h r o ti s a p a k r e p u s l e s k if i s e p s .) 8 n a d 7 r a b m a G ( t o l p t s i u q y N t u b e s r e t 3 l e b a T i r a D dapa tdiilha tbahwa tejrad ipe -n a ti s a p a k i a li n n a t a k g n i n s ispesiifkdar ise lsuperkapastio r m u n it a l p l e k it r a p o n a n n a h u b m u n e p n a k u k a li d h a l e t e s dan l e s k if i s e p s i s n a ti s a p a K . n o b r a k a d o rt k e l e a d a p m u i d a ll a p rt k e l e n a k a n u g g n e m n a g n e d a i m i k o rt k e l e r o ti s a p a k r e p u s o -H t il 2SO4 1M sebelum dtiumbuhkan nanoparitke llogam 8 r a s e b e s h a l a d a ,82F/g .Nlia ikapastians ispesiifk( Csp)i n i r a ti k e s k i a n g / F 0 2 , 0 2 i d a j n e m n a k if i n g i s a r a c e s k i a n r a ti k e s u a t a ) m u i d a ll a p ( g / F 2 2 , 0 1 n a d ) m u n it a l p ( , % 0 3 2 u ti d m u i d a ll a p n a d m u n it a l p l e k it r a p o n a n h a l e t e s % 0 6 1 m -C i a li N . n o b r a k t e l e p a d o rt k e l e s a t a i d n a k h u b spt eritngg i n a k a n u g g n e m a k it e k i a p a c i d ) m u n it a l p ( g / F 6 6 , 1 2 r a s e b e s ) m h O (" Z 0 2 4 6 8 10 ) mh O(' Z 0 2 4 6 8 0 1 M 1 M 5 , 0 M 5 2 , 0
4 2 1 n a k g n a d e S . M 5 , 0 r a s e b e s t il o rt k e l e n a t u r a l i s a rt n e s n o k n it r e t i a li n , m u i d a ll a p l e k it r a p o n a n n a g n e d l e p n a s a d a p g ig t il o rt k e l e i s a rt n e s n o k a d a p i d a jr e t y n k if i s e p s i s n a ti s a p a k . M 1 r a s e b e s ) a ( ( b) 8 r a b m a G . Nyquis t plo tse l superkapastio r elekrtoda a d a p m u i d a ll a p l e k it r a p o n a n n a g n e d n o b r a k 0 0 0 . 0 1 . ) a ( i s n e u k e r f -0,1 Hzdan(b) .10.000 – 3.000Hz . 3 l e b a T Paramete rse lsuperkapastio relekrtoda karbon m u n it a l p l e k it r a p o n a n a p n a t n a d n a g n e d l e S s R R ” Z m C sp ) m h O ( (Ohm) (Ohm) ( g) (F/g) M 1 C 0 ,69 0 ,22 62,03 0,0582 8 ,82 M 1 t P + C 40 , 0 ,15 27,99 0,0564 20,20 6 5 , 0 M 5 , 0 t P + C 0 ,22 23,99 0,0613 21,66 8 5 , 0 M 5 2 , 0 t P + C 0 ,27 50,68 0,0659 9 ,54 M 1 d P + C 0 ,62 0 ,26 42,96 0,0726 10,22 8 5 , 0 M 5 , 0 d P + C 0 ,38 55,15 0,0710 8 ,14 4 8 , 0 M 5 2 , 0 d P + C 0 ,58 81,94 0,0741 5 ,24 n a g n e r e t e K : C:Karbon ; M:Molartias ;Pt : Nanoparitke l k r e p u s l e s n a n a h a T : R ; ti l o rt k e l e n a n a h a T : s R ; m u n it a l P a ; a d o rt k e l e u t a s a s s a M : m ; r e n ij a m i n a d e p m I: ’ Z ; r o ti s a p k if i s e p s i s n a ti s a p a K : p s C
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