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3 1 1997 2 EL ECTROCH EM ISTR Y o l 3 N o 1 Feb 1997 96 ( 361005) XP24 XP27, 0 5 3 5 A gdm 2, 40 60, 1 05, ; ; XP24 XP27, 2,,,, [ 1 ] [ 2 14 ] [ 15 19 ],,,, 1 1 2 JW Y30S 791 P ine RD E4 3033 X2Y ( 0 196 cm 2 ), P t ( ), 50 m gs 1996210220 ; XP24 XP27 PPS FF

104 1997 70% PD 21,, 100 m s, Μ 1 2 (m o lgl ) : Pd (N H 3) 2C l2 0 1, K 3C 6H 5O 7 H 2O 0 3, (N H 4) 2C 2O 4 H 2O, 0 3, XP24 0 03 ggl, XP27 0 3 ggl : 0 5 3 5 A gdm 2, 50, ph 7 0,, 2 2 1 [ 20 21 ] 1 XP24 XP27 (267 m l), 50, 5 m in, 0 5 A,, 1 267 m l, 0 5 A, 5 m in, 50, (ggl ): 1, ; 2, XP24 0 015+ XP27 0 15; 3, XP24 0 03+ XP27 0 3 ( 0 1 mm ) F ig 1 Effects of the additives on the brigh t ranges of the depo sits ( 1), 8 9 cm, ; XP24 0 015 ggl XP27 0 15 ggl ( 2), ; XP24 XP27 0 03 0 3 ggl ( 3), XP24 XP27, XP24 XP27, [ 21 ] (> 5 [ 5 6 Λm ) Α Β ], PPS 0 2 ggl, XP24 XP27 0 012 ggl 0 12 ggl, 0 5 cm,, FF 3 ggl 2 2 1, [ 5 6 ], ;,

1 : 105 1 T ab 1 Surface mo rpho logy of palladium electrodepo sit A gdm 2 Λm CugN igpd 1 5 6 7,,, 75 CugN igpd i c p= 2 2 i a p= 0 5 Λm, 105 Λm 7 4,,,, 75 Λm, 50 Λm 2 3 2 ( ) XP24 0 03 ggl ( 2) XP24 0 03 ggl + XP27 0 3 gg L ( 3) 2 ( 1) - 0 45,, - 0 85, - 1 06, 0 [ 3 ], 1 05 2 (S = 0 196 cm 2 ), - 0 88 50 m gṡ 1, ; 2, - 0 70, XP24 0 03 ggl ; 3, XP24 0 03 ggl + XP27 0 3 ggl F ig 2 Cyclic vo ltammogram s on glassy carbon electrode in the bath of [ 22 ] palladium 2 Tab 2 Experim ental results from cyclic vo ltammogram s on glassy carbon electrode in the bath of palladium Υ a p, i a p, ma gcm 2 Υde, Υ, Υ c p, i c p, ma gcm 2 ih, ma gcm 2-0 003 23 1-0 846-0 696-1 061 34 1 43 6 0 78 XP24 (0 03 ggl ) + 0 086 21 0-0 954-0 664-1 123 36 1 31 8 1 14 XP24 0 03 + 0 054 11 4-1 091-0 965-1 360 30 3 13 9 2 18 XP27 0 3 (ggl ) c ipgih,

106 1997,, 1, XP24 0 03 ggl ( 2) 108 m, ( ) 31 8 ma gcm 2 ; XP24 0 03 ggl XP27 0 3 ggl, 245 m, 13 9 ma gcm 2 XP24 XP27, XP24 XP27, ipgih c 3 1,, E = - 0 83 ; 2, XP2 4 0 03 ggl + XP27 0 3 ggl E = - 1 12 F ig 3 Po tentio static instantaneous curves from the bath w ithout additive (E = - w ith additives(e = - 1 12 ) 0 83 ) and 4 I 2 gi m tgtm 2 1, 2, E = - 0 83 ; XP24 0 03 ggl + XP27 0 3 ggl E = - 1 12 F ig 4 D im ensionless I 2 gi 2 m tgtm figures on the po tentio static instantaneous curves 2 4 3 ( 1) XP24 0 03 ggl + XP27 0 3 ggl ( 2) i t,, [23 ] I 2 gi 2 m tgtm : I 2 gi 2 m = 1 9542g(tgtm ) {1- exp [- 1 2564 (tgtm ) ]} 2 ( ) I 2 gi 2 m = 1 2254g(tgtm ) {1- exp [- 2 3367 (tgtm ) ]} 2 ( ) 4 I 2 gi 2 m tgtm,, XP24 XP27 2

