electroless nickel plating of iron powder

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ELECTROLESS NICKEL PLATING OF IRON L. M. Kurvyakova, I. V. Pimenova, and E. P. Zakharova POWDER UDC 621.35:669.248T621.762 The object of the work described below was to study the electroless nickel plating of iron powder and determine conditions under which its particles become evenly coated with nickel and the extraction of nickel from a solution is a maximum [1-5]. Nickel deposition was performed with intense agitation (stirrer speed 500-800 rpm) in a solution containing 25 g/liter NiCI 2 6H20 , 25 g/liter NaH2PO4, 50 g/liter Na4P2OT, and 20 ml/Liter NH4OHconc" at pH 10 and a temperature of 18-25~ PZhCh-1 pure reduced iron powder, to TU 14- 127--90--77 technical specification, and electrolytic iron powders produced under laboratory conditions by the electrolysis of aqueous solutions were chosen for investigation. The particle size of the powders corresponded to that of a fraction passing through a No. 005 sieve (with an averaged size of 25 tim). Weighed samples of the powders were first pickled in 1% HC1 solution and washed until the water gave a neutral reaction~ To prevent powder losses due to stirring up during the washing, a magnetic base was employed. Aider nickel plating the powders were carefully washed free from the solution, dewatered with acetone, and dried in a desiccator at 40~ The degree of nicke] extraction from the solution was assessed photocolorimetrically by the change in the intensity of color of nickel in a solution with dimethyl glyoxime. The nickel contents of powder samples were determined by weighing the latter before and after nickel deposition. The distribution of nickel on the particle surfaces was studied with an MIM-7 metallographic microscope. This involved preparing masses containing metal powder samples and polymethyl methacrylate in the ratio 1 ." 10. The masses were pressed into glass tubes and polymerized in boiling water, after which stan- dard microsections were prepared. Before being examined, the microsections were lightly etched with 4% HNO 3. The results obtained were employed for plotting curves showing the effect of plating time on the nickel contents of the powders (Fig. la). With increasing plating time, the rate of the process decreased, indicating slower enrichment of the powders in nickel (curves 1-4). It will also be seen that, as the specific charge weight grew, the time required to reach this condition was shortened (curves I t and 1). 30 6 i r / / " I00 .//./d ~ X ~ gO ,• ,,/,,:,~S.:x2- ---, 2 ff eo i, / m ~ , ~'/_,')"~..,-~ .~ 50 20 a io r ,r b ~x t5 ~n t5 rain 5 r 5o #5 rain Fig. 1. Variation of nickel content of powder (a) and yield of nickel from solution (b) with plating time and powder charge weight: 1, I t) 100; 2, 2 w) 50; 3, 3 t) 20; 4, 4 t) 10 g/liter. Iron powders: 1-4) reduced; lY-4 t) electrolytic. D. I. Mendeleev Moscow Chemicotechnological Institute, Novomoskovsk Branch. Translated from Poro- shkovaya Metallurgiya, No. 5(197), pp. 15-17, May, 1979. Original article submitted July 11, 1978. 0038-5735/79/1805- 0295507.50 Plenum Publishing Corporation 295

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Page 1: Electroless nickel plating of iron powder

ELECTROLESS NICKEL PLATING OF IRON

L. M. Kurvyakova, I. V. Pimenova, and E. P. Zakharova

P O W D E R

UDC 621.35:669.248T621.762

The object of the work desc r ibed below was to study the e l e c t r o l e s s nickel plating of iron powder and de t e rmine conditions under which its pa r t i c l e s become evenly coated with nickel and the ex t rac t ion of nickel f rom a solution is a max imum [1-5]. Nickel deposit ion was p e r f o r m e d with intense agitat ion ( s t i r r e r speed 500-800 rpm) in a solution containing 25 g / l i t e r NiCI 2 �9 6H20 , 25 g / l i t e r NaH2PO4, 50 g / l i t e r Na4P2OT, and 20 ml /Li te r NH4OHconc" at pH 10 and a t e m p e r a t u r e of 18-25~ PZhCh-1 pure reduced iron powder, to TU 1 4 - 127--90--77 technical specif icat ion, and e lec t ro ly t i c iron powders produced under l abora to ry conditions by the e l e c t r o l y s i s of aqueous solutions were chosen fo r investigation.

The pa r t i c l e s ize of the powders co r responded to that of a f rac t ion pass ing through a No. 005 s ieve (with an ave raged size of 25 tim). Weighed s a m p l e s of the powders were f i r s t pickled in 1% HC1 solution and washed until the w a t e r gave a neut ra l reaction~ To prevent powder lo s ses due to s t i r r ing up during the washing, a magnet ic base was employed. Aider nickel plating the powders were ca re fu l ly washed f ree f rom the solution, dewatered with acetone, and dried in a d e s i c c a t o r at 40~ The degree of nicke] ex t rac t ion f rom the solution was a s s e s s e d pho toco lo r imet r i ca l ly by the change in the intensity of co lor of nickel in a solution with dimethyl g lyoxime. The nickel contents of powder s a m p l e s were de te rmined by weighing the l a t t e r before and a f t e r nickel deposit ion. The dis t r ibut ion of nickel on the par t ic le su r faces was studied with an MIM-7 meta l lographic m i c r o s c o p e . Th i s involved p repa r ing m a s s e s containing meta l powder s amples and polymethyl me thacry la te in the ra t io 1 ." 10. The m a s s e s were p r e s s e d into g lass tubes and po lymer i zed in boiling water , a f t e r which s t an- dard mic ro sec t i on s were p repa red . Before being examined, the mic rosec t ions were lightly etched with 4% HNO 3.

The r e su l t s obtained were employed for plotting cu rves showing the effect of plating t ime on the nickel contents of the powders (Fig. la) . With increas ing plating t ime , the ra te of the p r o c e s s dec reased , indicating s lower en r i chment of the powders in nickel (curves 1-4). It will a lso be seen that, as the specif ic charge weight grew, the t ime requ i red to r each this condition was shor tened (curves I t and 1).

30

6 i

r

/ / " I00 . / / . / d ~ X ~ gO

,• , , / , , : , ~ S . : x 2 - - - - , 2 f f eo i , / m ~

, ~'/_, ')"~.. ,-~ .~ 50

20 a

io

r

,r

b ~x

t5 ~n t5 rain 5 r 5o #5 rain

Fig. 1. Var ia t ion of nickel content of powder (a) and yield of nickel f r o m solution (b) with plating t ime and powder charge weight: 1, I t) 100; 2, 2 w) 50; 3, 3 t) 20; 4, 4 t) 10 g / l i t e r . I ron powders: 1-4) reduced; lY-4 t) e lec t ro ly t ic .

D. I. Mendeleev Moscow Chemicotechnological Insti tute, Novomoskovsk Branch. Trans la ted f rom P o r o - shkovaya Metal lurgiya, No. 5(197), pp. 15-17, May, 1979. Original a r t i c l e submit ted July 11, 1978.

0038-5735/79/1805- 0295507.50 �9 Plenum Publishing Corpora t ion 295

Page 2: Electroless nickel plating of iron powder

Fig. 2. Distr ibution of nickel on iron par t ic le su r - faces , • 340.

As e l ec t ro l e s s nickel-plat ing solutions are not ve ry stable, b reak down fa i r ly readi ly and a re difficult to co r r ec t , it is best to use them only once, ensuring a high degree of nickel extract ion. In our work the yield of nickel f rom the solution grew with increas ing specif ic charge weight and p roce s s t ime (Fig. lb). Examination of the distr ibution of nickel on the par t ic le sur faces made it possible to de termine conditions ensur ing full and even coating with nickel at a maximum ext rac t ion of meta l f rom the solution. At a charge weight of 100 g per l i t e r of the solution (curves 1 and 1'), in 30 rain 95-98% of then icke l in the solution was t r a n s f e r r e d to the pow- der . M i e r o s t r u c t u r a l examinat ions demonst ra ted tha t plating for 15-20 rain at this specific charge weight, a f te r which the powder had a nickel content of 7-8%, resu l ted in the format ion of even nickel coatings of 2- to 3 -#m thickness on the par t ic le su r faces (Fig. 2). Under these conditions the yield of nickel f rom the solution was 90-92%.

The p roce s s of e l ec t ro l e s s nickel plating was found to be affected also by the surface condition of the powder being t r ea ted . With the reduced powder, the amount of nickel in the powder and its yield f rom the solu- t ion were lower, o ther things being equal, than in the plating of the e lec t ro ly t ic powder (Fig, la and b). The reason for this was that in e l ec t ro l e s s nickel plating an important part is played by the catalyt ic action of the metal surface . A cata lyt ical ly active surface promotes the decomposit ion of the hypophosphite by water . A s a resu l t of this reac t ion e l ec t rons a r e l iberated, which reduce nickel ions to the metal . Elec t ro ly t ic i ron powder, being pu re r than reduced powder, apparent ly has g r e a t e r ca ta ly t ic power. As a resul t , the percentage amount of nickel is slightly h igher in e lec t ro ly t ic than in reduced powder.

C O N C L U S I O N S

A study was made of conditions ensur ing full and even coating of i ron powder par t ic les by nickel at a maximum ex t rac t ion of the metal f rom an e l ec t ro l e s s plating solution. The yield of nickel f rom the solution is h igher with e lec t ro ly t ic than with reduced iron powder.

L I T E R A T U R E C I T E D

1. I . M . Fedorchenko, "Scope and tasks of powder metal lurgy in the formulat ion of new mater ia l s , n Poroshk. Metall . , No. 1, 3-6 (1963).

2. Yu. A. Sidorenko and P. I. Kukin, "Phospho rus - f r ee e l ec t ro l e s s nickel deposits on powders," Poroshk. Metall. , No. 2, 29-31 (1977).

3. V . I . Pavlenko and D. S~ Yas' , "The copper plating of graphite powders in the manufacture of c o p p e r - graphite mate r ia l s , " Poroshk. Metall . , No. 2, 9-13 (1976).

4. N . L . Kctovskaya, A. V. Pomosov, and L. M. Kurvyakova, NSilver plating of coarse copper powder, n Poroshk. Metall . , No. 8, 16-19 (1971).

5. S .A . Vishenkov, Chemical and ChemicothermalMethods of Depositing Metal Coatings [in Russian], Mashinostroenie , Moscow (1975).

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