1 : 107 A Study on the E lectrodepo sition of Palladium and it s N ucleation Yang Fangzu Xu Shukai Yao Sh ib ing Chen B ingyi Zheng Xueqing Zhong X iaohu i Zhou Shaom in (Chem D ep ṫ, Insti of P hy s Chem X iam en U n iv, X iam en 361005) A bs tra c t T he electrodepo sition and nucleation of palladium are studied in the sys2 tem of po tassium citrate and amm on ium oxalate T he resu lts show that, w ith the additives of XP24 and XP27 p repared in ou r labo rato ry, a fu ll b righ t palladium electrodepo sits w ill be ob tained in the w ide ranges of the cathode cu rren t den sities 0 5 3 5 A gdm 2 and tem pera2 tu re 40 60 ; the qualities of the th ick depo sits w ill be effectively im p roved by m ean s of pulse cu rren t p lating Cyclic vo ltamm ogram s resu lts show that the division of peak s betw een anodic and cathodic on the electrode p rocess of palladium w ill be up to 1 05, w h ich show s the irreversib le electrode p rocess; and a inductive cu rren t cycle is appeared,w h ich m ean s the p rocess of nucleation; XP24 and XP27 inh ib it bo th palladium electrodepo sition and hydrogen evo lu tion, therefo re cau se the depo sition po ten tial of palladium to m o re negative; po ten tial step experim en ts fu rtherly show that the nucleation of palladium obeyed p rogressive un2 cleation m echan ism bo th w ith the studied additives o r w ithou t them Ke y w o rds Palladium, E lectrodepo sition, N ucleation, Pu lse electrop lation Re fe re nce s 1 Ronald J M o rrissey R hodium p lating P lating and S u rf ace F inish ing, 1995, 82 (8): 69 2 Jo seph A A byṡ Palladium p lating P lating and S u rf ace F inish ing, 1995, 82 (8): 67 68 3 L E Penven R, L evason W, P letcher D Studies of palladium electrodepo sition from bath s based on Pd (N H 3) 2X 2 Saltṡ I: [Pd (N H 3) 2C l2 ] bath ṡ J A pp l E lectrochem, 1992, 20: 399 404 4 L E Penven R, L evason W, P letcher D Studies of palladium electrodepo sition from bath s based on Pd (N H 3) 2X 2 Part II: X= B r and X= NO 2 J A pp l E lectrochem, 1992, 22: 421 424 5 Jayak rishnan S, N atarajan R S H ydrogen codepo sition in palladium p lating M etal F inish ing, 1991, 89 (1): 23 25 6 L ai C K, W ang Y Y, W an C C Palladium electrodepo sition from ammonia2free electro lyte J E lec2 troanal Chem, 1992, 322: 267 278 7 Su2Il Pyun, Chan L im A sutdy on the electrodepo sition m echanism of p lalladium from ammoniacal so lu2 tion using a ro tating P t R ing2cu disk electrode T R ansactions of the Institu te of M etal F inish ing, 1993, 71 (4): 156 160 8 Strasch il H K, A bbys J A, Kudrrak E J et al N ew palladium strike imp roves adhension and po ro sity M etal F inish ing, 1992, 90 (1): 42 47

108 1997 9 Kudrak E J, A bbys J A, Ch inchankar, J J M aisano Po ro sity of compo site palladium, palladium 2nickel and go ld electrodeo sitṡ P lating and S u rf ace F inish ing, 1992, 79 (2): 49 55 10 Enyo M, B isw as P C H ydrogen abso rp tion in palladium electrodes in alkaline so lution J E lectroanal Chem, 1992, 335: 309 319 11 Grimm R D, L ando lt D Investigation of the influence of pulse param eters on crack fo rm ation in palladi2 um electrodepo sitṡ S u rf ace and Coating s T echnology, 1987, 31 (2): 151 161 12 M artin J L, Toben M P Palladium and palladium alloy electrodepo sits in the electronics industry M etal F inish ing, 1990, 88 (1): 39 41 13 Graham A H, P ike2b iegunsk im J, U pdegraff S W Evaluation of palladium substitutes fo r go ld P lat2 ing and S u rf ace F inish ing, 1983, 70 (11): 52 57 14 Fukumo to Y, Kaw ash im a Y, H anda K, H ayash i Y Pulse current electrodepo sition of palladium M etal F inish ing, 1984, 82 (9): 77 80 15 M artin J L, M ccask ie J E, Toben M P Palladium p lating U S p atent 4, 622, 110 (N ov 11, 1986) and 4, 545, 868 (O cṫ 8, 1985) 16 F red I N ovel, Jam es L M artin, M ichael P Toben A lkaline bath s and m ethods fo r electrodepo sition of palladium and palladium alloyṡ E u rop ean P atent A pp lication 0225422 (June 6, 86) 17 F red I N ovel, Sands Po int, Jam es L M artin el al A lkaline bath s and m ethods fo r electrodepo sition of palladium and palladium alloyṡ U S P atent 4, 741, 818 (M ay 5, 1988) 18 A bys J A et al Palladium comp lexanṫ U S P atent 4, 911, 798 (M aṙ 27, 1990) 19 A bys J A et al Palladium additiveṡ U S P atent 4, 911, 799 (M ar 27, 1990) 20 F rank lin T C Som e m echanism s of action of additives in electrodepo sition p rocesseṡ S u rf ace and Coat2 ing s T echnology, 1987, 30: 415 428 21 :, 1987, 284 305 22 F letcher S Som e new fo rm ulae ap licable to electrochem ical nucleation grow thgco llision E lectroch im ica A cta, 1983, 28 (7): 917 923 23 Scharifker B, H ills G T heo retical and experim ental studies of m ultip le nucleation E lectroch im ica A cta, 1983, 28 (7): 879 889